CN111378371B - Application of pyrogallic acid in polishing of silicon dioxide - Google Patents
Application of pyrogallic acid in polishing of silicon dioxide Download PDFInfo
- Publication number
- CN111378371B CN111378371B CN201811627089.9A CN201811627089A CN111378371B CN 111378371 B CN111378371 B CN 111378371B CN 201811627089 A CN201811627089 A CN 201811627089A CN 111378371 B CN111378371 B CN 111378371B
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- CN
- China
- Prior art keywords
- polishing
- pyrogallic acid
- silicon dioxide
- cerium oxide
- chemical mechanical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000005498 polishing Methods 0.000 title claims description 114
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 66
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 title claims description 38
- 239000000377 silicon dioxide Substances 0.000 title claims description 33
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 25
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 32
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 27
- 239000000126 substance Substances 0.000 claims description 20
- 239000006061 abrasive grain Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000084 colloidal system Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 9
- 230000007547 defect Effects 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention discloses an application of pyrogallic acid in silicon dioxide polishing, wherein the pyrogallic acid is mixed with a chemical mechanical polishing solution for use, the chemical mechanical polishing solution comprises cerium oxide abrasive particles, the concentration of the pyrogallic acid is 20-1000ppm, and the pH of the chemical mechanical polishing solution is 4.5. According to the invention, the pyrogallic acid is added into the chemical mechanical polishing solution, so that the polishing rate of silicon dioxide can be properly inhibited, the butterfly defect generated on the surface of the silicon dioxide in the polishing process is avoided, and the quality of the polished product is improved.
Description
Technical Field
The invention relates to the field of chemical mechanical polishing, in particular to application of pyrogallic acid in polishing of silicon dioxide.
Background
Chemical Mechanical Polishing (CMP) consists of chemical action, mechanical action, and a combination of these two actions. It generally consists of a polishing table with a polishing pad and a polishing head for carrying a wafer. Wherein the polishing head holds the wafer and then presses the front side of the wafer against the polishing pad. When performing chemical mechanical polishing, the polishing head moves linearly over the polishing pad or rotates in the same direction of motion as the polishing table. At the same time, the slurry containing the abrasive particles is dropped onto the polishing pad and is spread on the polishing pad by centrifugation. The wafer surface is globally planarized under the dual actions of mechanical and chemical.
Cerium oxide is an important CMP polishing solution abrasive, and compared with the traditional silica sol abrasive, cerium oxide has higher polishing rate and better polishing effect on silicon dioxide materials, and is widely applied to the chemical mechanical polishing of silicon dioxide. However, an excessively high polishing rate causes dishing defects on the wafer surface during CMP, resulting in a reduction in the quality of a polished product.
Generally, in order to suppress the generation of dishing defects during CMP, it is necessary to add a dishing defect inhibitor to a ceria CMP polishing solution. However, this increases the production cost of the polishing liquid. On the other hand, if the polishing rate is not properly suppressed, it cannot be used to completely eliminate the dishing defect.
Disclosure of Invention
In order to solve the problems, the invention discloses the application of pyrogallic acid in polishing of silicon dioxide, which can properly inhibit the polishing rate of the silicon dioxide, and the cerium oxide colloid in the polishing solution has high stability.
Specifically, the invention discloses an application of pyrogallic acid in polishing of silicon dioxide, wherein the pyrogallic acid is mixed with a chemical mechanical polishing solution for use, the chemical mechanical polishing solution comprises cerium oxide abrasive particles, the concentration of the pyrogallic acid is 20-1000ppm, and the pH of the chemical mechanical polishing solution is 4.5.
Preferably, the pyrogallic acid is diffusively adsorbed to the surface of the cerium oxide abrasive particle under a concentration condition
Preferably, the pyrogallic acid concentration is 20ppm to 100 ppm.
Preferably, the content of the cerium oxide abrasive particles is 0.4wt% to 10 wt%.
Preferably, the chemical mechanical polishing solution of the present invention may further comprise polishing solution components conventionally used in the art for polishing silica, such as corrosion inhibitors, complexing agents, chelating agents, organic solvents, and the like.
In the present invention, the pH of the chemical mechanical polishing solution can be adjusted using a pH adjusting agent which is conventional in the art.
Compared with the prior art, the invention has the advantages that: 1) according to the invention, the pyrogallic acid is added into the chemical mechanical polishing solution, so that the polishing rate of silicon dioxide can be properly inhibited, the butterfly defect generated on the surface of the silicon dioxide in the polishing process is avoided, and the quality of the polished product is improved; 2) the pyrogallic acid is intensively adsorbed on the surface of the cerium oxide abrasive particles, so that the damage of the pyrogallic acid to the stability of the cerium oxide colloid can be avoided, and the stability of the cerium oxide colloid is improved, thereby prolonging the storage life of the chemical mechanical polishing solution and improving the commercial value of the chemical mechanical polishing solution.
