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CN104073803A - Etching composition for copper-based metal layer and method of preparing metal line - Google Patents

Etching composition for copper-based metal layer and method of preparing metal line Download PDF

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Publication number
CN104073803A
CN104073803A CN201410123681.0A CN201410123681A CN104073803A CN 104073803 A CN104073803 A CN 104073803A CN 201410123681 A CN201410123681 A CN 201410123681A CN 104073803 A CN104073803 A CN 104073803A
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CN
China
Prior art keywords
acid
copper
etching agent
etching
metal level
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CN201410123681.0A
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Chinese (zh)
Inventor
李恩远
李铉奎
权玟廷
金镇成
梁圭亨
赵成培
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Dongwoo Fine Chem Co Ltd
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Dongwoo Fine Chem Co Ltd
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Priority claimed from KR1020130033687A external-priority patent/KR20140119885A/en
Priority claimed from KR1020130033685A external-priority patent/KR20140119884A/en
Priority claimed from KR1020130034519A external-priority patent/KR20140119937A/en
Priority claimed from KR1020130034520A external-priority patent/KR20140118493A/en
Priority claimed from KR1020130034515A external-priority patent/KR20140118491A/en
Priority claimed from KR1020130034517A external-priority patent/KR20140118492A/en
Application filed by Dongwoo Fine Chem Co Ltd filed Critical Dongwoo Fine Chem Co Ltd
Publication of CN104073803A publication Critical patent/CN104073803A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00Etching metallic material by chemical means
    • C23F1/02Local etching
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/16Acidic compositions
    • C23F1/18Acidic compositions for etching copper or alloys thereof

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Weting (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

The invention relates to an etching composition for a copper-based metal layer and a method for preparing a metal line. The invention discloses an etching agent composition for the copper-based metal layer. The etching agent composition can represent an excellent cone angle profile. Furthermore the invention discloses a method of forming a wiring through the etching agent composition. The etching agent composition for the copper-based metal layer comprises the components of: 0.5-20% by weight of persulfate, 0.1-5% by weight of a triazole compound and the balance of water. Therefore the copper-based metal layer is selectively etched. An excellent straightness of the etched pattern is realized. Furthermore an improved cone angle profile is represented.

Description

For the etch combination and the method for preparing metal wire of the metal level based on copper
Technical field
The present invention relates to a kind of etching agent composite for excellent cone angle profile of can presenting of the metal level based on copper, and relate to the method that uses this etching agent composite to form wiring.
Background technology
For example, the representative semiconductor devices that is provided with the low resistance wiring that contains copper can comprise liquid-crystal display (LCD) device.
The flat-panel monitor (FPD) that aforementioned LCD device is the film type of lightweight and can substitute the existing display unit such as cathode ray tube (CRT), aforementioned LCD device utilizes the optical isotropy character of liquid crystal to express image, and can effectively be used in notebook computer or the desk-top computer with excellent resolving power, color displays and picture quality.
The liquid crystal layer that liquid crystal indicator conventionally has colored filter substrate, array substrate and forms between colored filter substrate and array substrate.
The driving method that is mainly used in LCD device is active matrix (AM), and it drives amorphous silicon film transistor (a-Si TFT) liquid crystal of pixel portion as switch device.
In LCD device, be selected for metal line if there is the metal of low-resistivity and high erosion resistance, the material that forms the metal line (for example, gate line or data line) in order to interference signal can improve reliability and the price competitiveness of product.Aluminium (Al) or Al alloy have mainly been used as metal line material as described above.
But along with the size of LCD device increases, for SVGA, XGA, SXGA, VXGA etc., it is higher that resolving power becomes, reduce synchronous signal processing sweep time and greatly accelerated.Therefore, must use the metallic substance of low-resistivity to form metal line, to process these situations.
Therefore, proposed recently to replace existing metal line material with the copper with the resistivity more excellent than current material and electromigration characteristic.
Under afore-mentioned, cause more concern in the application of new low resistivity metal film for the etching agent composite of copper layer or the metal level based on copper.Although the different types of etching agent composite for the metal level based on copper of current use, but the required performance of user can't be satisfactory.
For example, the open No.2005-0067934 of Korean Patent discloses for the etching reagent of etch copper metal level and stacking transparent semiconductor layer, and described etching reagent comprises nitric acid, hydrochloric acid, hydrogen peroxide and azole compounds.But the problem that above-mentioned patent has is that the copper metal layer on upper strata and the indium oxide layer of lower floor are etched, and electric short circuit or wiring trouble can occur thus.
Summary of the invention
Therefore, the object of this invention is to provide the etching agent composite of a kind of cone angle profile that can form improvement and excellent planeness.
Another object of the present invention is to provide a kind of etching agent composite for the metal level based on copper, and it can not leave the residue of the metal level based on copper.
Another object of the present invention is to provide a kind of for using etching agent composite to form the method for wiring.
Above-mentioned purpose of the present invention realizes by following feature:
(1) for an etching agent composite for the metal level based on copper, comprising: persulphate, 0.1 azole compounds of % by weight to 5 % by weight and the water of surplus of 0.5 % by weight to 20 % by weight.
(2) basis (1) described etching agent composite above, wherein, described persulphate is to be selected from Potassium Persulphate (K 2s 2o 8), Sodium Persulfate (Na 2s 2o 8) and ammonium persulphate ((NH 4) 2s 2o 8) at least one.
(3) basis (1) described etching agent composite above, wherein, described azole compounds is at least one being selected from triazole compounds, amino tetrazole compound, imidazolium compounds, benzazolyl compounds, purine compound, pyrazole compound, pyridine compounds, pyrimidine compound, azole compounds, pyrrolidine compound and pyrrolinium compound.
(4) basis (1) described etching agent composite above, also comprises: organic (peroxide) acid or its salt of 1 % by weight to 5 % by weight.
(5) basis (4) described etching agent composite above, wherein, described organic (peroxide) acid is at least one being selected from Peracetic Acid, benzoyl hydroperoxide, acetic acid, butyric acid, citric acid, formic acid, gluconic acid, oxyacetic acid, propanedioic acid, valeric acid and oxalic acid.
(6), according to the etching agent composite above (4) described, wherein, the salt of described organic (peroxide) acid is at least one in the sodium salt of the sylvite that is selected from organic (peroxide) acid, organic (peroxide) acid and the ammonium salt of organic (peroxide) acid.
(7), according to the etching agent composite above (1) described, also comprise the phosphonate compound of 3 % by weight to 15 % by weight.
(8) basis (7) described etching agent composite above, wherein, described phosphonate compound is to be selected from phosphoric acid, 2-amino-ethyl phosphonic acids, dimethyl methyl phosphonate, 1-hydroxy ethylene-1, 1-di 2 ethylhexyl phosphonic acid, amino three (methylene phosphonic acids), EDTMP, tetramethylene-diamine four (methylene phosphonic acid), hexamethylene-diamine four (methylene phosphonic acid), diethylene triamine penta(methylene phosphonic acid), phosphonic acids butane-tricarboxylic acid, N-((phosphonomethyl)) iminodiethanoic acid, 2-propyloic phosphonic acids, at least one in 2-hydroxy phosphinylidyne yl carboxylic acid and amino-tri--(methylene phosphonic acid).
(9) basis (7) described etching agent composite above, wherein, described phosphonate compound is at least one in sylvite, the sodium salt of phosphonate compound and the ammonium salt of phosphonate compound that is selected from phosphonate compound.
(10) basis (1) described etching agent composite above, also comprises: the mineral acid of 0.5 % by weight to 3 % by weight or its salt (wherein, except persulphate).
