CN100348709C - Aqueous cleaning composition for semiconductor copper process - Google Patents
Aqueous cleaning composition for semiconductor copper process Download PDFInfo
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- CN100348709C CN100348709C CNB2005100721364A CN200510072136A CN100348709C CN 100348709 C CN100348709 C CN 100348709C CN B2005100721364 A CNB2005100721364 A CN B2005100721364A CN 200510072136 A CN200510072136 A CN 200510072136A CN 100348709 C CN100348709 C CN 100348709C
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Abstract
本发明涉及一种用于集成电路处理中化学机械平坦化后的含铜导线晶圆的水相清洗组合物，其包括0.1-15重量%含氮杂环类有机碱、0.1-35重量%醇胺和水。与经化学机械平坦化后的含铜半导体晶圆接触一段有效时间后，本发明的水相清洗组合物可以有效地去除残留在晶圆表面上的污染物，同时维持含铜半导体晶圆优选的表面粗糙度。
The present invention relates to an aqueous cleaning composition for copper-containing conductor wafers after chemical mechanical planarization in integrated circuit processing, which comprises 0.1-15 wt % of nitrogen-containing heterocyclic organic base, 0.1-35 wt % of alcohol amine and water. After being in contact with the copper-containing semiconductor wafer after chemical mechanical planarization for an effective period of time, the aqueous cleaning composition of the present invention can effectively remove pollutants remaining on the wafer surface while maintaining the preferred surface roughness of the copper-containing semiconductor wafer.
Description
Technical field
The present invention relates to a kind of aqueous phase cleaning composition that is used for after unicircuit is handled chemical-mechanical planarization (CMP).
Background technology
About semiconductor element, just develop now towards the direction of littler live width, higher effective density.When the unicircuit minimum feature was reduced to below 0.25 micron, resistance and the caused time lag of dielectric layer stray capacitance (RC delay) by plain conductor itself had become the main key that influences the element arithmetic speed.Therefore, in order to improve the arithmetic speed of element, the dealer changes into gradually in the high-order processing procedure below 0.13 micron and adopts the copper plain conductor to replace traditional aluminum-copper alloy lead at present.
The technology of chemical-mechanical planarization (Chemical Mechanical Planarization) is applied in the copper plain conductor processing procedure, not only can overcome the problem that is difficult to define pattern that causes because be not easy to carry out the copper metal etch, and after grinding is the plane of a global planarization (global planarity), is easy to the carrying out of multi-layer conductor leads processing procedure.The principle of chemical-mechanical planarization is to match with chemical assistant by the abrasive grains in the lapping liquid, make crystal column surface is produced mechanical wear, thereby make the smooth higher position of air spots remove speed because of pressurized produces height greatly, the smooth lower of air spots then has because of pressurized is little and removes speed more slowly, thereby realizes the purpose of global planarization.
In the process of lapping of chemical-mechanical planarization, the chip of being peeled off in a large amount of fine ground particle in the lapping liquid and chemical assistant and the process of lapping may be attached to chip surface.General chip common pollutent after grinding is metal ion, organic compound or abrasive grains etc.If there is not effective wash procedure to remove above-mentioned pollutent, will influence the carrying out of successive process and the yield and the reliability of reduction element so.Therefore, can CMP grinds the back manufacturing process for cleaning, become the gordian technique that successfully CMP is applied to manufacture of semiconductor.
The lapping liquid that is used for copper wiring is many can use benzotriazole (benzotriazole, BTA), its derivative and anti-vitamin C deficiency acid etc. are as corrosion inhibitor.In the pollutent behind the copper wiring grinding wafer, be difficult to most remove with organic residues such as BTA, major cause for the BTA particulate be with chemisorption mode bond to copper conductor.Tradition only utilizes electrostatic repulsion, ultrasonic oscillation and polyvinyl alcohol (PVA) brush the mode of physical removal such as to scrub, and does not have excellent cleaning effect.
