CN117304813A - High stability STI CMP polishing fluid with adjustable removal rate selection ratio - Google Patents
High stability STI CMP polishing fluid with adjustable removal rate selection ratio Download PDFInfo
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- CN117304813A CN117304813A CN202311256351.4A CN202311256351A CN117304813A CN 117304813 A CN117304813 A CN 117304813A CN 202311256351 A CN202311256351 A CN 202311256351A CN 117304813 A CN117304813 A CN 117304813A
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- removal rate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- H10P52/402—
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- H10W10/014—
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- H10W10/17—
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention discloses a high-stability STI CMP polishing solution with an adjustable removal rate selection ratio, which is used for STI CMP under the acidic condition of pH=2-6, and comprises the following components in percentage by mass: ceO (CeO) 2 And (3) grinding materials: 0.1wt% to 5wt%; amino acid: 0.1wt% to 4wt%; polyol: 0.5wt% to 6wt%; polyvinyl alcohol: 0.01wt% to 1wt%; a pH regulator; the balance of deionized water; the molecular weight of the polyvinyl alcohol is 1 ten thousand to 10 ten thousand; the amino acid is: glycine, alanine, aspartic acid, glutamic acid, arginine, proline, picolinic acid, nicotinic acid or derivatives thereof; the polyol is: d-sorbitol, mannitol, lactitol and maltitolOne or more of maltotriose alcohol, xylitol, dulcitol, or derivatives thereof. The polishing solution can ensure the stability of the polishing rate within 112 months on the basis of high removal rate selection ratio.
Description
Technical Field
The invention relates to the technical field of Shallow Trench Isolation (STI) Chemical Mechanical Polishing (CMP), in particular to a high-stability STI CMP polishing solution with an adjustable removal rate selection ratio, and the polishing solution basically keeps the stability of the polishing rate within 12 months.
Background
Shallow Trench Isolation (STI) is an important method of isolating active devices in current IC fabrication, creating trenches on the Si substrate around the active elements, and filling with an insulating medium. When the trenches are filled, TEOS may also be deposited over unwanted areas of the wafer. Excess TEOS must be completely removed using Chemical Mechanical Polishing (CMP). Si (Si) 3 N 4 The stop layer is an important part of the process, si 3 N 4 Damage to the underlying epitaxial growth surface during CMP can be prevented.
TEOS and Si pairs in STI CMP 3 N 4 The removal rate is selected to have higher requirement, the TEOS removal rate is required to be higher, and Si is ensured to be removed 3 N 4 The removal rate of the trench oxide is well suppressed, and the purpose is to quickly remove redundant TEOS and ensure that the trench oxide is well protected. CeO (CeO) 2 The abrasive has softer hardness and can be combined with SiO 2 Chemical reaction occurs to form "chemical teeth" and is relatively high in hardness for Si 3 N 4 The removal effect is poor, so CeO is used in the STI CMP polishing solution 2 And (3) grinding materials.
The STI polishing solution to removal rate selectivity has been studied intensively, and most researchers have been on TEOS/Si 3 N 4 High removal rate selection ratios have led to effective research results. Patent CN111378372B adopts CeO 2 The abrasive material is added with acetic acid with a certain concentration under the condition of pH=4.5-4.8, so that the abrasive material has higher silicon dioxide polishing rate and higher silicon dioxide/silicon nitride polishing rate selection ratio, and TEOS and Si are obtained after polishing 3 N 4 The selection ratio of the removal rate is 979-3, the range of the selection ratio studied in the patent is too large, and the removal rate is not controlledRate stability studies were made.
Most of the current patents are mainly directed to TEOS and Si 3 N 4 Is studied for TEOS and Si 3 N 4 Is adjustable within a certain range of the removal rate selection ratio of TEOS and Si 3 N 4 Less is reported for removal rate stability.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the high-stability STI CMP polishing solution with adjustable removal rate selection ratio, which is used in STI CMP and has TEOS/Si 3 N 4 The CMP polishing solution with the higher removal rate selection ratio which can be adjusted within the range of 30-80 can ensure the stability of the polishing rate within 112 months on the basis of the higher removal rate selection ratio.
The invention provides a high-stability STI chemical mechanical polishing solution with adjustable removal rate selection ratio, which is used for STI CMP under acidic condition (pH=2-6), and mainly comprises CeO 2 Abrasive, amino acid, polyalcohol, polyvinyl alcohol, pH regulator and deionized water,
the components are measured according to the mass percentage as follows: ceO (CeO) 2 And (3) grinding materials: 0.1wt% to 5wt%; amino acid: 0.1wt% to 4wt%; polyol: 0.5wt% to 6wt%; polyvinyl alcohol: 0.01wt% to 1wt%; a pH regulator; the balance of deionized water.