Detailed Description
The advantages of the present invention are further illustrated by the following specific examples, but the scope of the present invention is not limited to the following examples.
Table 1 shows the basic components of the chemical mechanical polishing solutions of examples 1 to 5 of the present invention and comparative example 1. Weighing cerium oxide and pyrogallic acid according to the components and the contents thereof listed in the table 1, mixing, and adjusting to a corresponding pH value with ammonia water or nitric acid to obtain the polishing solution of the comparative example and the invention. In example 4, 500ppm pyrogallic acid was added to a slurry containing 10% cerium oxide and having a pH of 4.5 with stirring, and the stirring was continued for 30 minutes to obtain cerium oxide particles having a surface-enhanced adsorption of pyrogallic acid. Example 5 was obtained by diluting 25 times the mother liquor of example 4.
TABLE 1 comparative example 1 and polishing solutions 1 to 3 according to the invention
The chemical mechanical polishing solutions in the above examples 1 to 3 and comparative example 1 were used to polish the silicon dioxide blank wafer under different polishing pressures, so as to obtain corresponding polishing rates, and the specific results are shown in table 2.
Wherein the polishing conditions are as follows: and (3) selecting a Mirra polishing machine to polish, wherein the polishing pad is an IC1010 polishing pad, the rotating speeds of a polishing disk and the polishing head are 93rpm and 87rpm respectively, the pressure is 1psi-5psi, the flow rate of the polishing solution is 150mL/min, and the polishing time is 60 seconds.
TABLE 2 polishing rates for comparative example 1 and examples 1-5 for silicon dioxide and silicon nitride
As can be seen from Table 2, in comparative example 1, where pyrogallic acid was not added, the polishing rate of the polishing liquid for silica at 1psi was as high as that for comparative example 1
The polishing rate of the silicon dioxide by the polishing solution is increased along with the increase of the polishing pressure, and when the polishing pressure reaches 5psi, the polishing rate of the silicon dioxide by the polishing solution can be close to that of the silicon dioxide
However, as can be seen from examples 1 to 3 of the present invention, the polishing rate of silica by the polishing liquid was significantly suppressed by adding pyrogallic acid to the polishing liquid according to the present invention based on comparative example 1. Only 20ppm pyrogallic acid was added to the polishing solution of example 1, and the polishing rate of the polishing solution to silica was reduced by about 35% to 50% under a polishing pressure of 1 to 5psi, respectively, and the polishing rate of the polishing solution to silica was reduced from a high rate to a moderate rate. In example 2, the content of pyrogallic acid is further increased to 100ppm, the reduction rate of the polishing solution to silicon dioxide exceeds 95% under different polishing pressures, and the polishing rate of the polishing solution to silicon dioxide is further reduced to a low rate; example 3 when the content of pyrogallic acid was increased to 1000ppm, the polishing rate of silica by the polishing liquid was about 95% at different polishing pressures, and almost no change was observed in comparison with the case where the content of pyrogallic acid was 100ppm, and it was found that the polishing rate of silica by the polishing liquid was optimum when the content was in the range of 100ppm to 1000ppm in the case where pyrogallic acid was directly added to the polishing liquid. On the other hand, in the range of 100ppm or less, the effect of controlling the polishing rate of silica can be achieved by changing the content of gallic acid.
In practical application, the polishing solution has application value when the polishing rate of the polishing solution to the silicon dioxide is at a medium rate or a low rate, for example, the polishing solution can be applied to removing an Oxide film layer in the STI polishing process when the polishing rate of the polishing solution to the silicon dioxide is at the medium rate; when the polishing rate of the polishing liquid to silicon dioxide is at a low rate, the polishing liquid can be applied to selective polishing, for example: in polishing Poly and silicon dioxide simultaneously, it is desirable to provide a higher Poly: silicon dioxide selectivity requires the use of a polishing solution with a lower polishing rate for silicon dioxide.
The chemical mechanical polishing solutions of examples 1 to 5 and comparative example 1 were allowed to stand at room temperature for 1 day, and then the particle size of the cerium oxide abrasive grains was measured, and the increase value thereof with respect to the original particle size was calculated, and the results of the specific increase values are shown in table 3.
