CN113201284B - High-polishing-degree CMP polishing solution and preparation method thereof - Google Patents

High-polishing-degree CMP polishing solution and preparation method thereof Download PDF

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CN113201284B
CN113201284B CN202110445740.6A CN202110445740A CN113201284B CN 113201284 B CN113201284 B CN 113201284B CN 202110445740 A CN202110445740 A CN 202110445740A CN 113201284 B CN113201284 B CN 113201284B
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polishing
cyclodextrin
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polyethylene glycol
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CN113201284A (en
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王继宝
周翠苹
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Shenzhen Sapience Technology Co ltd
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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
    • 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
    • C09G1/06—Other polishing compositions
    • C09G1/14—Other polishing compositions based on non-waxy substances
    • 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
    • C09G1/06—Other polishing compositions
    • C09G1/14—Other polishing compositions based on non-waxy substances
    • C09G1/16—Other polishing compositions based on non-waxy substances on natural or synthetic resins
    • 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
    • C09G1/06—Other polishing compositions
    • C09G1/14—Other polishing compositions based on non-waxy substances
    • C09G1/18—Other polishing compositions based on non-waxy substances on other substances

Abstract

The application relates to the field of chemical mechanical polishing, and particularly discloses a high-polishing-degree CMP polishing solution and a preparation method thereof. The CMP polishing solution with high polishing degree comprises 10 to 45 parts of abrasive, 2 to 7 parts of pH regulator, 0.03 to 0.3 part of surfactant, 0.5 to 2.5 parts of water-soluble cyclodextrin, 0.03 to 0.15 part of polyethylene glycol and 100 parts of water; the preparation method comprises the following steps: after the grinding material and the water are mixed uniformly, the water-soluble cyclodextrin and the polyethylene glycol are sequentially added and mixed uniformly, and then the pH regulator and the surfactant are added and mixed uniformly to prepare the CMP polishing solution with high polishing degree. The high-polishing-degree CMP polishing solution has the advantage of high polishing degree.

