CN113122139B - Chemical mechanical polishing solution and application method thereof - Google Patents
Chemical mechanical polishing solution and application method thereof Download PDFInfo
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- CN113122139B CN113122139B CN201911397746.XA CN201911397746A CN113122139B CN 113122139 B CN113122139 B CN 113122139B CN 201911397746 A CN201911397746 A CN 201911397746A CN 113122139 B CN113122139 B CN 113122139B
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- polishing solution
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- 238000005498 polishing Methods 0.000 title claims abstract description 151
- 239000000126 substance Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims description 7
- 239000002194 amorphous carbon material Substances 0.000 claims abstract description 23
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 23
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 23
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 10
- 239000007800 oxidant agent Substances 0.000 abstract description 8
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 229910003481 amorphous carbon Inorganic materials 0.000 description 8
- 239000006061 abrasive grain Substances 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 6
- 150000000703 Cerium Chemical class 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- CVMIVKAWUQZOBP-UHFFFAOYSA-L manganic acid Chemical compound O[Mn](O)(=O)=O CVMIVKAWUQZOBP-UHFFFAOYSA-L 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- MLIWQXBKMZNZNF-KUHOPJCQSA-N (2e)-2,6-bis[(4-azidophenyl)methylidene]-4-methylcyclohexan-1-one Chemical compound O=C1\C(=C\C=2C=CC(=CC=2)N=[N+]=[N-])CC(C)CC1=CC1=CC=C(N=[N+]=[N-])C=C1 MLIWQXBKMZNZNF-KUHOPJCQSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- VZDYWEUILIUIDF-UHFFFAOYSA-J cerium(4+);disulfate Chemical compound [Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VZDYWEUILIUIDF-UHFFFAOYSA-J 0.000 description 1
- 229910000355 cerium(IV) sulfate Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
Abstract
The invention provides a chemical mechanical polishing solution, which comprises cerium oxide, cerium sulfate and a pH regulator. In the invention, the chemical mechanical polishing solution uses cerium oxide as polishing particles and cerium sulfate as an oxidant, so that the polishing rate of the amorphous carbon material can be improved, and the stability of the polishing solution can be improved.
Description
Technical Field
The invention relates to the field of chemical mechanical polishing solutions.
Background
With the continued development of semiconductor technology and the increasing number of interconnection layers for large scale integrated circuits, the planarization techniques of conductive layers and insulating dielectric layers have become particularly critical. In the twentieth century, the Chemical Mechanical Polishing (CMP) technology originated by IBM corporation was considered the most effective method of global planarization at present. Chemical Mechanical Polishing (CMP) consists of a combination of chemical action, mechanical action, and both actions. It generally consists of a polishing table with a polishing pad and a polishing head for carrying the chip. Wherein the polishing head holds the chip and then presses the front surface of the chip 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 platen. At the same time, slurry containing abrasive is dropped onto the polishing pad and laid flat on the polishing pad by centrifugation. The chip surface is globally planarized under the dual actions of machinery and chemistry.
Amorphous carbon is used as a new generation of wide band gap semiconductor material, has the characteristics of wide band gap, high heat conductivity, high critical breakdown electric field, high electron saturation migration rate, high chemical stability and the like, and has great application potential in the aspects of high-temperature, high-frequency, high-power, high-density integrated electronic devices and the like. However, the carbon-containing material is very stable at normal temperature, is not easy to cause chemical reaction, and has good tolerance to mechanical polishing, so that the common chemical mechanical polishing solution is difficult to obtain higher polishing speed when polishing the carbon-containing material.
It is often desirable to remove the carbonaceous material after oxidation with an oxidizing agent. The commonly used oxidant is hydrogen peroxide, but the oxidation capability of hydrogen peroxide is weak, and the ideal removal rate cannot be obtained. CN102464944A is added with strong oxidizing agents such as permanganic acid, manganic acid, salts thereof and the like in the polishing solution to improve the chemical mechanical polishing rate of the carbonaceous material. In the process of polishing carbonaceous materials by using permanganate, manganic acid and salts thereof as an oxidizing agent, by-products with a darker color are inevitably generated after the oxidizing agent such as the permanganate, the manganic acid and the like is reduced, and are easily deposited on the surface and holes of the polishing pad, so that the aggregation of the polishing by-products on the polishing pad is caused, the service life of the polishing pad is influenced, and the surface defects after polishing are increased. In addition, conventional strong oxidizers generally fail to polish amorphous carbon materials.