Between tradition stratum/metal intermetallic dielectric layer (inter layer/metal dielectric) and tungsten plug (Wplug) be behind chemical-mechanical planarization, often use ammonia soln and/or fluorochemicals to clean, but above-mentioned solution and be not suitable for the wafer of copper plain conductor.Ammonia soln can corrode copper metallic face unevenly, and causes the phenomenon of roughening.Fluorochemicalss such as hydrofluoric acid then not only can make roughened copper surfaceization, and for avoiding its harmful to human and environment, need paying more costs aspect personnel safety guard and the liquid waste disposal.
People's such as Ina United States Patent (USP) discloses a kind of abrasive composition that can remove the tantalum metal effectively from base material No. 6139763, is made up of the reductive agent (as oxalic acid) and the water of abrasive grain, the oxygenant of oxidable tantalum metal, reducible tantalum oxide.This abrasive composition can further comprise six hydrogen piperazines (piperazine, a kind of nitrogen heterocyclic ring organic bases).Instruction according to people such as Ina; six hydrogen piperazines can act in process of lapping on the copper laminar surface, and in order to the generation that prevents surface damage-as subside (recesses), dish falls into (dishing) or abrasion (erosion); it can also protect lapped face, to impel the surface of finishing as the minute surface.People such as Ina do not lecture or advise six hydrogen piperazines to be used for the water scavenging solution of copper wiring post-chemical mechanical planarization.
The United States Patent (USP) the 6th of Small, 546, No. 939 (No. the 396202nd, Republic of China's patent) discloses a kind of method from metal or dielectric layer surface removal chemical residue, and it is between enough time of removal chemical residue of 3.5 to 7 waterborne compositions contacting metal or dielectric layer surface one with a pH.This waterborne compositions comprises: the alkali of a kind of organic acid of single, double or trifunctional base, quaternary ammonium compound, ammonium hydroxide, azanol, hydroxylammonium salt or the diamine salt of a buffering capacity, and bursine (choline hydroxide).
People's such as Small United States Patent (USP) the 6th, 498, disclose a kind of clean-out system No. 131, form by non-ionic interfacial agent, amine, quaternary ammonium compound and the surperficial setting-up agent that is selected from ethylene glycol, propylene glycol, polyoxyethylene and its mixture, in order to clean the resistates of chemical mechanical planarization.
People's such as Naghshineh United States Patent (USP) discloses a kind of clean-out system the 6th, 492, No. 308, is made up of tetra-alkyl ammonium hydroxide, polarity organic amine and corrosion inhibitor, contains copper integrated circuit in order to cleaning.
The United States Patent (USP) of Nam discloses a kind of clean-out system the 5th, 863, No. 344, is made up of Tetramethylammonium hydroxide, acetate and water, and in order to clean semiconductor components, wherein preferred acetate is 1 to about 50 to the Tetramethylammonium hydroxide volumetric ratio.
People's such as Masahiko United States Patent (USP) discloses a kind of cleaning for the 6th, 716, No. 803 and has the method for copper conductor at its surperficial semiconductor substrate, and the clean-out system that described method is used comprises interfacial agent and nitrogenous alkaline matter.
People's such as Ward United States Patent (USP) discloses a kind of clean-out system the 5th, 988, No. 186, is made up of water soluble polar solvent, organic amine and phenyl ring corrosion inhibitor, in order to remove the organic or inorganic material.
Above-mentioned prior art is all used tetra-alkyl ammonium hydroxide and/or interfacial agent and/or the corrosion inhibitor component as scavenging solution.Tetra-alkyl ammonium hydroxide volatile (20 ℃ of following vapour pressures are about 18mmHg), toxicity height and the strong amine stink of tool will not work the mischief to personnel and environment if properly do not manage.In addition, add the clean effect that interfacial agent maybe can be promoted cleaning combination by the surface electrical behavior that changes pollutent and/or base material, but, then can't bring into play its effect for the pollutent that exists in the chemisorption mode.On the other hand; corrosion inhibitor is to provide protection to copper metallic face in cleaning process; avoiding copper metallic face to be cleaned that chemical substance too corrodes in the composition, but corrosion inhibitor itself may residue in copper metallic face after cleaning, cause the problem of organic substance residues.
Therefore, above-mentioned prior art still can't satisfy the scavenging solution demand of industrial community for the planarization of copper wiring post-chemical mechanical.Still need a kind of aqueous phase cleaning composition that can be used for the planarization of copper wiring post-chemical mechanical, this composition is not volatile, do not have a stink, cleaning the back composition itself does not remain on the wafer, and can remove the pollutent that remains on the copper wiring chip surface behind the chemical-mechanical planarization effectively, and make the copper plain conductor keep preferred surfaceness.