(11) basis (10) described etching agent composite above, wherein, described mineral acid is at least one being selected from nitric acid, sulfuric acid, phosphoric acid, boric acid and perchloric acid.
(12) basis (10) described etching agent composite above, wherein, the salt of described mineral acid is at least one (wherein, except the persulphate) in sylvite, the sodium salt of mineral acid and the ammonium salt of mineral acid that is selected from mineral acid.
(13), according to the etching agent composite above (1) described, also comprise sulfonic acid or its salt of 0.5 % by weight to 5 % by weight.
(14) basis (13) described etching agent composite above, wherein, described sulfonic acid is at least one being selected from thionamic acid, methylsulphonic acid, ethylsulfonic acid, tosic acid, trifluoromethanesulfonic acid, Phenylsulfonic acid, thionamic acid and polystyrolsulfon acid.
(15) basis (13) described etching agent composite above, wherein, the salt of described sulfonic acid is at least one being selected from sylvite, sodium salt and ammonium salt.
(16), according to the etching agent composite above (1) described, also comprise the mantoquita (wherein, except the persulphate of copper) of 0.5 % by weight to 3 % by weight.
(17) basis (16) described etching agent composite above, wherein, described mantoquita is at least one being selected from copper sulfate, cupric nitrate, cupric chloride, venus crystals and cupric fluoride.
(18) basis (1) described etching agent composite above, wherein, forms the described metal level based on copper, and the described metal level based on copper comprises: be selected from least one in copper, copper nitride and cupric oxide; Or comprise at least one and the alloy that is selected from least one metal in aluminium (Al), magnesium (Mg), calcium (Ca), titanium (Ti), silver (Ag), chromium (Cr), manganese (Mn), iron (Fe), zirconium (Zr), niobium (Nb), molybdenum (Mo), palladium (Pd), hafnium (Hf), tantalum (Ta) and tungsten (W) of being selected from copper, copper nitride and cupric oxide.
(19) basis (18) described etching agent composite above, wherein, the described metal level based on copper comprises: copper molybdenum layer, the metal level based on copper that it has molybdenum layer and forms on this molybdenum layer; Or copper molybdenum alloy layer, the metal level based on copper that it has molybdenum alloy layer and forms on this molybdenum alloy layer.
(20) be used to form the method for wiring, comprise:
(S1) on substrate, form metal oxide layer;
(S2) on described metal oxide layer, form the metal level based on copper;
(S3) on the described metal level based on copper, form photoetching agent pattern alternatively; With
(S4) by using according to the etching agent composite described in any one in above-mentioned (1) to (19), the only described metal level based on copper on metal oxide layer described in etching.
(21) method according to above (20), wherein, forms described metal oxide layer, and described metal oxide layer comprises: pass through A xb yc zwherein, A, B and C are respectively the metals being selected from zinc (Zn), titanium (Ti), cadmium (Cd), gallium (Ga), indium (In), tin (Sn), hafnium (Hf), zirconium (Zr) and tantalum (Ta) to O(; X, y and z all represent metal ratio and are 0 or are greater than 0 integer or prime number) the three-component system oxide compound or the four component system oxide compounds that represent.
(22) basis (20) described method above, wherein, forms the described metal level based on copper, and the described metal level based on copper comprises: be selected from least one in copper, copper nitride and cupric oxide; Or comprise at least one and the alloy that is selected from least one metal in aluminium (Al), magnesium (Mg), calcium (Ca), titanium (Ti), silver (Ag), chromium (Cr), manganese (Mn), iron (Fe), zirconium (Zr), niobium (Nb), molybdenum (Mo), palladium (Pd), hafnium (Hf), tantalum (Ta) and tungsten (W) of being selected from copper, copper nitride and cupric oxide.
(23) method according to above (22), wherein, the described metal level based on copper comprises: copper molybdenum layer, the metal level based on copper that it has molybdenum layer and forms on this molybdenum layer; Or copper molybdenum alloy layer, the metal level based on copper that it has molybdenum alloy layer and forms on this molybdenum alloy layer.
(24) manufacture, for a method for the array substrate of liquid crystal indicator, comprising:
A) on substrate, form grid wiring;
B) on the substrate that comprises described grid wiring, form gate insulator;
C) on described gate insulator, form semiconductor layer;
D) on described semiconductor layer, form source wiring and drain electrode wiring; With
E) form the pixel electrode that is connected to described drain electrode wiring,
Wherein, described a) step comprises: on described substrate, form the metal level based on copper, and use according to the metal level based on copper described in the etching agent composite etching described in any one in above-mentioned (1) to (19) to form described grid wiring.
(25) manufacture, for a method for the array substrate of liquid crystal indicator, comprising:
A) on substrate, form grid wiring;
B) on the substrate that comprises described grid wiring, form gate insulator;
C) on described gate insulator, form semiconductor layer;
D) on described semiconductor layer, form source wiring and drain electrode wiring; With
E) form the pixel electrode that is connected to described drain electrode wiring,
Wherein said d) step comprises: on described semiconductor layer, form the metal level based on copper, and use according to the metal level based on copper described in the etching agent composite etching described in any one in above-mentioned (1) to (19) to form described source wiring and drain electrode wiring.
The selectively metal level of etching based on copper and without the oxide skin of etching lower floor of etching agent composite of the present invention.
In addition, etching agent composite of the present invention can have excellent etched pattern planeness, present the cone angle profile of improvement and there is the beneficial effect that prevents the residue that forms metal level based on copper, therefore the excellent effect preventing such as electric short circuit, wiring trouble, brightness reduction etc. is provided.
Adopt wet etch process instead of adopt dry etching method according to the method for formation wiring of the present invention, therefore, it does not need expensive equipment, has thus economic advantages.
Embodiment
The invention discloses a kind of etching agent composite for the metal level based on copper, it comprises: persulphate, 0.1 azole compounds of % by weight to 5 % by weight and the water of surplus of 0.5 % by weight to 20 % by weight, the metal level of etching based on copper optionally thus, there is the planeness of excellent etched pattern, and present the cone angle profile of improvement.
Below will specifically describe the present invention.
Etching agent composite of the present invention comprises the water of persulphate, azole compounds and surplus, and this etching agent composite is the composition of the metal level based on copper for etching.
Metal level based on copper according to the present invention be as raw-material film to form metal line so that transmission electronic signal, and can be called the metal level of cupric.The metal level based on copper that can apply etching agent composite of the present invention can be the design that comprises unitary film or multilayer film, and is not particularly limited, as long as above-mentioned layer can be consistent with above-mentioned design.For example, aforementioned layers can refer to formed metal level, and this metal level comprises: be selected from least one in copper, copper nitride and cupric oxide; Or any one comprises and is selected from least one metal in aluminium (Al), magnesium (Mg), calcium (Ca), titanium (Ti), silver (Ag), chromium (Cr), manganese (Mn), iron (Fe), zirconium (Zr), niobium (Nb), molybdenum (Mo), palladium (Pd), hafnium (Hf), tantalum (Ta) and tungsten (W) and is selected from least one the alloy in copper, copper nitride and cupric oxide, but is not limited to this.
In addition, the metal level based on copper can be the design that comprises unitary film and multilayer (for example, bilayer) film.The aforementioned metal level based on copper can be the film of single or multiple lift (for example, copper molybdenum layer or copper molybdenum alloy layer).Copper molybdenum layer refers to the metal level based on copper that comprises molybdenum layer and form on this molybdenum layer, and copper molybdenum alloy layer refers to the metal level based on copper that comprises molybdenum alloy layer and form on this molybdenum alloy layer.Molybdenum alloy can comprise molybdenum and the alloy that is selected from least one metal in Ti, Ta, Cr, Ni, Nd and In.