Description

High-polishing-degree CMP polishing solution and preparation method thereof
Technical Field
The application relates to the field of chemical mechanical polishing, in particular to a high-polishing-degree CMP polishing solution and a preparation method thereof.
Background
Since silica sol and silica gel are applied to polishing of silicon wafers for the first time, the CMP polishing solution becomes one of the most important and indispensable auxiliary materials in the semiconductor manufacturing industry. The polishing process of the silicon wafer is an intermediate process for preparing the device, the polishing effect greatly influences the quality of the semiconductor device, and the polishing process is used for eliminating the surface damage of the silicon wafer in the previous process and controlling the defects and impurities of the silicon wafer.
Because the foreign semiconductor technology is developed quickly, most of CMP polishing solution used in China is imported foreign polishing solution. At present, in order to promote the development of semiconductor technology in China, more and more enterprises are dedicated to the research of CMP polishing solution. For example, an alkaline silicon wafer polishing solution disclosed in publication No. CN1944559A, which has a pH of 8-13 and a particle diameter of 15nm-150nm, is prepared by mixing an abrasive 10-50%, a pH adjusting agent 1-6%, a surfactant 0.01-0.6%, and water 44-89%.
In view of the related art in the above, the inventors found that: since the polishing degree of the polishing solution is poor, it is necessary to research a CMP polishing solution with high polishing degree.
Disclosure of Invention
In order to improve the polishing degree of the polishing solution, the application provides a high-polishing-degree CMP polishing solution and a preparation method thereof.
In a first aspect, the present application provides a high-polishing CMP polishing solution, which adopts the following technical scheme:
every 100 weight portions of the polishing solution comprises 10 to 45 portions of abrasive, 2 to 7 portions of pH regulator, 0.03 to 0.3 portion of surfactant, 0.5 to 2.5 portions of water-soluble cyclodextrin, 0.03 to 0.15 portion of polyethylene glycol and 100 portions of water for complement.
By adopting the technical scheme, the water-soluble cyclodextrin and the polyethylene glycol are added into the CMP polishing solution, wherein the water-soluble cyclodextrin molecules are in a ring cylinder shape, the water-soluble cyclodextrin molecules have high water solubility, the inner cavity can contain a large amount of other substances, the hydroxyl of the polyethylene glycol can easily form hydrogen bonds, the water-soluble cyclodextrin molecules can interact with the water-soluble cyclodextrin molecules, the compatibility among raw materials is improved, the water-soluble cyclodextrin molecules and the polyethylene glycol are crosslinked to form a three-dimensional network structure, the polishing effect of the CMP polishing solution is improved, and the polishing degree of the CMP polishing solution is improved.
Preferably, the water-soluble cyclodextrin is at least two of methyl beta cyclodextrin, water-soluble polymeric cyclodextrin and salicylic acid cyclodextrin inclusion compound.
By adopting the technical scheme, the compatibility of the methyl beta cyclodextrin, the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin with the abrasive, the surfactant and the polyethylene glycol is higher, and the methyl beta cyclodextrin, the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin are compounded in pairs, so that the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
Preferably, the water-soluble cyclodextrin is a mixture of water-soluble polymeric cyclodextrin and salicylic acid cyclodextrin inclusion compound.
By adopting the technical scheme, the interaction between the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin inclusion compound is stronger, the compatibility among raw materials in the CMP polishing solution is improved, the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
Preferably, the weight ratio of the water-soluble polymeric cyclodextrin to the salicylic acid cyclodextrin inclusion compound is 1: (0.3-0.7).
By adopting the technical scheme, the application further enhances the interaction between the water-soluble cyclodextrin and the polyethylene glycol by controlling the weight ratio of the water-soluble polymeric cyclodextrin to the salicylic acid cyclodextrin, enhances the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol, and improves the polishing degree of the CMP polishing solution.
Preferably, the polyethylene glycol is selected from one or more of PEG-400, PEG-600, PEG-800 and PEG-1000.
By adopting the technical scheme, the compatibility of the PEG-400, the PEG-600, the PEG-800 and the PEG-1000 with the abrasive and the water-soluble cyclodextrin is higher, so that the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
Preferably, the polyethylene glycol is a mixture of PEG-600 and PEG-800.
By adopting the technical scheme, the PEG-600 and the PEG-800 are compounded and interact with each other, so that the interaction between the water-soluble cyclodextrin and the polyethylene glycol is further enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
Preferably, the weight ratio of the PEG-600 to the PEG-800 is (0.2-0.5): 1.
by adopting the technical scheme, the compatibility among the raw materials in the CMP polishing solution is further improved by controlling the weight ratio of the PEG-600 to the PEG-800, the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
Preferably, the abrasive is silica sol.
By adopting the technical scheme, the silica sol has higher water solubility and higher compatibility with water-soluble cyclodextrin and polyethylene glycol, and is suitable for being used as an abrasive of CMP polishing solution.
Preferably, the surfactant is a cationic surfactant.
By adopting the technical scheme, the cationic surfactant has positive charge and has better compatibility with the water-soluble cyclodextrin, the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
In a second aspect, the present application provides a method for preparing a CMP polishing solution with high polishing degree, which adopts the following technical scheme: a preparation method of a CMP polishing solution with high polishing degree comprises the following steps: after the grinding material and the water are mixed uniformly, the water-soluble cyclodextrin and the polyethylene glycol are sequentially added and mixed uniformly, and then the pH regulator and the surfactant are added and mixed uniformly to prepare the CMP polishing solution with high polishing degree.
