CN113122139A - Chemical mechanical polishing solution and use method thereof - Google Patents
Chemical mechanical polishing solution and use method thereof Download PDFInfo
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- CN113122139A CN113122139A CN201911397746.XA CN201911397746A CN113122139A CN 113122139 A CN113122139 A CN 113122139A CN 201911397746 A CN201911397746 A CN 201911397746A CN 113122139 A CN113122139 A CN 113122139A
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- polishing
- chemical mechanical
- polishing solution
- mechanical polishing
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- 238000005498 polishing Methods 0.000 title claims abstract description 147
- 239000000126 substance Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 24
- 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 24
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002194 amorphous carbon material Substances 0.000 claims abstract description 23
- 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
- 239000007788 liquid Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 15
- 239000007800 oxidant agent Substances 0.000 abstract description 8
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 9
- 229910003481 amorphous carbon Inorganic materials 0.000 description 8
- 150000000703 Cerium Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 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
- 229910052799 carbon Inorganic materials 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- CVMIVKAWUQZOBP-UHFFFAOYSA-L manganic acid Chemical compound O[Mn](O)(=O)=O CVMIVKAWUQZOBP-UHFFFAOYSA-L 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 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
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 description 2
- 239000006227 byproduct Substances 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
- 238000002360 preparation method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 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
- 239000003086 colorant Substances 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
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention provides a chemical mechanical polishing solution, which comprises cerium oxide, cerium sulfate and a pH regulator. The chemical mechanical polishing solution uses cerium oxide as polishing particles and uses cerium sulfate as an oxidant, so that the polishing rate of the amorphous carbon material can be increased, and the stability of the polishing solution can be improved.
Description
Technical Field
The invention relates to the field of chemical mechanical polishing solution.
Background
With the continuous development of semiconductor technology and the continuous increase of interconnect layers of large-scale integrated circuits, the planarization technology of the conductive layer and the insulating dielectric layer becomes more critical. In the 80's of the twentieth century, Chemical Mechanical Polishing (CMP) technology pioneered by IBM corporation was considered the most effective method of global planarization at present. 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 the chip. Wherein the polishing head holds the chip and then presses the front side 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 table. At the same time, the slurry containing the abrasive is dropped onto the polishing pad and is spread on the polishing pad by centrifugation. The chip surface is globally planarized under the dual actions of mechanical and chemical.
The amorphous carbon as a new generation of wide band gap semiconductor material has the characteristics of wide band gap, high thermal 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 and high-density integrated electronic devices and the like. However, the carbon-containing material is very stable at normal temperature, is not easy to generate chemical reaction, and has good tolerance to mechanical grinding, so that the commonly used chemical mechanical polishing solution is difficult to obtain higher polishing speed when the carbon-containing material is polished.
It is generally necessary to remove the carbonaceous material after oxidation with an oxidizing agent. The common oxidant is hydrogen peroxide, but the oxidation capacity of the hydrogen peroxide is weak, so that an ideal removal rate cannot be obtained. CN102464944A strong oxidizing agents such as permanganic acid, manganic acid and salts thereof are added into the polishing solution to improve the chemical mechanical polishing rate of the carbon-containing material. In the process of polishing carbon-containing materials by using permanganate, manganic acid and salts thereof as oxidants, the permanganate, manganic acid and other oxidants are reduced to inevitably generate byproducts with dark colors and are easy to deposit on the surface and holes of the polishing pad, so that the polishing byproducts are accumulated on the polishing pad, the service life of the polishing pad is influenced, and the defects on the polished surface are increased. In addition, conventional strong oxidizers are generally incapable of polishing amorphous carbon materials.
Disclosure of Invention
In order to solve the above problems, the present invention provides a chemical mechanical polishing solution, in which cerium oxide is used as polishing particles and cerium sulfate is used in combination, so that not only the polishing rate of an amorphous carbon material can be increased, but also 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 mass percentage concentration of the cerium sulfate is 0.8-2%.
In the invention, the pH value of the chemical mechanical polishing solution is 0.6-1.3.
In another aspect of the invention, a method for using the chemical mechanical polishing solution is provided, and any of the polishing solutions is used for chemical mechanical polishing of amorphous carbon materials.