The persulphate comprising in etching agent composite of the present invention is the main component of the metal level of etching based on copper.With respect to the gross weight of composition, the weight percent content of the persulphate that can comprise is 0.5% to 20%, preferably 1% to 15%.If the content of persulphate is less than 0.5 % by weight, etching speed reduces, thereby cause insufficient etching of the metal level based on copper, and in the time that the content of persulphate exceedes 20 % by weight, total etching speed becomes suitable height and makes because the over etching of the metal level based on copper causes etching degree and controls the difficulty on etch process.
Operable persulphate is not particularly limited in the present invention, and can comprise, for example, and Potassium Persulphate (K 2s 2o 8), Sodium Persulfate (Na 2s 2o 8), ammonium persulphate ((NH 4) 2s 2o 8), these materials can use separately or with two kinds or more than two kinds be used in combination.
The effect that the azole compounds comprising in etching agent composite of the present invention can play is: the CD(critical size of controlling etching speed and minimizing pattern) loss, increase thus process margin.With respect to the gross weight of composition, the content range of azole compounds can be from 0.1 % by weight to 5 % by weight, preferably from 0.5 % by weight to 2 % by weight.If the content of azole compounds is less than 0.1 % by weight, can there is too large CD loss; And in the time that the content of azole compounds exceedes 5 % by weight, it is too low that the etching speed of the metal level based on copper becomes, thereby greatly extend process period.
Azole compounds is not particularly limited, as long as it can be included in arbitrary conventional azole compounds used in correlation technique.For example, azole compounds preferably has 1 azole compounds to 30 carbon atoms.More specifically, triazole compounds, amino tetrazole compound, imidazolium compounds, benzazolyl compounds, purine compound, pyrazole compound, pyridine compounds, pyrimidine compound, azole compounds, pyrrolidine compound and pyrrolinium compound can use separately or with two kinds or more than two kinds be used in combination.
For example, triazole compounds can comprise the compound representing by following formula 1, and it can use separately or with two kinds or more than two kinds be used in combination.
[formula 1]
(wherein, R 1and R 2be respectively hydrogen atom; Carboxyl; Amino; Hydroxyl; Cyano group; Formyl radical; Or sulfonic group; Or there is 1 alkyl to 20 carbon atoms or alkylsulfonyl, described in there is 1 alkyl to 20 carbon atoms or alkylsulfonyl is not substituted or is replaced by carboxyl, amino, hydroxyl, cyano group, formyl radical or sulfonic group, and R 1and R 2can comprise ester group, and
Q is hydrogen atom; Hydroxyl; The substituting group representing by following formula 2; Or there is 1 alkyl to 10 carbon atoms or alkoxyl group, described in there is 1 alkyl to 10 carbon atoms or alkoxyl group is not substituted or had 6 aryl to 20 carbon atoms or hydroxyl replaces; And Q can comprise at least one in amino or ester group).
[formula 2]
(wherein R 3to there is 1 alkylidene group to 6 carbon atoms, and R 4and R 5it is respectively hydrogen atom; Hydroxyl; Or have 1 alkyl to 10 carbon atoms, hydroxyalkyl or alkoxyalkyl, it is not substituted or is replaced by hydroxyl).
The compound that through type 1 represents can comprise 1, 2, 3-benzotriazole, 5-Methylbenzotriazole, benzotriazole, 1-(2, 2-dihydroxy ethyl) benzotriazole, I-hydroxybenzotriazole, 1-methoxyl group benzo triazole, 1-(1, 2-dihydroxypropyl) benzotriazole, 1-(2, 3-dihydroxypropyl) benzotriazole, N, N-pair-(2-ethylhexyl)-arylmethyl-1H-benzotriazole-1-methylamine, 2, 2'-{[(4-methyl isophthalic acid H-benzotriazole-1-yl) methyl] imino-} di-alcohol, 2, 2'-{[(5-methyl isophthalic acid H-benzotriazole-1-yl) methyl] imino-} di-alcohol, 5-carboxyl benzotriazole butyl ester, 5-carboxyl benzotriazole monooctyl ester, 5-carboxyl benzotriazole dodecyl ester etc.
Except the compound that through type 1 represents, etching agent composite of the present invention also can be included in the triazole compounds of the arbitrary routine using in correlation technique.For example, triazole compounds can comprise 1,2,3-triazoles, 1,2,4-triazole, tolyl-triazole, 4-amino-1,2,4-triazole etc., and these triazole compounds are used alone or with two kinds or more than two kinds be used in combination.
For example, imidazolium compounds can comprise: glyoxal ethyline, 2-ethyl imidazol(e), 2-propyl imidazole, 2-aminooimidazole, 4-methylimidazole, 4-ethyl imidazol(e), 4-propyl imidazole etc., these imidazolium compoundss are used alone or with two kinds or more than two kinds be used in combination.
For example, amino tetrazole compound can comprise: amino tetrazole, 5-amino-1-phenyltetrazole, 5-amino-1-(1-naphthyl) tetrazolium, 1-methyl-5-amino tetrazole, 1,5-diamino tetrazoliums etc., preferably use amino tetrazole.
For example, benzazolyl compounds can comprise: aminoalkyl indole, benzoyl indoles, skatole, phenylacetyl indoles, indole carbazole, these benzazolyl compounds use separately or with two kinds or more than two kinds be used in combination.
For example, purine compound can comprise: 6-dimethylaminopurine, 2, the chloro-7-methyl-7H-of 6-bis-purine, 6-(γ, γ-dimethyl-allyl amino) purine, the chloro-9H-purine-9-of 2-amino-6-acetic acid etc., these materials are used alone or with two kinds or more than two kinds be used in combination.
For example, pyrazole compound can comprise: 3-phenyl-1H-pyrazoles, 3-(amino methyl) pyrazoles, 5-(2-thienyl) pyrazoles, 1-(2-hydroxyethyl)-pyrazoles, 3-(2-thienyl) pyrazoles, 5-methyl isophthalic acid H-pyrazoles, 4-nitro-1H-pyrazoles, 1H-pyrazoles-5-boric acid etc., these pyrazole compounds are used alone or with two kinds or more than two kinds be used in combination.
For example, pyridine compounds can comprise: 4-(amino-ethyl) pyridine, 2-(methylamino) pyridine, pyridine trifluoro-acetate, pyridine-4-ethanamide, 2-[(pyridine-3-carbonyl)-amino]-phenylformic acid etc., these pyridine compounds are used alone or with two kinds or more than two kinds be used in combination.
For example, pyrimidine compound can comprise: pyrimidine-5-carboxylic acid, pyrimidine-2-carboxylic acid etc., these pyrimidine compounds are used alone or with two kinds or more than two kinds be used in combination.
For example, azole compounds can comprise: pyrroles-2-carboxylic acid, pyrroles-3-carboxylic acid, 1-(2-aminophenyl) pyrroles, 1H-pyrroles-1-propionic acid etc., these azole compounds are used alone or with two kinds or more than two kinds be used in combination.
For example, pyrrolidine compound can comprise: 1-(2-amino-ethyl) tetramethyleneimine, tetramethyleneimine-3-carboxylic acid, tetramethyleneimine-3-carboxylic acid hydrochloride, tetramethyleneimine-1,2-dicarboxylic acid 1-phenyl esters etc., these pyrrolidine compounds are used alone or with two kinds or more than two kinds be used in combination.
For example, pyrrolinium compound can comprise: 3-pyrroline, 2-methyl isophthalic acid-pyrroline, 1-benzyl-3-pyrroline etc., these pyrrolinium compounds are used alone or with two kinds or more than two kinds be used in combination.
Alternatively, etching agent composite of the present invention also can comprise organic (peroxide) acid or its salt.