Through adopting above-mentioned technical scheme, this application can form three-dimensional network structure through using water-soluble cyclodextrin can with polyethylene glycol interact, the cross-linking, and mix the raw materials in proper order, makes CMP polishing solution misce bene, has improved the polishing degree of CMP polishing solution.
In summary, the present application has the following beneficial effects:
1. because the water-soluble cyclodextrin and the polyethylene glycol are added into the CMP polishing solution, the polyethylene glycol can interact with the water-soluble cyclodextrin, the compatibility among the raw materials is improved, and the water-soluble cyclodextrin and the polyethylene glycol form a three-dimensional network structure through crosslinking, so that the polishing degree of the CMP polishing solution is improved;
2. according to the application, the methyl beta cyclodextrin, the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin are preferably compounded in pairs, and the methyl beta cyclodextrin, the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin have high compatibility with abrasive materials, surfactants and polyethylene glycol, so that the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved;
3. according to the method, the raw materials are mixed in sequence, so that the CMP polishing solution is uniformly mixed, the polishing degree of the CMP polishing solution is improved, and the method is simple to operate and convenient to prepare.
Detailed Description
The present application is further illustrated by the following examples, wherein the sources of the raw materials used in the present application are shown in Table 1.
TABLE 1 sources of raw materials used in the present application
Figure BDA0003036340360000031
Examples
Example 1
A CMP polishing solution with high polishing degree is prepared by the following steps: uniformly mixing 30kg of grinding material and 64.2kg of water, sequentially adding 1.5kg of water-soluble cyclodextrin and 0.1kg of polyethylene glycol, uniformly mixing, adding 4kg of pH regulator and 0.2kg of surfactant, and uniformly mixing to obtain the high-polishing-degree CMP polishing solution;
the abrasive is silica sol, the pH regulator is sodium hydroxide, the surfactant is anionic polyacrylamide, the polyethylene glycol is PEG-2000, and the water soluble cyclodextrin is hydroxypropyl beta cyclodextrin.
Examples 2 to 7
Examples 2 to 7 are based on example 1 and differ from example 1 only in that: the dosage of each raw material is different, and the specific table is shown in table 2.
TABLE 2 examples 1-7 sources of the respective raw materials
Figure BDA0003036340360000041
Example 8
Example 8 is based on example 1 and differs from example 1 only in that: the water-soluble cyclodextrin is a mixture of methyl beta cyclodextrin and water-soluble polymerized cyclodextrin, and the weight ratio of the methyl beta cyclodextrin to the water-soluble polymerized cyclodextrin is 1: 1.
example 9
Example 9 is based on example 1 and differs from example 1 only in that: the water-soluble cyclodextrin is a mixture of methyl beta cyclodextrin and a salicylic acid cyclodextrin inclusion compound, and the weight ratio of the methyl beta cyclodextrin to the salicylic acid cyclodextrin inclusion compound is 1: 1.
example 10
Example 10 is based on example 1 and differs from example 1 only in that: the water-soluble cyclodextrin is a mixture of water-soluble polymeric cyclodextrin and a salicylic acid cyclodextrin inclusion compound, and the weight ratio of the water-soluble polymeric cyclodextrin to the salicylic acid cyclodextrin inclusion compound is 1: 1.
examples 11 to 13
Examples 11 to 13 are based on example 10 and differ from example 10 only in that: the weight ratio of the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin inclusion compound is different, and the specific weight ratio is shown in table 3.
TABLE 3 examples 11-13 weight ratios of Water-soluble Polycyclodextrin and salicylic acid Cyclodextrin Inclusion complexes
Figure BDA0003036340360000051
Examples 14 to 17
Examples 14 to 17 are based on example 13 and differ from example 13 only in that: the polyethylene glycol used was of different kinds, as shown in Table 4.
TABLE 4 types of polyethylene glycols used in examples 14-17
Figure BDA0003036340360000052
Examples 18 to 21
Examples 18 to 21 are based on example 17 and differ from example 17 only in that: the polyethylene glycol used was a mixture of PEG-600 and PEG-800, and the weight ratio of PEG-600 to PEG-800 was varied, as shown in Table 5.
TABLE 5 examples 18-21PEG-600 and PEG-800 differ by weight ratio
Figure BDA0003036340360000053
Example 22
Example 22 is based on example 21 and differs from example 21 only in that: the surfactant is quaternary ammonium salt cationic surfactant.
Comparative example
Comparative example 1
Comparative example 1 is based on example 7 and differs from example 7 only in that: the water-soluble cyclodextrin is replaced by the abrasive with equal mass.
Comparative example 2
Comparative example 2 is based on example 7 and differs from example 7 only in that: equal mass of abrasive was substituted for the polyethylene glycol.
Comparative example 3
A CMP polishing solution with high polishing degree is prepared by the following steps: uniformly mixing 60kg of abrasive with 28.8kg of water, sequentially adding 5kg of water-soluble cyclodextrin and 2kg of polyethylene glycol, uniformly mixing, adding 4kg of pH regulator and 0.2kg of surfactant, and uniformly mixing to obtain the CMP polishing solution with high polishing degree;
the abrasive is silica sol, the pH regulator is sodium hydroxide, the surfactant is anionic polyacrylamide, the polyethylene glycol is PEG-2000, and the water soluble cyclodextrin is hydroxypropyl beta cyclodextrin.
Performance test
The high-polishing CMP polishing liquids prepared in examples 1 to 22 and comparative examples 1 to 3 were subjected to the following performance tests, respectively.