Disclosure of Invention
In order to solve the problems, the invention provides a chemical mechanical polishing solution, which uses cerium oxide as polishing particles and is matched with cerium sulfate, so that the polishing rate of an amorphous carbon material can be improved, and the stability of the polishing solution can be improved.
Specifically, the invention provides a chemical mechanical polishing solution, which comprises cerium oxide, cerium sulfate and a pH regulator.
In the invention, the pH regulator is selected from one or more of potassium hydroxide and sulfuric acid.
In the invention, the mass percentage concentration of the cerium oxide is 0.1-1%.
In the invention, the mass percentage concentration of the cerium sulfate is 0.8-6.5%; preferably, the concentration of the cerium sulfate is 0.8-2% by mass.
In the invention, the pH value of the chemical mechanical polishing solution is 0.6-1.3.
In another aspect of the present invention, a method of using a chemical mechanical polishing solution is provided, wherein any of the above polishing solutions is used for chemical mechanical polishing of an amorphous carbon material.
Compared with the prior art, the invention has the advantages that: the cerium oxide abrasive particles and the cerium sulfate are added in a certain content range at the same time in the chemical mechanical polishing solution, and the polishing rate of the chemical mechanical polishing solution on the amorphous carbon material can be enhanced and stabilized by utilizing the compound action of the cerium oxide abrasive particles and the cerium sulfate.
Detailed Description
The advantages of the present invention will be described in detail below in conjunction with the specific embodiments.
The components are uniformly mixed according to the content in the table 1, and the polishing solution is adjusted to the target pH value by using potassium hydroxide solution or sulfuric acid solution, so that the corresponding chemical mechanical polishing solution can be prepared.
Polishing tests were performed on 4 x 4cm square amorphous carbon material using a Logitech IPM52 polisher table, corresponding to polishing conditions including: IC1010 polishing pad, platen and Carrier speeds were 93rpm and 87rpm, respectively, with a pressure of 2.5psi and a slurry flow rate of 100mL/min. The amorphous carbon material film thickness was measured using a NanoSpec film thickness measurement system (NanoSpec 6100-300,Shanghai Nanospec Technology Corporation). The film thickness of the blank was measured from the center position of the amorphous carbon material having a square shape of 4×4cm, and the angles on the diameter line were 0 degrees, 90 degrees, and 180 degrees, 270 degrees, respectively, and the center distances were 1cm and 2cm, respectively, at 9 points in total. The polishing rate is an average of the 9 points.
The specific components and the component contents of the polishing solutions of comparative examples 1 to 12 and examples 1 to 8, the pH value of the polishing solution, and the polishing rates of the amorphous carbon material by the polishing solutions after 5min, 24h and 72h of the measured configuration are shown in Table 1.
Table 1 comparative examples 1 to 12 and examples 1 to 8 were chemical mechanical polishing solutions in terms of components, component contents, pH values of the polishing solutions, and polishing rates thereof.
Comparing the polishing rates of the polishing solutions of comparative examples 1 to 3 with respect to amorphous carbon, it was found that, when the polishing solution does not contain abrasive grains, the polishing rate of the ceric ammonium nitrate solution was much greater than the polishing rate of the ceric ammonium sulfate solution, which had no polishing effect on the amorphous carbon material; as is clear from the data of comparative examples 1 and 2, the chemical mechanical polishing solutions added with only ceric ammonium nitrate and ceric sulfate showed a significant decrease in polishing rates from 457A/min and 82A/min to 30A/min and 12A/min, respectively, after being prepared for 72 hours.
From the polishing data of the amorphous carbon material by the polishing solutions of comparative examples 5 and 8, it is known that the polishing solution has no polishing effect on the amorphous carbon material by adding only cerium oxide or silicon oxide abrasive grains.
From the polishing data of the amorphous carbon by the polishing solutions of comparative examples 10 and 11, it is known that the polishing solution has no polishing effect on the amorphous carbon material by using cerium oxide as polishing abrasive grains and ammonium persulfate or potassium periodate as an oxidizing agent.