Summary of the invention
Main purpose of the present invention is to provide a kind of aqueous phase cleaning composition that is used for the planarization of copper wiring post-chemical mechanical, and it comprises nitrogen heterocyclic ring organic bases, hydramine and water.Contact one period working lipe with aqueous phase cleaning composition of the present invention with cupric semiconductor crystal wafer after chemical-mechanical planarization grinds, can remove the pollutent that remains in after the grinding on the crystal column surface effectively, keep the preferred surfaceness of copper conductor simultaneously.
Characteristics of the present invention are to avoid using volatile components such as tetra-alkyl ammonium hydroxide (as, Tetramethylammonium hydroxide), can reduce the potential hazard of solution loss to environment and HUMAN HEALTH.Another characteristics of the present invention are; need not use interfacial agent and be used for the corrosion inhibitor (as BTA and/or its derivative and anti-vitamin C deficiency acid etc.) that cleaning process is protected copper metallic face; promptly can remove the pollutent that remains in after the grinding on the crystal column surface effectively; keep the preferred surfaceness of copper conductor simultaneously, thereby can avoid interfacial agent and corrosion inhibitor to remain in risk on the wafer.
Description of drawings
Fig. 1: atomic force microscope (AFM) photo of copper chip after cleaning combination of the present invention (numbering 1) cleans.
Fig. 2: atomic force microscope (AFM) photo of copper chip after improper cleaning combination (numbering 12) cleans.
Embodiment
Aqueous phase cleaning composition of the present invention in composition total weight, comprises the nitrogen heterocyclic ring organic bases of 0.1-15 weight %, hydramine and the water of 0.1-35 weight %.
Be to use the basicity of nitrogen heterocyclic ring organic bases in the cleaning combination of the present invention, and then avoid use can cause the alkali metal group oxyhydroxide of the ammoniacal liquor of the serious roughening in copper surface, volatile Tetramethylammonium hydroxide and serious metal ion pollution with the increase composition.On the other hand, the not share electron pair of nitrogen can carry out bond with copper conductor on the heterocycle of nitrogen heterocyclic ring organic bases, thereby the organic pollutant of avoiding breaking away from copper conductor is gone back by absorption again.
Nitrogen heterocyclic ring organic bases used in the present invention, the preferable group that six hydrogen piperazines, 2-(1-six hydrogen piperazines) ethanol, 2-(1-six hydrogen piperazines) ethamine and its combination are formed, the more preferably six hydrogen piperazines of being selected from.The content of nitrogen heterocyclic ring organic bases used in the present invention with the total restatement of composition, is 0.1-15 weight %, is preferably 0.1-10 weight %, more preferably 0.2-10 weight %.
Hydramine used in the present invention is preferably selected from the group that thanomin, diethanolamine, trolamine, Propanolamine and its combination are formed, and more preferably is selected from the group that diethanolamine, trolamine and its combination are formed.The content of hydramine used in the present invention with the total restatement of composition, is 0.1-35 weight %, is preferably 0.1-30 weight %, more preferably 0.5-25 weight %.
As previously mentioned, crystal column surface after the employed corrosion inhibitor of the lapping liquid that is used for the copper wiring chemical-mechanical planarization (as BTA, its derivative and anti-vitamin C deficiency acid) can residue in grinding, and the physical method that described organic residue is difficult to only depend on general using electrostatic repulsion, ultrasonic oscillation and polyvinyl alcohol (PVA) brush to scrub is removed.
Nitrogen heterocyclic ring organic bases and alcohol amine compound that cleaning combination of the present invention contained can promote the saturation solubility of cleaning combination to organic residue (as BTA), thereby can provide bigger motivating force with dissolving BTA particulate.With the mode that conventional physical is removed, disclosed cleaning combination is used in collocation, can reach good wash result.