The pH value that organic (peroxide) acid or its salt can be controlled etching reagent, to increase the activity of persulphate, is controlled the etching speed of the metal level based on copper thus, and for suppressing the degraded of persulphate, and the oxygenizement of the metal level of performance assisted etch based on copper.In the present invention, organic (peroxide) acid refers to organic acid, organic peroxide acid or its combination.
With respect to the gross weight of composition, the amount that organic (peroxide) acid or its salt can be included is 1 % by weight to 5 % by weight, preferably 1 % by weight to 3 % by weight.If the content of organic (peroxide) acid or its salt is less than 1 % by weight, in the metal level based on copper, can there is not etched part; And in the time that the content of organic (peroxide) acid or its salt exceedes 5 % by weight, thereby etching speed becomes the very high difficulty causing in technology controlling and process.
The concrete example of organic (peroxide) acid can comprise at least one being selected from Peracetic Acid, benzoyl hydroperoxide, acetic acid, butyric acid, citric acid, formic acid, gluconic acid, oxyacetic acid, propanedioic acid, valeric acid and oxalic acid.The salt of organic (peroxide) acid is selected from least one in sylvite, sodium salt and ammonium salt.
Alternatively, etching agent composite of the present invention also can comprise phosphonate compound.
Phosphonate compound can be combined into inner complex to control the activity of cupric ion with the cupric ion being eluted in etching reagent during etched copper, suppresses thus the degraded of persulphate.Owing to having reduced the activity of cupric ion, therefore this technique can stably be carried out during using etching reagent.With respect to the gross weight of composition, the amount that phosphonate compound can be included is 3 % by weight to 15 % by weight, preferably 5 % by weight to 10 % by weight.If the content of phosphonate compound is less than 3 % by weight, the degraded of etched homogeneity reduction and persulphate is accelerated, and has reduced thus working ability; And in the time that the content of phosphonate compound exceedes 15 % by weight, thereby total etching speed becomes the very high difficulty causing in technology controlling and process, and the viscosity of etching reagent increases.
Phosphonate compound comprises phosphonic acid ester, phosphate derivatives and its salt.The concrete example of phosphonate compound can comprise and is selected from phosphoric acid, 2-amino-ethyl phosphonic acids (2-AEP), dimethyl methyl phosphonate (DMMP), 1-hydroxy ethylene-1, 1-di 2 ethylhexyl phosphonic acid (HEDP), amino three (methylene phosphonic acids) (ATMP), EDTMP (EDTMP), tetramethylene-diamine four (methylene phosphonic acid) (TDTMP), hexamethylene-diamine four (methylene phosphonic acid) (HDTMP), diethylene triamine penta(methylene phosphonic acid) (DTPMP), phosphonic acids butane-tricarboxylic acid (PBTC), N-((phosphonomethyl)) iminodiethanoic acid (PMIDA), 2-propyloic phosphonic acids (CEPA), 2-hydroxy phosphinylidyne yl carboxylic acid (HPAA) and amino-tri--(methylene phosphonic acid) are (AMP), or at least one in its salt.
The salt of phosphonate compound can comprise at least one in sylvite, the sodium salt of phosphonate compound and the ammonium salt of phosphonate compound that is selected from phosphonate compound.
Alternatively, etching agent composite of the present invention also can comprise mineral acid or its salt (wherein, except persulphate).
The pH value that mineral acid or its salt (wherein, persulphate except) can be controlled etching reagent, to increase the activity of persulphate, is controlled the etching speed of the metal level based on copper thus, and for increasing the cone angle of etched surfaces.With respect to the gross weight of composition, the amount that mineral acid or its salt can be included is 0.5 % by weight to 3.0 % by weight, preferably 1.0 % by weight to 2.0 % by weight.If the content of mineral acid or its salt is less than 0.5 % by weight, etching speed reduces, and in the time that the content of mineral acid or its salt exceedes 3.0 % by weight, thereby etching speed causes over etching problem and the damage to photoresist material very soon.
The concrete example of mineral acid or its salt can comprise at least one being selected from nitric acid, sulfuric acid, phosphoric acid, boric acid and perchloric acid.Aspect this, because hydrochloric acid can damage the metal level based on copper and the metal oxide layer in some situation described below, therefore mineral acid or its salt cannot comprise hydrochloric acid.The salt of mineral acid can comprise at least one being selected from sylvite, sodium salt and ammonium salt, still, and except persulphate.
Alternatively, etching agent composite of the present invention also can comprise sulfonic acid or its salt.
Sulfonic acid or its salt in the aqueous solution by dissociation (RSO 3h →-RSO 3 -+ H +) to present sour performance.The acidity ratio of sulfonic acid is much better than such as the carboxylic acid of acetic acid, and is substantially similar to sulfuric acid.Sulfonic acid in etching agent composite of the present invention can be controlled the pH value of etching reagent to increase the activity of persulphate, controls thus the etching speed of the metal level based on copper, and for suppressing the degraded of persulphate and the cone angle of reduction etched surfaces.In the present invention, sulfonic acid all refers to have-SO 3the compound of H, and comprise inorganic sulfonic acid and organic sulfonic acid.
With respect to the gross weight of composition, the amount that sulfonic acid or its salt can be included is 0.5 % by weight to 5 % by weight, preferably 1 % by weight to 3 % by weight.If the content of sulfonic acid or its salt is less than 0.5 % by weight, etching speed reduces, and in the time that the content of sulfonic acid or its salt exceedes 5 % by weight, thereby etching speed causes the difficulty in technology controlling and process very soon.
The concrete example of sulfonic acid can comprise at least one being selected from thionamic acid, methylsulphonic acid, ethylsulfonic acid, tosic acid, trifluoromethanesulfonic acid, Phenylsulfonic acid, thionamic acid and polystyrolsulfon acid.The salt of sulfonic acid can comprise at least one being selected from sylvite, sodium salt and ammonium salt.
Alternatively, etching agent composite of the present invention also can comprise mantoquita (wherein, except the persulphate of copper).
Mantoquita can be controlled the pH value of etching reagent to increase the activity of persulphate, and the etching speed of controlling thus the metal level based on copper changes (deflection) to control CD, and for suppressing the degraded of persulphate and the cone angle of reduction etched surfaces.
With respect to the gross weight of composition, the amount that mantoquita can be included is 0.5 % by weight to 3 % by weight, preferred 1 % by weight to 2 % by weight.If the content of mantoquita is less than 0.5 % by weight, the CD that pending many sheet materials can seriously occur changes (deflection), and in the time that the content of mantoquita exceedes 3 % by weight, thereby the oxidation susceptibility of primary oxidant is lowered the quantity reduction that causes pending sheet material.
The concrete example of mantoquita can comprise at least one being selected from copper sulfate, cupric nitrate, cupric chloride, venus crystals and cupric fluoride.
In etching agent composite of the present invention, can also comprise the water of the surplus except the content of aforementioned composition of the composition that amounts to 100 % by weight.Water used is not particularly limited in the present invention, but preferred deionized water.In addition, more preferably using resistivity value is 18M Ω cm or the deionized water that is greater than 18M Ω cm.The degree of ion is removed in resistivity value instruction from water.
Alternatively, etching agent composite of the present invention also can comprise tensio-active agent.Tensio-active agent can play and reduce surface tension to increase the effect of etching uniformity coefficient.Tensio-active agent is not particularly limited, as long as it can have resistibility and compatible with etching agent composite of the present invention to etching agent composite of the present invention, but, for example, preferably include, be selected from least one or two kinds or more kinds of in anion surfactant, cats product, amphoterics, nonionogenic tenside and EPE polyol EPE.
Except aforementioned composition, etching agent composite of the present invention also can comprise the additive of arbitrary routine.For example, this additive can be metal ion chelation agent, corrosion inhibitor etc.