From the polishing data of the amorphous carbon by the polishing solutions of comparative examples 6 and 7, it was found that when ceric ammonium nitrate and cerium oxide or silicon oxide abrasive grains were simultaneously added to the polishing solution, the polishing rate of the polishing solution was still greatly reduced after 24 hours of the polishing solution preparation.
As can be seen from the above, conventional oxidizing agents such as potassium periodate or ammonium persulfate have no polishing effect on amorphous carbon materials; when cerium oxide or cerium salt is added into the polishing solution alone, the polishing solution has no polishing effect on the amorphous carbon material or the stability of the polishing solution is poor; when cerium oxide and other cerium salts are simultaneously added to the polishing liquid, the polishing rate of the polishing liquid on the amorphous carbon material is high but the stability of the polishing liquid is poor.
From the polishing rates of the polishing solutions of comparative example 2 and example 1, it was found that the polishing rate of the polishing solution to which cerium sulfate and cerium oxide abrasive grains were added simultaneously was increased from 82A/min to 106A/min, while the polishing rate of the polishing solution was maintained at 102A/min after 24 hours, and the polishing rate was maintained stable, as compared with the polishing solution to which cerium sulfate alone was added. As is clear from the polishing rates of the polishing solutions of example 1 and comparative example 9, when the abrasive grains added to the polishing solution were silicon oxide, the polishing rate of amorphous carbon with respect to the polishing solution was low.
Therefore, the addition of both cerium oxide abrasive particles and cerium sulfate to the polishing liquid can increase the polishing rate of the polishing liquid to the amorphous carbon material while enhancing the stability of the polishing liquid.
Comparing the polishing effects of the polishing solutions of examples 3 and 4 and examples 6 and 7, it is understood that the higher the content of cerium sulfate, the higher the polishing rate after 5 minutes of the corresponding polishing solution preparation; however, the polishing rate tends to be uniform with the placement of the polishing solution, and is kept in the range of 183-198A/min. Comparing the polishing effects of the polishing solutions of examples 1 and 3, it is understood that lowering the pH helps to increase the polishing rate of amorphous carbon without changing the composition of the polishing solution. Comparing the polishing effects of the polishing liquids of examples 4, 5 and 6, it is understood that the polishing rate of amorphous carbon by the polishing liquid is independent of the content of cerium oxide, and the polishing rate of the corresponding polishing liquid gradually tends to be uniform with the extension of the standing time. As is clear from comparison of the polishing effects of the polishing solutions of examples 7 and 8, the polishing rate of the polishing solution having a cerium sulfate content of 0.8% was increased from 143A/min to 198A/min after 72 hours of the arrangement, while the polishing rate of the polishing solution having a cerium sulfate content of 0.4% was decreased from 111A/min to 55A/min, which means that the polishing rate could not be ensured to be decreased within 72 hours even when the cerium sulfate content was 0.4%. From the above, it was found that when the polishing liquid comprising the ceria abrasive grains and the ceria sulfate was used, the polishing rate of the amorphous carbon material could be maintained at 155 to 198A/min for 24 to 72 hours when the mass percentage concentration of the ceria was 0.2 to 1% and the mass percentage concentration of the ceria sulfate was 0.8 to 6.5%.
Therefore, the polishing solution has selectivity to the content of cerium salt and cerium oxide abrasive particles, namely, cerium sulfate and cerium oxide abrasive particles added in a certain content range, and has higher polishing rate and higher stability to the amorphous carbon material through the compounding action between the cerium sulfate and the cerium oxide.
In summary, when cerium salt is added to a chemical mechanical polishing solution alone to polish amorphous carbon, the polishing solution has selectivity to the kind of cerium salt, and the polishing rate of the polishing solution to the amorphous carbon material is greatly reduced with the increase of the configuration time; if cerium oxide abrasive particles are added alone to a chemical mechanical polishing liquid, the polishing liquid has no polishing effect on an amorphous carbon material. The cerium oxide abrasive particles and the cerium sulfate are added in a certain content range at the same time in the chemical mechanical polishing solution, and the polishing rate of the chemical mechanical polishing solution on the amorphous carbon material can be enhanced and stabilized by utilizing the compound action of the cerium oxide abrasive particles and the cerium sulfate.