The amino acid: glycine, alanine, aspartic acid, glutamic acid, arginine, proline, picolinic acid, nicotinic acid or derivatives thereof.
The polyol: d-sorbitol, mannitol, lactitol, maltitol, maltotriose alcohol, xylitol, dulcitol, or one or more of their derivatives.
The molecular weight of the polyvinyl alcohol is 1 ten thousand to 10 ten thousand, preferably 1 ten thousand to 7 ten thousand, and the polyvinyl alcohol comprises at least one of polyvinyl alcohol 10000, polyvinyl alcohol 20000, polyvinyl alcohol 27000, polyvinyl alcohol 67000, polyvinyl alcohol 89000 or other molecular weight polyvinyl alcohol.
The CeO 2 The abrasive grain diameter of the abrasive is 60-300nm, preferably 80-200nm;
the pH adjusting agents include, but are not limited to: the inorganic or organic acid comprises one or more of nitric acid, phosphoric acid, citric acid, oxalic acid and acetic acid; inorganic or organic base: including one or more of potassium hydroxide, sodium hydroxide, ammonium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, ethanolamine, and diethanolamine.
TEOS/Si using polishing solution 3 N 4 The polishing conditions were:
polishing machine: universal-150B; projectile/dish rotational speed: 87/93rpm; pressure: 2.8psi/3psi; the flow rate is 150ml/min; polishing time: 60s; the prepared polishing liquid was stirred for 40 minutes using a high-speed stirrer (3500 r/min) before polishing.
Compared with the prior art, the invention has the beneficial effects that:
the amino acid according to the present invention has different effects on TEOS removal, and has an inhibitory effect on TEOS removal rate or no inhibitory effect on TEOS removal rate, and has an effect on Si 3 N 4 Inhibition of removal rate; the polyol maintains a substance form in an acidic environment, and inhibits Si while ensuring that the TEOS removal rate is not affected 3 N 4 The amino acid and the polyol cooperate to obtain TEOS/Si within a given doping amount range 3 N 4 The removal rate selection ratio is adjustable within the range of 30-80, and the CeO is cooperatively treated by combining the polyvinyl alcohol 2 The polishing liquid was dispersed so that the polishing liquid could maintain a stable polishing rate for 12 months.
Drawings
FIG. 1 shows TEOS and Si as an embodiment 3 N 4 A schematic representation of removal rate as a function of month number; wherein (a) is a graph of TEOS removal rate versus months, and (b) is Si 3 N 4 The removal rate is plotted against month number.
FIG. 2 shows comparative examples TEOS and Si 3 N 4 A schematic representation of removal rate as a function of month number; wherein,(a) Is a graph of TEOS removal rate versus month number, (b) is Si 3 N 4 The removal rate is plotted against month number.
FIG. 3 shows exemplary di-TEOS and Si 3 N 4 A schematic representation of removal rate as a function of month number; wherein (a) is a graph of TEOS removal rate versus months, and (b) is Si 3 N 4 The removal rate is plotted against month number.
FIG. 4 shows comparative examples of di-TEOS and Si 3 N 4 A schematic representation of removal rate as a function of month number; wherein (a) is a graph of TEOS removal rate versus months, and (b) is Si 3 N 4 The removal rate is plotted against month number.
FIG. 5 shows an example of tri-TEOS and Si 3 N 4 A schematic representation of removal rate as a function of month number; wherein (a) is a graph of TEOS removal rate versus months, and (b) is Si 3 N 4 The removal rate is plotted against month number.
FIG. 6 shows comparative examples of tri-TEOS and Si 3 N 4 A schematic representation of removal rate as a function of month number; wherein (a) is a graph of TEOS removal rate versus months, and (b) is Si 3 N 4 The removal rate is plotted against month number.
FIG. 7 shows four pairs of TEOS and Si of the embodiment 3 N 4 Schematic of the effect of removal rate as a function of month number; wherein (a) is a graph of TEOS removal rate versus months, and (b) is Si 3 N 4 The removal rate is plotted against month number.
FIG. 8 is a graph showing the effect of different molecular weight polyvinyl alcohols on TEOS removal rate as a function of months;
FIG. 9 shows the ratio of polyvinyl alcohols of different molecular weights to Si 3 N 4 Schematic of the effect of removal rate as a function of month number.