Aforementioned etching agent composite of the present invention can be pressed into the block metal level based on copper and metal oxide layer by etch layer, and forms the tapered profiles with excellent planeness, is therefore effectively used in the formation of wiring.
Be used to form according to the method for wiring of the present invention embodiment and can comprise: (S1) on substrate, form metal oxide layer; (S2) on described metal oxide layer, form the metal level based on copper; (S3) on the described metal level based on copper, form photoetching agent pattern alternatively; (S4) by using according to aforementioned etching agent composite of the present invention, be only etched in the described metal level based on copper on described metal oxide layer.
According to the method being used to form according to wiring of the present invention, use conventional photoresist material, can form photoetching agent pattern by exposure and the developing process of arbitrary routine.
According to the method that is used to form wiring of the present invention, metal oxide layer is the film that can form oxide semiconductor layer, and can be arbitrary common metal oxide skin used in correlation technique.For example, metal oxide layer can comprise: adopt A xb yc zwherein, A, B and C are respectively the metals being selected from zinc (Zn), titanium (Ti), cadmium (Cd), gallium (Ga), indium (In), tin (Sn), hafnium (Hf), zirconium (Zr) and tantalum (Ta) to O(independently; X, y and z all refer to metal ratio and are 0 or are greater than 0 integer or prime number) the three-component system oxide compound or the four component system oxide compounds that represent.
Be used to form according to the method for wiring of the present invention and can be applied to the array substrate of manufacturing LCD device.Hereinafter by the method specifically describing for the manufacture of the array substrate of LCD device according to the present invention.
First, on substrate, form grid wiring.The effect that grid wiring can play is, according to the electrical signal being transmitted by grid lead, to be controlled at the electric current between source/drain.The material of grid wiring can comprise the aforementioned metal level based on copper, therefore, by using according to etching agent composite of the present invention, can form the metal level based on copper with required pattern.
Then, on grid wiring, form gate insulator.The effect that gate insulator can play is: the active layer at grid wiring and top is separated, to prevent that the electric current that flows into active layer from flowing into grid wiring.
Form as follows gate insulator.For example, plasma activated chemical vapour deposition (CVD) method is used to be formed uniformly gate insulator on the substrate that comprises grid wiring.Use by being selected from silicon-dioxide (SiO 2), at least one insulating material of making in silicon nitride (SiNx) and silicon oxynitride (SiONx) etc., can form gate insulator.
Then, on gate insulator, form semiconductor layer.Semiconductor layer becomes according to the path of the electric current of the electrical signal from grid wiring.Use aforementioned metal oxide material (A xb yc zo), can on gate insulator, be formed uniformly active layer by plasma CVD method.
After this, on semiconductor layer, form source wiring and drain electrode wiring.Source wiring and drain electrode wiring can be used for electrical signal to be transformed into pixel.The material of source/drain wiring used can comprise the aforementioned metal level based on copper in this article, therefore, by using according to etching agent composite of the present invention, can form source/drain wiring with required pattern.
Then, form the pixel electrode that is connected to drain electrode wiring.
According to preceding method, can manufacture the array substrate for LCD device.
Hereinafter, describe preferred embodiment in connection with embodiment, more clearly to understand the present invention.But, it will be appreciated by those skilled in the art that, such embodiment is provided for illustrative object, can make multiple modification and variation and not depart from the scope of the present invention and spirit, such modification and variation are suitably included in the present invention who limits by appending claims.
Embodiment
1-1. embodiment 1 to embodiment 5 and comparing embodiment 1 are to comparing embodiment 4
According to the component of enumerating in following table 1, to comparing embodiment 4, prepare etching agent composite (unit: with respect to the weight percent of total weight percent 100%) at embodiment 1 to embodiment 5 and comparing embodiment 1.
[table 1]
1-2. EXPERIMENTAL EXAMPLE 2
After metal oxide materials (ITO) being deposited on glass substrate (100mm × 100mm) and copper being deposited upon on above-mentioned layer, by photolithography, the photoresist material with required pattern is formed on substrate.Then, use respectively in embodiment 1 to embodiment 5 and comparing embodiment 1 to every kind of prepared composition in comparing embodiment 4, the metal level based on copper is carried out to etch process.
Use the equipment (model name: ETCHER(TFT) of injection etching pattern, SEMES company), and be maintained at the temperature of approximately 30 DEG C at during etching etching agent composite.But, if needed, can, according to other processing condition and other factors, suitably change temperature.Etching is carried out approximately 100 seconds conventionally, and this time can change according to etch temperature.During etch process the profile of the etched metal level based on copper adopt section S EM(scanning electronic microscope, by the manufacturing of Hitachi company, model name: S-4700) detect, and detected result is as shown in table 2 below.
< evaluates the standard > of etching outline
Zero: 35 °≤cone angle≤60 °
△: cone angle <35 ° or cone angle >60 °
Х: undercutting or back taper
Unetched: not etching
< is for evaluating the standard > of etching planeness
Zero: straight pattern
△: 20% or be less than 20% bending pattern
Х: exceed 20% bending pattern
Unetched: not etching
[table 2]
As shown in table 2, the etching agent composite in embodiment 1 to 5 all presents favourable etch features.
But, the content concn of the persulphate that the content concn of the persulphate having in comparing embodiment 1(comparing embodiment 1 has lower than the present invention), the etching of copper layer is impossible; There is a large amount of persulphates in comparing embodiment 2(comparing embodiment 2), confirm to occur over etching situation.In addition, there is a small amount of azole compounds in comparing embodiment 3(comparing embodiment 3), confirm to occur over etching situation.In addition, there is a large amount of azole compounds in comparing embodiment 4(comparing embodiment 4), the etching of copper layer is impossible.
2-1. embodiment 6 to embodiment 11 and comparing embodiment 5 are to comparing embodiment 10
According to the component of enumerating in following table 3, to comparing embodiment 10, prepare etching agent composite (unit: with respect to the weight percent of total weight percent 100%) at embodiment 6 to embodiment 11 and comparing embodiment 5.
[table 3]
2-2. EXPERIMENTAL EXAMPLE 2
After metal oxide materials (ITO) being deposited on glass substrate (100mm × 100mm) and copper being deposited upon on above-mentioned layer, by photolithography, the photoresist material with required pattern is formed on substrate.Then, use respectively in embodiment 6 to embodiment 11 and comparing embodiment 5 to every kind of prepared composition in comparing embodiment 10, the metal level based on copper is carried out to etch process.
Use the equipment (model name: ETCHER(TFT) of injection etching pattern, SEMES company), and be maintained at the etching agent composite of during etching at the temperature of approximately 30 DEG C.But, if needed, can, according to other processing condition and other factors, suitably change temperature.Etching is carried out approximately 100 seconds conventionally, and this time can change according to etch temperature.During etch process the profile of the etched metal level based on copper adopt section S EM(by the manufacturing of Hitachi company, model name: S-4700) detect, detected result is as shown in table 4 below.
< evaluates the standard > of etching outline
60 ° of zero: 35 °≤cone angle <
△: 35 ° of 30 °≤cone angle <; Or 60 °≤cone angle≤65 °
Х: cone angle≤30 ° or cone angle >65 °
Unetched: not etching
< is for evaluating the standard > of etching planeness
Zero: straight pattern
△: 20% or be less than 20% bending pattern
Х: exceed 20% bending pattern
Unetched: not etching
[table 4]
As shown in table 4, the etching agent composite in embodiment 6 to embodiment 11 all presents favourable etch features.