Cleaning combination of the present invention can directly use, or to re-use after the ultrapure water dilution.For saving production, transportation and warehouse cost, the composition of higher concentration is provided usually, use with ultrapure water dilution back in use side again.The multiple of dilution uses situation to determine according to reality, generally between 10 to 60 times.Under the specific demand situation, as saving the treatment time, cleaning combination stoste that can concentration is higher is directly in order to cleaning wafer.
Can use under the cleaning combination normal temperature of the present invention, this cleaning combination is contacted one period working lipe with cupric semiconductor crystal wafer after chemical-mechanical planarization grinds, can remove the pollutent that remains in after the grinding on the crystal column surface effectively, keep the preferred surfaceness of copper conductor simultaneously.Generally speaking, when working concentration is low, need long duration of contact (for example, 1-3 minute), when working concentration is higher, only need short duration of contact (for example, being shorter than 1 minute).When reality is used, can seek cleaning combination concentration and the most appropriate operation between duration of contact by examination mistake mode (try and error).
Following examples will the present invention is further illustrated, and not in order to limit the scope of the invention, modification that any those skilled in the art can realize easily and change are all contained within the scope of the invention.
Embodiment one
With six hydrogen piperazines, diethanolamine and trolamine concentration is the factor (factor), utilize the different cleaning solutions of forming of field mouth formula experimental plan method L8 configuration tool (numbering 1-8), inquire into the effect (numbering 9-12) of composition water, six hydrogen piperazines, diethanolamine and ammoniacal liquor, and measure the copper dissolution ability and the BTA saturation solubility of 40 times of diluents of each composition.
The measurement of copper dissolution ability is that the copper blank wafer is cut into each chip of 1.5 centimeters of length and width, behind the cupric oxide of chip pre-treatment removal top layer, is immersed in 50 milliliters of test solns, takes out chip after one minute, and measures copper ion concentration in the solution with ICP-MS.
The measurement of BTA saturation solubility is that test soln is placed under the environment of 25 ℃ of constant temperature, adds excessive BTA stirring and dissolving in addition, and the insolubles after 4 hours in the filtering test soln is with the BTA concentration in high-performance liquid chromatograph (HPLC) analytical solution.
The copper dissolution ability of table one, different cleaning combinations and BTA saturation solubility
| Numbering | Form | Extension rate | Copper dissolution ability (ppb) | BTA saturation solubility (%) | ||
| Six hydrogen | Diethanolamine | Trolamine | ||||
| 1 | 7.2％ | 9.0％ | 13.5％ | 40 | 25.3 | ?2.76 |
| 2 | 7.2％ | 9.0％ | 20.0％ | 40 | 25.7 | ?2.86 |
| 3 | 10.8％ | 9.0％ | 13.5％ | 40 | 21.1 | ?2.92 |
| 4 | 10.8％ | 9.0％ | 20.0％ | 40 | 23.1 | ?3.02 |
| 5 | 7.2％ | 13.5％ | 13.5％ | 40 | 19.3 | ?2.90 |
| 6 | 7.2％ | 13.5％ | 20.0％ | 40 | 20.6 | ?3.02 |
| 7 | 10.8％ | 13.5％ | 13.5％ | 40 | 20.1 | ?3.08 |
| 8 | 10.8％ | 13.5％ | 20.0％ | 40 | 22.6 | ?3.18 |
| Comparative examples | ||||||
| 9 | Ultrapure water | - | ＜2 | ?2.00 | ||
| 10 | Six hydrogen piperazines 9.0% | 40 | ＜2 | ?2.40 | ||
| 11 | Diethanolamine 16.9% | 40 | 16.0 | ?2.60 | ||
| 12 | Diethanolamine 16.9% ammoniacal liquor 3.0% | 40 | 42.9 | ?3.43 | ||
By the result of above-mentioned composition 9 and 10 as can be known, water and six hydrogen piperazines there is no the ability of dissolve copper metal, and the interpolation of six hydrogen piperazines then can promote the saturation solubility of cleaning compositions to BTA.By the result of above-mentioned composition 11 and 12 as can be known, adding ammoniacal liquor can significantly increase the etching dissolution rate of copper metal and can obviously promote the saturation solubility of cleaning combination to BTA.By the result of above-mentioned composition 1-8 and 11 as can be known, hydramine has the ability of etching dissolve copper metal, also can promote the saturation solubility of cleaning combination to BTA.Copper dissolving metal ability that the cleaning compositions tool is strong more and high more BTA saturation solubility, representing has good more cleaning performance to organic pollutants such as pollutent on the copper metal and BTA, but copper metal etch dissolving power (too fast and/or inhomogeneous) then need be careful the negative impact that roughness causes improperly.