Detailed Description
The present invention is further explained below with reference to examples and drawings, but is not to be construed as limiting the scope of the present application.
The invention adds amino acid, polyalcohol and polyvinyl alcohol into polishing solution, and protonated amino group of amino acid, TEOS and Si under acidic condition 3 N 4 The hydrogen bond is formed on the surface and then adsorbed on the surface to form a film, and part of amino acid can inhibit the removal rate of TEOS, but can certainly inhibit Si 3 N 4 Is used for the removal rate of (a). Polyols are prepared from hydroxyl groups and TEOS and Si by protonation in acidic environments 3 N 4 Hydrogen bond is formed on the surface to be adsorbed on the surface for film formation, but the removal rate of TEOS is not affected, and Si is inhibited 3 N 4 Is used for the removal rate of (a). The STI CMP polishing solution with the removal rate selection ratio of 30-80 can be obtained by adjusting the ratio of amino acid to polyalcohol within the given doping amount range, the selection ratio is adjustable within the range, and CeO is cooperatively treated by polyvinyl alcohol 2 The polishing liquid was dispersed so that the polishing liquid could maintain a stable polishing rate over a period of 12 months.
The average particle diameter of cerium oxide in the following examples and comparative examples is in the range of 80 to 100nm and pH 4.0 is exemplified. Experiment one: TEOS and Si 3 N 4 Polishing experiment with removal Rate selection ratio controlled in the range of 30-80
Embodiment one: polishing solution with different picolinic acid contents
Table 1 CeO of example one 2 Composition of polishing liquid
The comparison of the polishing liquid to which only D-sorbitol or only picolinic acid was added is shown in Table 2.
Table 2 CeO of comparative example one 2 Composition of polishing liquid
The experimental results of example one are shown in tables 3 and 4.
Table 3 example one experimental result
Table 4 comparative example one experiment result
As a result of experiments in comparative examples and comparative examples, it was found that the addition of only sorbitol alone did not affect the TEOS removal rate relative to the cerium oxide abrasive alone, and Si was suppressed to some extent 3 N 4 Is used for the removal rate of (a). The addition of only a single picolinic acid can inhibit both TEOS and Si 3 N 4 Removal rate. As is clear from the experimental results of the examples and the comparative examples, the polishing solution of the first example has a single additive polishing solution selection ratio of less than 30, and the polishing solution of the first example has a mixture ratio of TEOS to Si 3 N 4 The ratio of the removal rate is in the range of 30-80, and the variation of the selection ratio can be controlled by controlling the proportion content. The simultaneous presence of three substances of sorbitol, picolinic acid and PVA10000 enables Si to be 3 N 4 The removal rate inhibition of (2) is more obvious, and the selection ratio is improved under the condition of ensuring higher TEOS removal rate, so that the removal rate is in the range of 30-80.
Embodiment two: polishing solution with different glutamic acid contents
Table 5 CeO of example two 2 Composition of polishing liquid
The comparison of glutamic acid alone without the addition of polyol to the polishing liquid is shown in Table 6.
Table 6 CeO of comparative example two 2 Composition of polishing liquid
The experimental results of example two are shown in tables 7 and 8.
Table 7 results of example two experiments
Table 8 comparative example two test results
As a result of experiments in comparative examples and comparative examples, it was found that the polishing liquid containing only glutamic acid was effective against Si 3 N 4 The removal rate suppressing effect is weak, and the selection ratio is below 30. As shown by experimental results, the polishing solution of the second embodiment can reach the ratio of TEOS to Si 3 N 4 The ratio of the removal rate is in the range of 30-80, and the variation of the selection ratio can be controlled by controlling the proportion content. Embodiment III: polishing solution with different nicotinic acid contents
Table 9 CeO of example three 2 Composition of polishing liquid
The comparison of niacin alone in the polishing solutions is shown in table 10, for example.
Table 10 CeO of comparative example three 2 Composition of polishing liquid
The experimental results of example three are shown in tables 11 and 12.
Table 11 results of the example three experiments
Table 12 comparative example three test results
As is clear from the experimental results of examples and comparative examples, the polishing solution containing only a single nicotinic acid has a certain inhibition effect on TEOS and Si 3 N 4 The removal rate was not as suppressed as in example three, and the removal rate selection ratios were all less than 30. As shown by experimental results, the polishing solution in the third embodiment can reach TEOS and Si 3 N 4 The removal rate selection ratio is in the range of 30-80, and the change of the selection ratio can be controlled by controlling the proportioning content in the presence of the polyalcohol and the amino acid.