TABLE 3 increase in particle size and colloidal stability of cerium oxide abrasive particles in comparative example 1 and examples 1 to 5
As shown in Table 3, the stability of cerium oxide colloid in the polishing slurry was affected by the addition of pyrogallic acid. Comparing example 1 with comparative example 1, it can be seen that after 20ppm pyrogallic acid was added to the polishing solution containing cerium oxide abrasive particles, the particle size of the cerium oxide particles increased 2930nm within 24 hours, and the cerium oxide colloid was unstable; after the content of pyrogallic acid is increased from 20ppm to 100ppm, the increase value of the particle size of the cerium oxide particles is reduced within 24h, but the cerium oxide colloid is still in an unstable state; after the pyrogallic acid content was further increased to 1000ppm, the particle size of the cerium oxide particles did not increase within 24 hours, and the cerium oxide colloid was in a stable state. Therefore, the stability of the polishing solution is affected by directly adding pyrogallic acid into the polishing solution, and the stability of the abrasive particle colloid can be ensured only when the addition amount of the pyrogallic acid is enough. But this increases the cost of the polishing solution.
Referring to example 5, pyrogallic acid was adsorbed onto the surface of cerium oxide particles by concentration in example 4, and then diluted before use to obtain a polishing solution. In table 3, it can be seen from comparison between example 1 and example 5 that, under the same conditions, after the pyrogallic acid is added in a concentrated and enhanced manner instead of being directly added to the surface of the cerium oxide particles, the particle size of the cerium oxide particles within 24 hours is changed from a large increase to no change, and the stability of the cerium oxide colloid is greatly improved. Therefore, less pyrogallic acid can be used, higher polishing rate and higher stability of grinding particles can be obtained, and the cost is greatly reduced.
In conclusion, after pyrogallic acid is intensively adsorbed to the surface of cerium oxide particles in the polishing solution containing cerium oxide abrasive particles, the polishing rate of silicon dioxide can be effectively inhibited, the stability of cerium oxide colloid in the polishing solution is greatly improved, and compared with the polishing solution directly added with pyrogallic acid, the storage life of the polishing solution is prolonged, so that the application value of the polishing solution in the polishing industry is improved.
The "content" in the present application is a content of mass percent unless otherwise specified.
It should be understood that the detailed description and specific examples, while indicating exemplary embodiments of the invention, are given by way of illustration only, since the invention is not limited to the specific embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (3)
1. The application of pyrogallic acid in polishing of silicon dioxide, wherein the pyrogallic acid is mixed with a chemical mechanical polishing solution for use, the chemical mechanical polishing solution comprises cerium oxide abrasive particles, the concentration of the pyrogallic acid is 20-1000ppm, and the pH of the chemical mechanical polishing solution is 4.5;
the content of the cerium oxide grinding particles is 0.4wt% -10 wt%.
2. The use according to claim 1, wherein pyrogallic acid is diffusion-adsorbed to the surface of the cerium oxide abrasive grains under a concentrated condition.
3. The use according to claim 1, wherein the pyrogallic acid is present in a concentration of 20ppm to 500 ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811627089.9A CN111378371B (en) | 2018-12-28 | 2018-12-28 | Application of pyrogallic acid in polishing of silicon dioxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811627089.9A CN111378371B (en) | 2018-12-28 | 2018-12-28 | Application of pyrogallic acid in polishing of silicon dioxide |
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| Publication Number | Publication Date |
|---|---|
| CN111378371A CN111378371A (en) | 2020-07-07 |
| CN111378371B true CN111378371B (en) | 2022-05-13 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696235A (en) * | 2004-04-21 | 2005-11-16 | Cmp罗姆和哈斯电子材料控股公司 | Barrier Polishing Solution |
| CN101942667A (en) * | 2009-07-07 | 2011-01-12 | 气体产品与化学公司 | Be used for the prescription and the method for cleaning behind the CMP |
| CN104745092A (en) * | 2013-12-26 | 2015-07-01 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid used in STI field, and use method thereof |
| CN105778774A (en) * | 2014-12-23 | 2016-07-20 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing solution |
| CN105802506A (en) * | 2014-12-29 | 2016-07-27 | 安集微电子（上海）有限公司 | Chemico-mechanical polishing solution |
-
2018
- 2018-12-28 CN CN201811627089.9A patent/CN111378371B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696235A (en) * | 2004-04-21 | 2005-11-16 | Cmp罗姆和哈斯电子材料控股公司 | Barrier Polishing Solution |
| CN101942667A (en) * | 2009-07-07 | 2011-01-12 | 气体产品与化学公司 | Be used for the prescription and the method for cleaning behind the CMP |
| CN104745092A (en) * | 2013-12-26 | 2015-07-01 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid used in STI field, and use method thereof |
| CN105778774A (en) * | 2014-12-23 | 2016-07-20 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing solution |
| CN105802506A (en) * | 2014-12-29 | 2016-07-27 | 安集微电子（上海）有限公司 | Chemico-mechanical polishing solution |
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| CN111378371A (en) | 2020-07-07 |
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