Embodiment two
Cleaning combination shown in the embodiment one is upward cleaned the copper blank wafer that ground in cleaning machine Ontrak, and scavenging period two minutes, clean-out system flow are 600 milliliters of per minutes.After finishing, cleaning measures the surfaceness (average roughness Ra and r.m.s. roughness Rq) of copper wafer with atomic force microscope (AFM).
Table two, the surfaceness of copper wafer after different cleaning combinations clean
| Numbering | Form | Extension rate | Surface roughness Ra (nm) | Surfaceness Rq (nm) | ||
| Six hydrogen | Diethanolamine | Trolamine | ||||
| 1 | 7.2％ | 9.0％ | 13.5％ | 40 | 0.616 | 0.813 |
| 2 | 7.2％ | 9.0％ | 20.0％ | 40 | 0.699 | 0.997 |
| 3 | 10.8％ | 9.0％ | 13.5％ | 40 | 0.663 | 0.888 |
| 4 | 10.8％ | 9.0％ | 20.0％ | 40 | 0.842 | 1.153 |
| 5 | 7.2％ | 13.5％ | 13.5％ | 40 | 0.677 | 0.885 |
| 6 | 7.2％ | 13.5％ | 20.0％ | 40 | 0.714 | 0.945 |
| 7 | 10.8％ | 13.5％ | 13.5％ | 40 | 0.721 | 0.977 |
| 8 | 10.8％ | 13.5％ | 20.0％ | 40 | 0.763 | 0.986 |
| Comparative examples | ||||||
| 9 | Ultrapure water | - | - | - | ||
| 10 | Six hydrogen piperazines 9.0% | 40 | 0.590 | 0.732 | ||
| 11 | Diethanolamine 16.9% | 40 | 0.785 | 1.040 | ||
| 12 | Diethanolamine 16.9% ammoniacal liquor 3.0% | 40 | 9.555 | 15.234 | ||
By relatively numbering 1 and 3 cleaning combinations, to number 1 and 2 cleaning combinations and number 1 and 5 cleaning combinations as can be known, six hydrogen piperazines of more amount and hydramine all can make surfaceness increase, but still keep level preferably.Show that cleaning combination of the present invention not only can the etching dissolve copper metal in extensive concentration range, and can keep good copper metallic face roughness.Result by numbering 12 cleaning compositions can find that ammoniacal liquor can seriously corrode the copper surface, and then causes the roughness result of extreme difference.Result by numbering 10 cleaning compositions can find that six hydrogen piperazines are because itself there is no the ability of etching dissolve copper metal, so fabulous roughness result is still kept on the copper surface after handling.
Embodiment three
The copper blank wafer is immersed in the lapping liquid that is used for copper wiring that contains corrosion inhibitor BTA to be polluted in one minute.After the pollution, at the Rotary drying in addition after 18 seconds of flushing on the cleaning machine Ontrak, measure instrument with TOPCON WM-1700 wafer particulate again and measure the particle number that pollutes on the wafer of back with ultrapure water.The known wafer that pollutes the back particle number was scrubbed on cleaning machine Ontrak two minutes with the different cleaning composition, last and with ultrapure water flushing Rotary drying in addition after 18 seconds, measure instrument with TOPCON WM-1700 wafer particulate once more and measure the particle number that cleans on the wafer of back, so calculate each cleaning compositions to the removal efficient of crystal column surface particulate pollutant.