But, the content concn of the persulphate that the content concn of the persulphate having in comparing embodiment 5(comparing embodiment 5 has lower than the present invention), the etching of copper layer is impossible; There is a large amount of persulphates in comparing embodiment 6(comparing embodiment 6), confirm to occur over etching situation.In addition, there is a small amount of azole compounds in comparing embodiment 7(comparing embodiment 7), confirm to occur over etching situation.In addition, there is a large amount of azole compounds in comparing embodiment 8(comparing embodiment 8), the etching of copper layer is impossible.In addition, there is a large amount of organic (peroxide) acid or its salt in comparing embodiment 9(comparing embodiment 9), confirm over etching situation, and there is a small amount of organic (peroxide) acid or its salt in comparing embodiment 10(comparing embodiment 10), etching speed is low and etching outline is poor.
3-1. embodiment 12 to embodiment 17 and comparing embodiment 11 are to comparing embodiment 16
According to the component of listing in following table 5, to comparing embodiment 16, prepare etching agent composite (unit: with respect to the weight percent of total weight percent 100%) at embodiment 12 to embodiment 17 and comparing embodiment 11.
[table 5]
3-2. EXPERIMENTAL EXAMPLE 3
After metal oxide materials (ITO) being deposited on glass substrate (100mm × 100mm) and copper being deposited upon on above-mentioned layer, by photolithography, the photoresist material with required pattern is formed on substrate.Then, use respectively in embodiment 12 to embodiment 17 and comparing embodiment 11 to every kind of prepared composition in comparing embodiment 16, the metal level based on copper is carried out to etch process.
Use the equipment (model name: ETCHER(TFT) of injection etching pattern, SEMES company), and be maintained at the etching agent composite of during etching at the temperature of approximately 30 DEG C.But, if needed, can, according to other processing condition and other factors, suitably change temperature.Etching is carried out approximately 100 seconds conventionally, and this time can change according to etch temperature.During etch process the profile of the etched metal level based on copper adopt section S EM(by the manufacturing of Hitachi company, model name: S-4700) detect, detected result is as shown in table 6 below.
< evaluates the standard > of etching outline
60 ° of zero: 35 °≤cone angle <
△: 35 ° of 30 °≤cone angle <; Or 60 °≤cone angle≤65 °
Х: cone angle≤30 ° or cone angle >65 °
Unetched: not etching
< is for evaluating the standard > of etching planeness
Zero: straight pattern
△: 20% or be less than 20% bending pattern
Х: exceed 20% bending pattern
Unetched: not etching
[table 6]
As shown in table 6, the etching agent composite in embodiment 12 to embodiment 17 all presents favourable etch features.
But, the content concn of the persulphate that the content concn of the persulphate having in comparing embodiment 11(comparing embodiment 11 has lower than the present invention), the etching of copper layer is impossible; There is a large amount of persulphates in comparing embodiment 12(comparing embodiment 12), confirm to occur over etching situation.In addition, there is a small amount of azole compounds in comparing embodiment 13(comparing embodiment 13), confirm to occur over etching situation.In addition, there is a large amount of azole compounds in comparing embodiment 14(comparing embodiment 14), the etching of copper layer is impossible.In addition, there is a small amount of phosphonate compound in comparing embodiment 15(comparing embodiment 15), etching speed is low and etching outline is poor; And there is a large amount of phosphonate compounds in comparing embodiment 16(comparing embodiment 16), confirm to occur over etching situation.
4-1. embodiment 18 to embodiment 23 and comparing embodiment 17 are to comparing embodiment 22
According to the component of listing in following table 7, to comparing embodiment 22, prepare etching agent composite (unit: with respect to the weight percent of total weight percent 100%) at embodiment 18 to embodiment 23 and comparing embodiment 17.
[table 7]
4-2. EXPERIMENTAL EXAMPLE 4
After metal oxide materials (ITO) being deposited on glass substrate (100mm × 100mm) and copper being deposited upon on above-mentioned layer, by photolithography, the photoresist material with required pattern is formed on substrate.Then, use respectively in embodiment 18 to embodiment 23 and comparing embodiment 17 to every kind of prepared composition in comparing embodiment 22, the metal level based on copper is carried out to etch process.
Use the equipment (model name: ETCHER(TFT) of injection etching pattern, SEMES company), and be maintained at the etching agent composite of during etching at the temperature of approximately 30 DEG C.But, if needed, can, according to other processing condition and other factors, suitably change temperature.Etching is carried out approximately 100 seconds conventionally, and this time can change according to etch temperature.During etch process the profile of the etched metal level based on copper adopt section S EM(by the manufacturing of Hitachi company, model name: S-4700) detect, and detected result is as shown in table 8 below.
< evaluates the standard > of etching outline
Zero: 35 °≤cone angle≤60 °
△: cone angle <35 ° or cone angle >60 °
Х: undercutting or back taper
Unetched: not etching
< is for evaluating the standard > of etching planeness
Zero: straight pattern
△: 20% or be less than 20% bending pattern
Х: exceed 20% bending pattern
Unetched: not etching
[table 8]
As shown in table 8, the etching agent composite in embodiment 18 to 23 all presents favourable etch features.But, the content concn of the persulphate that the content concn of the persulphate having in comparing embodiment 17(comparing embodiment 17 has lower than the present invention), the etching of copper layer is impossible; There is a large amount of persulphates in comparing embodiment 18(comparing embodiment 18), confirm to occur over etching situation.In addition, there is a small amount of azole compounds in comparing embodiment 19(comparing embodiment 19), confirm to occur over etching situation.In addition, there is a large amount of azole compounds in comparing embodiment 20(comparing embodiment 20), the etching of copper layer is impossible.In addition, there is a small amount of mineral acid or its salt in comparing embodiment 21(comparing embodiment 21), etching outline and planeness are poor; And there is a large amount of mineral acids or its salt in comparing embodiment 22(comparing embodiment 22), because Cu pattern degree of lacking appears in photoresist material (PR) rise phenomenon.
5-1. embodiment 24 to embodiment 29 and comparing embodiment 23 are to comparing embodiment 28
According to the component of listing in following table 9, to comparing embodiment 28, prepare etching agent composite (unit: with respect to the weight percent of total weight percent 100%) at embodiment 24 to embodiment 29 and comparing embodiment 23.
[table 9]
5-2. EXPERIMENTAL EXAMPLE 5
After metal oxide materials (ITO) being deposited on glass substrate (100mm × 100mm) and copper being deposited upon on above-mentioned layer, by photolithography, the photoresist material with required pattern is formed on substrate.Then, use respectively in embodiment 24 to embodiment 29 and comparing embodiment 23 to every kind of prepared composition in comparing embodiment 28, the metal level based on copper is carried out to etch process.
Use the equipment (model name: ETCHER(TFT) of injection etching pattern, SEMES company), and be maintained at the temperature of approximately 30 DEG C at during etching etching agent composite.But, if needed, can, according to other processing condition and other factors, suitably change temperature.Etching is carried out approximately 100 seconds conventionally, and this time can change according to etch temperature.During etch process the profile of the etched metal level based on copper adopt section S EM(by the manufacturing of Hitachi company, model name: S-4700) detect, and detected result is as shown in table 10 below.
< evaluates the standard > of etching outline
60 ° of zero: 35 °≤cone angle <
△: 35 ° of 30 °≤cone angle <; Or 60 °≤cone angle≤65 °
Х: cone angle≤30 ° or cone angle >65 °
Unetched: not etching
< is for evaluating the standard > of etching planeness
Zero: straight pattern
△: 20% or be less than 20% bending pattern
Х: exceed 20% bending pattern
Unetched: not etching
[table 10]
As shown in table 10, the etching agent composite in embodiment 24 to embodiment 29 all presents favourable etch features.