Embodiment four: polishing liquid with modified polyol
Table 13 CeO of example four 2 Composition of polishing liquid
Table 14 example four experimental results
From example four, it is evident that changing the type of polyol in the range described can also meet the 30-80 selection ratio range described in this patent, suggesting that the selected polyol of the present invention can also meet an adjustable removal rate selection ratio in the 30-80 range.
Experiment II: based on experiment one, polishing rate stability monitoring experiment is established
Fifth embodiment: stability monitoring experiment of example one
As shown in FIGS. 1 and 2, the polishing solution of the first embodiment was used for polishing TEOS and Si in a period of 12 months 3 N 4 The polishing rate stability of (C) was substantially maintained constant, and in comparative example one, the polishing solutions of comparative examples 1-1 and comparative examples 1-2 were used for polishing TEOS and Si in a range of 12 months 3 N 4 The polishing rate stability of (2) was substantially stable, but the selection ratio was less than 30, indicating that the presence of sorbitol increased stability, but the selection of a single material was relatively low, and the remaining comparative example components remained stable to TEOS and Si for only 2 months 3 N 4 Is used for polishing rate stability.
Example six: stability monitoring experiment of example two
As shown in FIGS. 3 and 4, the polishing solution of the second embodiment was used for polishing TEOS and Si in a period of 12 months 3 N 4 The polishing rate stability of (C) was kept substantially stable, the fluctuation was not large, and the polishing liquid composition shown in comparative example II was kept to TEOS and Si for only 2 months 3 N 4 Is used for polishing rate stability.
Embodiment seven: stability monitoring experiment of example three
As shown in FIG. 5, the polishing solution of example III was used for polishing TEOS and Si in a range of 12 months 3 N 4 The polishing rate stability of (c) was substantially maintained stable, and as shown in fig. 6, the polishing liquid composition shown in comparative example three was maintained for only 3 months against TEOS and Si 3 N 4 Is used for polishing rate stability.
Example eight: stability monitoring experiment of example four
The polishing solution of example four shown in FIG. 7 was used for polishing TEOS and Si in a range of 12 months 3 N 4 Is substantially stable.
Example nine: different molecular weight polyvinyl alcohol to TEOS and Si 3 N 4 Is to be used for polishing rate stability
The polishing solution comprises the following components:
reference examples: ceO (CeO) 2 And (3) grinding materials: 0.25wt%; d-sorbitol: 0.5wt%; picolinic acid: 0.25wt%; the balance of deionized water. Example 9-1: ceO (CeO) 2 And (3) grinding materials: 0.25wt%; d-sorbitol: 0.5wt%; picolinic acid: 0.25wt%; 10000:0.02wt% of polyvinyl alcohol; the balance of deionized water.
Example 9-2: ceO (CeO) 2 And (3) grinding materials: 0.25wt%; d-sorbitol: 0.5wt%; picolinic acid: 0.25wt%; polyvinyl alcohol 20000:0.02wt%; the balance of deionized water.
Example 9-3: ceO (CeO) 2 And (3) grinding materials: 0.25wt%; d-sorbitol: 0.5wt%; picolinic acid: 0.25wt%; polyvinyl alcohol 67000:0.02wt%; the balance of deionized water.
Comparative example 9-1: ceO (CeO) 2 And (3) grinding materials: 0.25wt%; d-sorbitol: 0.5wt%; picolinic acid: 0.25wt%; polyvinyl alcohol 195000:0.02wt%; the balance of deionized water.
As shown in FIGS. 8 and 9, the reference polishing solution containing no polyvinyl alcohol was used for TEOS and Si in the range of 1 month 3 N 4 The polishing rate stability of (C) was substantially stable, and the polishing liquid compositions shown in example 9-1, example 9-2, and example 9-3 were kept to TEOS and Si within 12 months 3 N 4 Is unable to stabilize TEOS and Si in comparative example 9-1 3 N 4 Is used for polishing.
Examples ten
In this example, the amino acid is any two or three of glycine, alanine, aspartic acid, glutamic acid, arginine, proline, picolinic acid and nicotinic acid, and the stability and the selection ratio are tested under the same conditions as in example 1, and the formula can meet the selection ratio of TEOS and Si within 30-80 within 12 months 3 N 4 Is substantially stable.