Compared with the prior art, the invention has the advantages that: in the chemical mechanical polishing solution, cerium oxide abrasive particles and cerium sulfate within a certain content range are simultaneously added, and the polishing rate of the chemical mechanical polishing solution to the amorphous carbon material can be enhanced and stabilized by utilizing the compounding effect of the cerium oxide abrasive particles and the cerium sulfate.
Detailed Description
The advantages of the invention are explained in detail below with reference to specific embodiments.
The components are uniformly mixed according to the content in the table 1, and the polishing solution is adjusted to a target pH value by using a potassium hydroxide solution or a sulfuric acid solution, so that the corresponding chemical mechanical polishing solution can be prepared.
Polishing test is carried out on the amorphous carbon material with the square shape of 4 multiplied by 4cm by adopting a Logitech IPM52 polishing machine table, and the corresponding polishing conditions comprise: the IC1010 polishing pad, Platen and Carrier were rotated at 93rpm and 87rpm, respectively, at a pressure of 2.5psi, and at a slurry flow rate of 100 mL/min. The amorphous carbon material film thickness was measured with a NanoSpec film thickness measuring system (NanoSpec6100-300, Shanghai NanoSpec Technology Corporation). The thickness of the blank film was measured from the center of 4X 4cm square amorphous carbon material at 9 points on the diameter line at 0 degree, 90 degree and 180 degree 270 degree angles and at center distances of 1cm and 2cm, respectively. The polishing rate is an average of the 9 points.
The specific components and component contents of the polishing solutions of comparative examples 1 to 12 and examples 1 to 8, the pH values of the polishing solutions, and the polishing rates of the polishing solutions to the amorphous carbon material after the polishing solutions were prepared for 5min, 24h, and 72h are shown in Table 1.
TABLE 1 Components, component contents, pH values and polishing rates of the chemical mechanical polishing solutions of comparative examples 1 to 12 and examples 1 to 8.
Comparing the polishing rates of the polishing solutions of comparative examples 1 to 3 to amorphous carbon, it can be seen that, when the polishing solution does not contain abrasive particles, the polishing rate of the ammonium ceric nitrate solution is much greater than that of the cerium sulfate solution, and the ammonium ceric sulfate solution has no polishing effect on the amorphous carbon material; as can be seen from the data of comparative examples 1 and 2, the CMP slurry containing only ammonium cerium nitrate and cerium sulfate showed a significant decrease in polishing rate from 457A/min and 82A/min to 30A/min and 12A/min, respectively, after 72 hours of preparation.
From the polishing data of the polishing solutions of comparative examples 5 and 8 on the amorphous carbon material, it can be seen that the polishing solution only contains cerium oxide or silicon oxide abrasive particles, and has no polishing effect on the amorphous carbon material.
From the polishing data of the polishing solutions of comparative examples 10 and 11 on amorphous carbon, it can be seen that the polishing solutions using cerium oxide as polishing abrasive particles and ammonium persulfate or potassium periodate as oxidizer have no polishing effect on amorphous carbon materials.
From the polishing data of comparative examples 6 and 7 on amorphous carbon, it can be seen that when ammonium cerium nitrate and cerium oxide or silicon oxide abrasive grains are added to the polishing solution at the same time, the polishing rate of the polishing solution is greatly reduced after the polishing solution is prepared for 24 hours.
As can be seen from the above, conventional oxidizing agents such as potassium periodate or ammonium persulfate do not have a polishing effect on amorphous carbon materials; when cerium oxide or cerium salt is added into the polishing solution, the polishing solution has no polishing effect on the amorphous carbon material or has poor stability; when cerium oxide and other cerium salts are added into the polishing solution at the same time, the polishing solution has a high polishing rate to the amorphous carbon material but has poor stability.
As can be seen from the polishing rates of the polishing solutions of comparative example 2 and example 1, the polishing rate of the polishing solution with the simultaneous addition of cerium sulfate and cerium oxide abrasive grains was increased from 82A/min to 106A/min, and the polishing rate of the polishing solution remained at 102A/min after 24 hours, which was stable. From the polishing rates of the polishing solutions of example 1 and comparative example 9, it can be seen that when the abrasive particles added to the polishing solution are silicon oxide, the polishing rate of the corresponding polishing solution to amorphous carbon is low.
Therefore, the cerium oxide abrasive particles and the cerium sulfate are added into the polishing solution simultaneously, so that the polishing rate of the polishing solution to the amorphous carbon material can be improved, and the stability of the polishing solution is enhanced.