But, the content concn of the persulphate that the content concn of the persulphate having in comparing embodiment 23(comparing embodiment 23 has lower than the present invention), the etching of copper layer is impossible; There is a large amount of persulphates in comparing embodiment 24(comparing embodiment 24), confirm to occur over etching situation.In addition, there is a small amount of azole compounds in comparing embodiment 25(comparing embodiment 25), confirm to occur over etching situation.In addition, there is a large amount of azole compounds in comparing embodiment 26(comparing embodiment 26), the etching of copper layer is impossible.In addition, there is a large amount of sulfonic acid or its salt in comparing embodiment 27(comparing embodiment 27), over etching situation be there is; And there is a small amount of sulfonic acid or its salt in comparing embodiment 28(comparing embodiment 28), etching speed is low and etching outline is poor.
6-1. embodiment 30 to embodiment 35 and comparing embodiment 29 are to comparing embodiment 34
According to the component of listing in following table 11, to comparing embodiment 34, prepare etching agent composite (unit: with respect to the weight percent of total weight percent 100%) at embodiment 30 to embodiment 35 and comparing embodiment 29.
[table 11]
6-2. EXPERIMENTAL EXAMPLE 6
After metal oxide materials (ITO) being deposited on glass substrate (100mm × 100mm) and copper being deposited upon on above-mentioned layer, by photolithography, the photoresist material with required pattern is formed on substrate.Then, use respectively in embodiment 30 to embodiment 35 and comparing embodiment 29 to every kind of prepared composition in comparing embodiment 34, the metal level based on copper is carried out to etch process.
Use the equipment (model name: ETCHER(TFT) of injection etching pattern, SEMES company), and be maintained at the temperature of approximately 30 DEG C at during etching etching agent composite.But, if needed, can, according to other processing condition and other factors, suitably change temperature.Etching is carried out approximately 100 seconds conventionally, and this time can change according to etch temperature.During etch process the profile of the etched metal level based on copper adopt section S EM(by the manufacturing of Hitachi company, model name: S-4700) detect, and detected result is as shown in table 12 below.
< evaluates the standard > of etching outline
Zero: 35 °≤cone angle≤60 °
△: cone angle <35 ° or cone angle >60 °
Х: undercutting or back taper
Unetched: not etching
< is for evaluating the standard > of etching planeness
Zero: straight pattern
△: 20% or be less than 20% bending pattern
Х: exceed 20% bending pattern
Unetched: not etching
[table 12]
As shown in table 12, the etching agent composite in embodiment 30 to embodiment 35 all presents favourable etch features.
But, the content concn of the persulphate that the content concn of the persulphate having in comparing embodiment 29(comparing embodiment 29 has lower than the present invention), the etching of copper layer is impossible; There is a large amount of persulphates in comparing embodiment 30(comparing embodiment 30), confirm to occur over etching situation.In addition, there is a small amount of azole compounds in comparing embodiment 31(comparing embodiment 31), confirm to occur over etching situation.In addition, there is a large amount of azole compounds in comparing embodiment 32(comparing embodiment 32), the etching of copper layer is impossible.In addition, there is a large amount of mantoquitas in comparing embodiment 33(comparing embodiment 33), etching outline and planeness variation; And there is a small amount of mantoquita in comparing embodiment 34(comparing embodiment 34), because etching outline and planeness variation also appear in low etching speed.

Claims (25)

1. for an etching agent composite for the metal level based on copper, comprising: persulphate, 0.1 azole compounds of % by weight to 5 % by weight and the water of surplus of 0.5 % by weight to 20 % by weight.
2. etching agent composite according to claim 1, wherein, described persulphate is to be selected from Potassium Persulphate (K 2s 2o 8), Sodium Persulfate (Na 2s 2o 8) and ammonium persulphate ((NH 4) 2s 2o 8) at least one.
3. etching agent composite according to claim 1, wherein, described azole compounds is at least one being selected from triazole compounds, amino tetrazole compound, imidazolium compounds, benzazolyl compounds, purine compound, pyrazole compound, pyridine compounds, pyrimidine compound, azole compounds, pyrrolidine compound and pyrrolinium compound.
4. etching agent composite according to claim 1, also comprises: organic (peroxide) acid or its salt of 1 % by weight to 5 % by weight.
5. etching agent composite according to claim 4, wherein, described organic (peroxide) acid is at least one being selected from Peracetic Acid, benzoyl hydroperoxide, acetic acid, butyric acid, citric acid, formic acid, gluconic acid, oxyacetic acid, propanedioic acid, valeric acid and oxalic acid.
6. etching agent composite according to claim 4, wherein, the salt of described organic (peroxide) acid is at least one in the sodium salt of the sylvite that is selected from organic (peroxide) acid, organic (peroxide) acid and the ammonium salt of organic (peroxide) acid.
7. etching agent composite according to claim 1, also comprises the phosphonate compound of 3 % by weight to 15 % by weight.
8. etching agent composite according to claim 7, wherein, described phosphonate compound is to be selected from phosphoric acid, 2-amino-ethyl phosphonic acids, dimethyl methyl phosphonate, 1-hydroxy ethylene-1, 1-di 2 ethylhexyl phosphonic acid, amino three (methylene phosphonic acids), EDTMP, tetramethylene-diamine four (methylene phosphonic acid), hexamethylene-diamine four (methylene phosphonic acid), diethylene triamine penta(methylene phosphonic acid), phosphonic acids butane-tricarboxylic acid, N-((phosphonomethyl)) iminodiethanoic acid, 2-propyloic phosphonic acids, at least one in 2-hydroxy phosphinylidyne yl carboxylic acid and amino-tri--(methylene phosphonic acid).
9. etching agent composite according to claim 7, wherein, described phosphonate compound is at least one in sylvite, the sodium salt of phosphonate compound and the ammonium salt of phosphonate compound that is selected from phosphonate compound.
10. etching agent composite according to claim 1, also comprises: the mineral acid of 0.5 % by weight to 3 % by weight or its salt, wherein, except persulphate.
11. etching agent composites according to claim 10, wherein, described mineral acid is at least one being selected from nitric acid, sulfuric acid, phosphoric acid, boric acid and perchloric acid.
12. etching agent composites according to claim 10, wherein, the salt of described mineral acid is at least one in sylvite, the sodium salt of mineral acid and the ammonium salt of mineral acid that is selected from mineral acid, wherein, except persulphate.
13. etching agent composites according to claim 1, also comprise sulfonic acid or its salt of 0.5 % by weight to 5 % by weight.
14. etching agent composites according to claim 13, wherein, described sulfonic acid is at least one being selected from thionamic acid, methylsulphonic acid, ethylsulfonic acid, tosic acid, trifluoromethanesulfonic acid, Phenylsulfonic acid, thionamic acid and polystyrolsulfon acid.
15. etching agent composites according to claim 13, wherein, the salt of described sulfonic acid is at least one being selected from sylvite, sodium salt and ammonium salt.
16. etching agent composites according to claim 1, also comprise the mantoquita of 0.5 % by weight to 3 % by weight, wherein, and except persulphate.
17. etching agent composites according to claim 16, wherein, described mantoquita is at least one being selected from copper sulfate, cupric nitrate, cupric chloride, venus crystals and cupric fluoride.
18. etching agent composites according to claim 1, wherein, form the described metal level based on copper, and the described metal level based on copper comprises: be selected from least one in copper, copper nitride and cupric oxide; Or comprise at least one and the alloy that is selected from least one metal in aluminium (Al), magnesium (Mg), calcium (Ca), titanium (Ti), silver (Ag), chromium (Cr), manganese (Mn), iron (Fe), zirconium (Zr), niobium (Nb), molybdenum (Mo), palladium (Pd), hafnium (Hf), tantalum (Ta) and tungsten (W) of being selected from copper, copper nitride and cupric oxide.