Table three, cleaning combination are to the removal effect of copper crystal column surface particulate
| Numbering | Original composition | The dilution back is formed | Dilution back pH-value | Pollutants removal rate |
| 10 | Six hydrogen piperazines 9.0% | Six hydrogen piperazines 0.225% | 11.1 | 79.1％ |
| 11 | Diethanolamine 16.9% | Diethanolamine 0.423% | 10.7 | 75.0％ |
| 13 | Six hydrogen piperazines, 9.0% diethanolamine 16.9% | Six hydrogen piperazines, 0.225% diethanolamine 0.423% | 11.2 | 92.1％ |
| 14 | Six hydrogen piperazines, 9.0% trolamine 16.9% | Six hydrogen piperazines, 0.225% trolamine 0.423% | 11.4 | 87.8％ |
| 1 | Six hydrogen piperazines, 7.2% diethanolamine, 9.0% trolamine 13.5% | Six hydrogen piperazines, 0.180% diethanolamine, 0.225% trolamine 0.338% | 11.3 | 94.1％ |
| 8 | Six hydrogen piperazines, 10.8% diethanolamine, 13.5% trolamine 20.0% | Six hydrogen piperazines, 0.270% diethanolamine, 0.338% trolamine 0.500% | 11.4 | 96.7％ |
Can find to use six hydrogen piperazines or hydramine in the cleaning compositions separately and can't obtain good wash result by the result of last table, when six hydrogen piperazines and hydramine use jointly, then can significantly promote cleaning performance.
Claims (6)
1. aqueous phase cleaning composition that is used for the post-chemical mechanical planarization, it comprises the nitrogen heterocyclic ring organic bases of (a) 0.1-15 weight %; (b) hydramine of 0.1-35 weight %; (c) water, wherein said organic bases are to be selected from six hydrogen piperazines, 2-(1-six hydrogen piperazines) ethanol, 2-(1-six hydrogen piperazines) ethamine and its combination, and wherein said hydramine is to be selected from thanomin, diethanolamine, trolamine, Propanolamine and its combination.
2. composition according to claim 1, it comprises the six hydrogen piperazines of (a) 0.1-15 weight %; (b) hydramine of 0.1-35 weight %, described hydramine are to be selected from diethanolamine, trolamine and its combination; (c) water.
3. composition according to claim 1, the consumption of wherein said nitrogen heterocyclic ring organic bases are 0.1-10 weight %.
4. composition according to claim 1, the consumption of wherein said nitrogen heterocyclic ring organic bases are 0.2-10 weight %.
5. composition according to claim 1, the consumption of wherein said hydramine are 0.1-30 weight %.
6. composition according to claim 1, the consumption of wherein said hydramine are 0.5-25 weight %.
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| CN1433567A (en) * | 2000-06-06 | 2003-07-30 | Esc公司 | Post chemical-mechanical planarization (CMP) cleaning composition |
| US20030181342A1 (en) * | 2002-03-25 | 2003-09-25 | Seijo Ma. Fatima | pH buffered compositions useful for cleaning residue from semiconductor substrates |
| WO2004005528A2 (en) * | 2002-07-05 | 2004-01-15 | Nihon New Chrome Co., Ltd. | Pyrophosphoric acid bath for use in copper-tin alloy plating |
| JP2004302463A (en) * | 2003-03-28 | 2004-10-28 | Everlight Chemical Industrial Corp | Chemically amplified photoresist composition |
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2005
- 2005-05-20 CN CNB2005100721364A patent/CN100348709C/en not_active Expired - Lifetime
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020045563A1 (en) * | 1996-10-21 | 2002-04-18 | Basf Aktiengesellschaft | Use of polycationic condensates as color transfer inhibiting and color release reducing additive to detergents and fabric conditioners |
| US6139763A (en) * | 1998-12-01 | 2000-10-31 | Fujimi Incorporated | Polishing composition and polishing method employing it |
| CN1433567A (en) * | 2000-06-06 | 2003-07-30 | Esc公司 | Post chemical-mechanical planarization (CMP) cleaning composition |
| CN1403876A (en) * | 2001-08-31 | 2003-03-19 | 东京应化工业株式会社 | Stripping liquid for photoetching colloid and photoetching colloid stripping method using the same stripping liquid |
| US20030181342A1 (en) * | 2002-03-25 | 2003-09-25 | Seijo Ma. Fatima | pH buffered compositions useful for cleaning residue from semiconductor substrates |
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| JP2004302463A (en) * | 2003-03-28 | 2004-10-28 | Everlight Chemical Industrial Corp | Chemically amplified photoresist composition |
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Granted publication date: 20071114 |
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| CX01 | Expiry of patent term |