The above description of the specific embodiments of the present invention has been given by way of example only, and the present invention is not limited to the above described specific embodiments. Any equivalent modifications and substitutions for the present invention will occur to those skilled in the art, and are also within the scope of the present invention. Accordingly, equivalent changes and modifications are intended to be included within the scope of the present invention without departing from the spirit and scope thereof.
Claims (4)
1. A chemical mechanical polishing solution consists of cerium oxide, cerium sulfate, a pH regulator and water;
the mass percentage concentration of the cerium oxide is 0.1-1%;
the mass percentage concentration of the cerium sulfate is 0.8-6.5%;
the pH value of the chemical mechanical polishing solution is 0.6-1.3.
2. The chemical mechanical polishing liquid according to claim 1, wherein,
the pH regulator is one or more selected from potassium hydroxide and sulfuric acid.
3. The chemical mechanical polishing liquid according to claim 1, wherein,
the mass percentage concentration of the cerium sulfate is 0.8-2%.
4. A method for using chemical polishing solution is characterized in that,
a chemical mechanical polishing solution according to any one of claims 1 to 3 for chemical polishing of amorphous carbon materials.
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| CN201911397746.XA CN113122139B (en) | 2019-12-30 | 2019-12-30 | Chemical mechanical polishing solution and application method thereof |
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| CN201911397746.XA CN113122139B (en) | 2019-12-30 | 2019-12-30 | Chemical mechanical polishing solution and application method thereof |
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| CN113122139A CN113122139A (en) | 2021-07-16 |
| CN113122139B true CN113122139B (en) | 2024-04-05 |
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|---|---|---|---|---|
| CN1248994A (en) * | 1996-12-30 | 2000-03-29 | 卡伯特公司 | Composition for oxide CMP |
| CN1313374A (en) * | 2000-03-10 | 2001-09-19 | 长兴化学工业股份有限公司 | Grinding milk and its application |
| CN1556840A (en) * | 2001-09-24 | 2004-12-22 | Rare earth salt oxidizer based CMP method | |
| CN101506325A (en) * | 2006-08-30 | 2009-08-12 | 卡伯特微电子公司 | Compositions and methods for cmp of semiconductor materials |
| CN101818047A (en) * | 2010-02-08 | 2010-09-01 | 中国科学院上海微系统与信息技术研究所 | Silicon oxide-cerium oxide nuclear shell compounded abrasive granules, and preparation and application thereof |
| CN103021837A (en) * | 2011-09-27 | 2013-04-03 | 中芯国际集成电路制造(上海)有限公司 | Method of processing and forming amorphous carbon layer and production method of semiconductor device |
| JPWO2018179062A1 (en) * | 2017-03-27 | 2019-12-26 | 日立化成株式会社 | Polishing liquid, polishing liquid set, additive liquid and polishing method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6752844B2 (en) * | 1999-03-29 | 2004-06-22 | Intel Corporation | Ceric-ion slurry for use in chemical-mechanical polishing |
| US7368388B2 (en) * | 2005-04-15 | 2008-05-06 | Small Robert J | Cerium oxide abrasives for chemical mechanical polishing |
| JP6560155B2 (en) * | 2016-04-20 | 2019-08-14 | 信越化学工業株式会社 | Polishing agent for synthetic quartz glass substrate and method for polishing synthetic quartz glass substrate |
-
2019
- 2019-12-30 CN CN201911397746.XA patent/CN113122139B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1248994A (en) * | 1996-12-30 | 2000-03-29 | 卡伯特公司 | Composition for oxide CMP |
| CN1313374A (en) * | 2000-03-10 | 2001-09-19 | 长兴化学工业股份有限公司 | Grinding milk and its application |
| CN1556840A (en) * | 2001-09-24 | 2004-12-22 | Rare earth salt oxidizer based CMP method | |
| CN101506325A (en) * | 2006-08-30 | 2009-08-12 | 卡伯特微电子公司 | Compositions and methods for cmp of semiconductor materials |
| CN101818047A (en) * | 2010-02-08 | 2010-09-01 | 中国科学院上海微系统与信息技术研究所 | Silicon oxide-cerium oxide nuclear shell compounded abrasive granules, and preparation and application thereof |
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| JPWO2018179062A1 (en) * | 2017-03-27 | 2019-12-26 | 日立化成株式会社 | Polishing liquid, polishing liquid set, additive liquid and polishing method |
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