The invention is applicable to the prior art where it is not described.
Claims (5)
1. A high-stability STI CMP polishing solution with adjustable removal rate selection ratio,the method is characterized in that: in STI CMP with TEOS/Si in acidic conditions at ph=2-6 3 N 4 The removal rate selection ratio is in the range of 30-80, and the polishing solution can ensure the stability of the polishing rate within 12 months on the basis of high removal rate selection ratio;
the polishing solution comprises the following components in percentage by mass: ceO (CeO) 2 And (3) grinding materials: 0.1wt% to 5wt%; amino acid: 0.1wt% to 4wt%; polyol: 0.5wt% to 6wt%; polyvinyl alcohol: 0.01wt% to 1wt%; a pH regulator; the balance of deionized water;
the molecular weight of the polyvinyl alcohol is 1 ten thousand to 10 ten thousand;
the amino acid is: glycine, alanine, aspartic acid, glutamic acid, arginine, proline, picolinic acid, nicotinic acid or derivatives thereof;
the polyol is: d-sorbitol, mannitol, lactitol, maltitol, maltotriose alcohol, xylitol, dulcitol, or one or more of their derivatives.
2. The STI CMP slurry of high stability with an adjustable removal rate selectivity according to claim 1, characterized in that: the CeO 2 The grain diameter of the abrasive in the abrasive is 60-300nm; the pH regulator is as follows: inorganic or organic acids, inorganic or organic bases.
3. The STI CMP slurry of high stability with an adjustable removal rate selectivity according to claim 1, characterized in that: the inorganic or organic acid comprises one or more of nitric acid, phosphoric acid, citric acid, oxalic acid and acetic acid, and the inorganic or organic base comprises one or more of potassium hydroxide, sodium hydroxide, ammonium hydroxide, tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, ethanolamine and diethanolamine;
the polyvinyl alcohol: at least one of polyvinyl alcohol 10000, polyvinyl alcohol 20000, polyvinyl alcohol 27000, polyvinyl alcohol 67000, polyvinyl alcohol 89000, or other molecular weight polyvinyl alcohols.
4. According toThe STI CMP slurry of claim 1 having an adjustable removal rate selectivity and high stability, wherein: TEOS/Si using polishing solution 3 N 4 The polishing conditions were:
polishing machine: universal-150B; projectile/dish rotational speed: 87/93rpm; pressure: 2.8psi/3psi; the flow rate is 150ml/min; polishing time: 60s; the prepared polishing solution is stirred for 40min by a high-speed stirrer before polishing, and the stirring speed is 3500r/min.
5. The STI CMP slurry of high stability with an adjustable removal rate selectivity according to claim 1, characterized in that: protonated amino groups of the amino acid under acidic conditions with TEOS and Si 3 N 4 The hydrogen bond is formed on the surface and then adsorbed on the surface to form a film, and part of amino acid can inhibit the removal rate of TEOS, but can certainly inhibit Si 3 N 4 Is a removal rate of (2); polyols are prepared from hydroxyl groups and TEOS and Si by protonation in acidic environments 3 N 4 Hydrogen bond is formed on the surface to be adsorbed on the surface for film formation, but the removal rate of TEOS is not affected, and Si is inhibited 3 N 4 Is a removal rate of (2); through the synergistic effect of amino acid, polyvinyl alcohol and polyalcohol, the STI CMP polishing solution with the removal rate selection ratio of 30-80 is obtained, and the polishing solution can keep the polishing rate stable within 12 months.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119592231A (en) * | 2024-12-25 | 2025-03-11 | 河北工业大学 | Silica/nitrided silicic acid polishing solution based on cerium oxide abrasive and preparation method thereof |
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| TW202319494A (en) * | 2021-10-05 | 2023-05-16 | 美商慧盛材料美國責任有限公司 | Chemical mechanical planarization polishing for shallow trench isolation |
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| CN102149789A (en) * | 2008-09-12 | 2011-08-10 | 费罗公司 | Chemical-mechanical polishing compositions and methods of making and using the same |
| US20140154884A1 (en) * | 2011-05-24 | 2014-06-05 | Kuraray Co., Ltd. | Erosion inhibitor for chemical mechanical polishing, slurry for chemical mechanical polishing, and chemical mechanical polishing method |
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| CN119592231A (en) * | 2024-12-25 | 2025-03-11 | 河北工业大学 | Silica/nitrided silicic acid polishing solution based on cerium oxide abrasive and preparation method thereof |
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