19. etching agent composites according to claim 18, wherein, the described metal level based on copper comprises: copper molybdenum layer, the metal level based on copper that described copper molybdenum layer has molybdenum layer and forms on described molybdenum layer; Or copper molybdenum alloy layer, the metal level based on copper that described copper molybdenum alloy layer has molybdenum alloy layer and forms on described molybdenum alloy layer.
20. 1 kinds are used to form the method for wiring, comprise:
(S1) on substrate, form metal oxide layer;
(S2) on described metal oxide layer, form the metal level based on copper;
(S3) on the described metal level based on copper, form photoetching agent pattern alternatively; With
(S4) by using according to the etching agent composite described in any one in claim 1 to 19, the only described metal level based on copper on metal oxide layer described in etching.
21. methods according to claim 20, wherein, form described metal oxide layer, and described metal oxide layer comprises: pass through A xb yc zthe three-component system oxide compound that O represents or four component system oxide compounds, wherein, A, B and C are respectively the metals that is selected from zinc (Zn), titanium (Ti), cadmium (Cd), gallium (Ga), indium (In), tin (Sn), hafnium (Hf), zirconium (Zr) and tantalum (Ta); X, y and z all represent metal ratio and are 0 or are greater than 0 integer or prime number.
22. methods according to claim 20, wherein, form the described metal level based on copper, and the described metal level based on copper comprises: be selected from least one in copper, copper nitride and cupric oxide; Or comprise at least one and the alloy that is selected from least one metal in aluminium (Al), magnesium (Mg), calcium (Ca), titanium (Ti), silver (Ag), chromium (Cr), manganese (Mn), iron (Fe), zirconium (Zr), niobium (Nb), molybdenum (Mo), palladium (Pd), hafnium (Hf), tantalum (Ta) and tungsten (W) of being selected from copper, copper nitride and cupric oxide.
23. methods according to claim 22, wherein, the described metal level based on copper comprises: copper molybdenum layer, the metal level based on copper that described copper molybdenum layer has molybdenum layer and forms on described molybdenum layer; Or copper molybdenum alloy layer, the metal level based on copper that described copper molybdenum alloy layer has molybdenum alloy layer and forms on described molybdenum alloy layer.
24. 1 kinds of manufactures are used for the method for the array substrate of liquid crystal indicator, comprising:
A) on substrate, form grid wiring;
B) on the described substrate that comprises described grid wiring, form gate insulator;
C) on described gate insulator, form semiconductor layer;
D) on described semiconductor layer, form source wiring and drain electrode wiring; With
E) form the pixel electrode that is connected to described drain electrode wiring,
Wherein, described a) step comprises: on described substrate, form the metal level based on copper, and use according to the metal level based on copper described in the etching agent composite etching described in any one in claim 1 to 19 to form described grid wiring.
25. 1 kinds of manufactures are used for the method for the array substrate of liquid crystal indicator, comprising:
A) on substrate, form grid wiring;
B) on the described substrate that comprises described grid wiring, form gate insulator;
C) on described gate insulator, form semiconductor layer;
D) on described semiconductor layer, form source wiring and drain electrode wiring; With
E) form the pixel electrode that is connected to described drain electrode wiring,
Wherein said d) step comprises: on described semiconductor layer, form the metal level based on copper, and use according to the metal level based on copper described in the etching agent composite etching described in any one in claim 1 to 19 to form described source wiring and described drain electrode wiring.
CN201410123681.0A 2013-03-28 2014-03-28 Etching composition for copper-based metal layer and method of preparing metal line Pending CN104073803A (en)

Applications Claiming Priority (12)

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KR1020130033687A KR20140119885A (en) 2013-03-28 2013-03-28 Etching composition for copper-based metal layer and method of preparing metal line
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CN105887091A (en) * 2015-02-16 2016-08-24 东友精细化工有限公司 Etchant Composition For Ag Thin Layer And Method For Fabricating Metal Pattern Using The Same And Method For Fabricating Array Substrate By Using The Same
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CN110819991A (en) * 2019-11-08 2020-02-21 日月光半导体(上海)有限公司 Etching solution and method for manufacturing package substrate using same
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WO2016041407A1 (en) * 2014-09-15 2016-03-24 南通万德科技有限公司 Etching solution and application thereof
CN107004719B (en) * 2014-11-28 2020-07-03 夏普株式会社 Semiconductor device and method of manufacturing the same
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US10748939B2 (en) 2014-11-28 2020-08-18 Sharp Kabushiki Kaisha Semiconductor device formed by oxide semiconductor and method for manufacturing same
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CN104480469B (en) * 2014-12-12 2018-02-23 江阴润玛电子材料股份有限公司 A kind of TFT copper-molybdenums stacked film etchant and engraving method
CN105734570A (en) * 2014-12-26 2016-07-06 三星显示有限公司 Etchant composition and method for manufacturing metal wiring using the same
CN105887091A (en) * 2015-02-16 2016-08-24 东友精细化工有限公司 Etchant Composition For Ag Thin Layer And Method For Fabricating Metal Pattern Using The Same And Method For Fabricating Array Substrate By Using The Same
CN105887091B (en) * 2015-02-16 2020-05-26 东友精细化工有限公司 Etchant composition for silver thin layer, method of forming metal pattern using the same, and method of fabricating array substrate using the same
CN104947109A (en) * 2015-07-09 2015-09-30 湖南城市学院 Etching solution for micro-ultrasonic machining assistance and preparation method thereof
CN106555187B (en) * 2015-09-22 2019-12-17 东友精细化工有限公司 Etchant composition, etching method of copper-based metal layer, array substrate manufacturing method and array substrate manufactured by the method
CN106555187A (en) * 2015-09-22 2017-04-05 东友精细化工有限公司 The array base palte that etching agent composite, the engraving method of copper base metal layer, array substrate manufacturing method and the method make
CN107587135A (en) * 2016-07-08 2018-01-16 深圳新宙邦科技股份有限公司 A kind of molybdenum aluminium-molybdenum etching liquid
CN112680228A (en) * 2019-10-18 2021-04-20 三星Sdi株式会社 Etching composition for silicon nitride layer and method for etching silicon nitride layer using the same
US11254871B2 (en) 2019-10-18 2022-02-22 Samsung Sdi Co., Ltd. Etching composition for silicon nitride layer and method of etching silicon nitride layer using the same
CN112680228B (en) * 2019-10-18 2022-04-19 三星Sdi株式会社 Etching composition for silicon nitride layer and method for etching silicon nitride layer using the same
CN110819991A (en) * 2019-11-08 2020-02-21 日月光半导体(上海)有限公司 Etching solution and method for manufacturing package substrate using same
CN110819991B (en) * 2019-11-08 2022-07-15 日月光半导体(上海)有限公司 Etching solution and manufacturing method of package substrate using the same
CN111876780A (en) * 2020-08-31 2020-11-03 武汉迪赛新材料有限公司 Ammonium persulfate system etching solution for etching TFT copper-molybdenum layer
CN112080747A (en) * 2020-09-02 2020-12-15 Tcl华星光电技术有限公司 Etching solution composition for etching molybdenum/copper/molybdenum or molybdenum alloy/copper/molybdenum alloy three-layer metal wiring structure and application thereof
CN114807942A (en) * 2022-03-07 2022-07-29 上海富柏化工有限公司 Sodium persulfate microetching additive and application thereof
CN114807942B (en) * 2022-03-07 2024-02-13 上海富柏化工有限公司 Sodium persulfate microetching additive and application thereof
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CN115161641B (en) * 2022-07-08 2024-06-11 苏州迈为科技股份有限公司 Etching solution additive, etching solution, application of etching solution and etching process

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