Comparing the polishing effects of the polishing solutions of examples 3 and 4 and examples 6 and 7, it can be seen that the higher the content of cerium sulfate, the higher the polishing rate after 5 minutes of the preparation of the corresponding polishing solution; but the polishing rate tends to be consistent with the placement of the polishing solution and is kept within the range of 183- & ltSUB & gt 198A/min. Comparing the polishing effects of the polishing solutions of examples 1 and 3, it can be seen that lowering the pH value without changing the composition of the polishing solution contributes to increasing the polishing rate of amorphous carbon. Comparing the polishing effects of the polishing solutions of examples 4, 5 and 6, it can be seen that the polishing rate of the polishing solution to amorphous carbon is independent of the cerium oxide content, and the polishing rate of the corresponding polishing solution gradually becomes uniform as the standing time is prolonged. Comparing the polishing effects of the polishing solutions of examples 7 and 8, it can be seen that the polishing rate of the polishing solution with cerium sulfate content of 0.8% was increased from 143A/min to 198A/min after 72 hours of the configuration, while the polishing rate of the polishing solution with cerium sulfate content of 0.4% was decreased from 111A/min to 55A/min, which indicates that the polishing rate could not be decreased within 72 hours even when the content of cerium sulfate was 0.4%. From the above, it can be seen that when the polishing solution using the cerium oxide abrasive particles and the cerium sulfate has a mass percentage concentration of 0.2-1% and a mass percentage concentration of 0.8-6.5%, the polishing rate of the amorphous carbon material can be maintained at 155-198A/min for 24-72 hours.
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 in a certain content range are added, and the polishing solution has high polishing rate and high stability to the amorphous carbon material through the compounding effect between cerium sulfate and cerium oxide.
In summary, when cerium salt is added to the chemical mechanical polishing solution alone to polish the amorphous carbon, the polishing solution has selectivity to the type 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 the cerium oxide abrasive particles are added into the chemical mechanical polishing solution separately, the polishing solution has no polishing effect on the amorphous carbon material. In the chemical mechanical polishing solution, cerium oxide abrasive particles and cerium sulfate within a certain content range are simultaneously added, and the polishing rate of the chemical mechanical polishing solution to the amorphous carbon material can be enhanced and stabilized by utilizing the compounding effect of the cerium oxide abrasive particles and the cerium sulfate.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the 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 (7)
1. A chemical mechanical polishing solution comprises cerium oxide, cerium sulfate and a pH regulator.
2. The chemical mechanical polishing solution according to claim 1,
the pH regulator is selected from one or more of potassium hydroxide and sulfuric acid.
3. The chemical mechanical polishing solution according to claim 1,
the mass percentage concentration of the cerium oxide is 0.1-1%.
4. The chemical mechanical polishing solution according to claim 1,
the mass percentage concentration of the cerium sulfate is 0.8-6.5%.
5. The chemical mechanical polishing solution according to claim 4,
the mass percentage concentration of the cerium sulfate is 0.8-2%.
6. The chemical mechanical polishing solution according to claim 1,
the pH value of the chemical mechanical polishing solution is 0.6-1.3.
7. A method for using chemical polishing liquid is characterized in that,
the chemical mechanical polishing solution as set forth in any one of claims 1 to 6 for use in chemical polishing of amorphous carbon material.
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| CN113122139B CN113122139B (en) | 2024-04-05 |
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| 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 |
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| US20020053656A1 (en) * | 1999-03-29 | 2002-05-09 | Anne E. Miller | Ceric-ion slurry for use in chemical-mechanical polishing |
| CN1556840A (en) * | 2001-09-24 | 2004-12-22 | Rare earth salt oxidizer based CMP method | |
| US20060234509A1 (en) * | 2005-04-15 | 2006-10-19 | Small Robert J | Cerium oxide abrasives for chemical mechanical polishing |
| 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 |
| US20190119524A1 (en) * | 2016-04-20 | 2019-04-25 | Shin-Etsu Chemical Co., Ltd. | Polishing agent for synthetic quartz glass substrate and method for polishing synthetic quartz glass substrate |
| 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 |
-
2019
- 2019-12-30 CN CN201911397746.XA patent/CN113122139B/en active Active
Patent Citations (10)
| 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 |
| US20020053656A1 (en) * | 1999-03-29 | 2002-05-09 | Anne E. Miller | Ceric-ion slurry for use in chemical-mechanical polishing |
| 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 | |
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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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