And (3) testing the polishing degree: the silicon wafers were polished using the high-polishing CMP polishing liquid prepared in the present application, polishing tests were performed on the silicon wafers corresponding to the CMP polishing liquids of examples 1 to 22 and comparative examples 1 to 3, and the surface roughness of the polished silicon wafers was tested using a New view 5022B model 3D surface profiler from Zygo corporation. The higher the surface roughness, the lower the polish, the lower the surface roughness, the higher the polish, and the test results are shown in Table 6.
The polishing machine used in polishing is a single-side polishing machine, the polishing machine is provided with 4 polishing heads, each polishing head can polish 4 silicon wafers, the polishing pressure in polishing is 32kPa, the rotating speed of a polishing turntable is 90r/min, the rotating speed of the polishing heads is 100r/min, the polishing time is 20min, the flow of polishing solution in polishing is 230ml/min, and the polishing temperature is 20 ℃. The polishing pad is a polyurethane foam cured polishing pad, and the polyurethane foam cured polishing pad is a 600-type polishing pad, which is purchased from SUB Rodel company; silicon wafers are available from Qian and Youngao Seisakusho Inc. in P type <100>, 100mm in diameter and 0.1-100 Ω cm in resistivity.
TABLE 6 surface roughness of examples 1 to 22 and comparative examples 1 to 3
Figure BDA0003036340360000061
The above data were analyzed.
The surface roughness of the silicon wafer polished by the high-polishing-degree CMP polishing solution prepared by the method is lower than 6, the surface roughness is at least 3.1A, the polishing degree of the CMP polishing solution is higher, and the data of comparative examples 1-7 show that example 1 is the best example of examples 1-7.
Comparing the data of examples 1 to 7 with the data of comparative examples 1 to 3, it can be seen that in the present application, water-soluble cyclodextrin and polyethylene glycol are added to the CMP polishing solution, wherein the water-soluble cyclodextrin molecule is in a ring cylinder shape, has high water solubility, and the inner cavity can accommodate a large amount of other substances, and the hydroxyl group of the polyethylene glycol is easy to form a hydrogen bond, and can interact with the water-soluble cyclodextrin, so that the compatibility between the raw materials is improved, and the water-soluble cyclodextrin and the polyethylene glycol are crosslinked to form a three-dimensional network structure, so that the polishing effect of the CMP polishing solution is improved, and the polishing degree of the CMP polishing solution is improved.
Comparing the data of examples 8-10 with the data of example 1, it can be seen that the compatibility of the methyl beta cyclodextrin, the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin with the abrasive, the surfactant and the polyethylene glycol is high, and the methyl beta cyclodextrin, the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin are compounded in pairs, so that the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
It can be seen from the data of comparative example 10 and examples 8 to 9 that the interaction between the water-soluble polymeric cyclodextrin and the salicylic acid cyclodextrin inclusion compound is strong, the compatibility between the raw materials in the CMP polishing solution is improved, the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
Comparing the data of examples 11-13 with the data of example 10, it can be seen that the present application further enhances the interaction between the water-soluble cyclodextrin and the polyethylene glycol by controlling the weight ratio of the water-soluble polymeric cyclodextrin to the salicylic acid cyclodextrin, enhances the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol, and improves the polishing degree of the CMP polishing solution. Wherein when the weight ratio of the water-soluble polymeric cyclodextrin to the salicylic acid cyclodextrin is 1: when the polishing rate is 0.5, the polishing degree of the CMP polishing solution is high.
Comparing the data of examples 14-17 and 13, it can be seen that the compatibility of PEG-400, PEG-600, PEG-800, and PEG-1000 with the abrasive and the water-soluble cyclodextrin is high, the interaction between the water-soluble cyclodextrin and the polyethylene glycol is enhanced, the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, and the polishing degree of the CMP polishing solution is improved.
Comparing the data of example 18 with the data of example 17 and example 15, it can be seen that the interaction between the water-soluble cyclodextrin and the polyethylene glycol is further enhanced by the use of the PEG-600 and PEG-800 in combination, and the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol is enhanced, so that the polishing degree of the CMP polishing solution is improved.
Comparing the data of examples 19-21 and example 18, it can be seen that the present application further improves the compatibility between the raw materials in the CMP polishing solution, enhances the interaction between the water-soluble cyclodextrin and the polyethylene glycol, enhances the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol, and improves the polishing degree of the CMP polishing solution by controlling the weight ratio of PEG-600 to PEG-800. Wherein when the weight ratio of PEG-600 to PEG-800 is 0.3: the polishing degree of the CMP polishing solution was higher at 1 hour.
The data of comparative example 22 and example 21 show that the quaternary ammonium salt cationic surfactant has a positive charge, has excellent compatibility with the water-soluble cyclodextrin, enhances the interaction between the water-soluble cyclodextrin and the polyethylene glycol, enhances the three-dimensional network structure formed by the water-soluble cyclodextrin and the polyethylene glycol, and improves the polishing degree of the CMP polishing solution.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (4)

1. A CMP polishing solution with high polishing degree is characterized in that every 100 weight portions of the polishing solution comprises 10-45 portions of abrasive, 2-7 portions of pH regulator, 0.03-0.3 portion of surfactant, 0.5-2.5 portions of water-soluble cyclodextrin, 0.03-0.15 portion of polyethylene glycol and water for complementing 100 portions;
the water-soluble cyclodextrin is a mixture of water-soluble polymeric cyclodextrin and a salicylic acid cyclodextrin inclusion compound;
the weight ratio of the water-soluble polymeric cyclodextrin to the salicylic acid cyclodextrin inclusion compound is 1: (0.3-0.7);
the polyethylene glycol is a mixture of PEG-600 and PEG-800;
the weight ratio of the PEG-600 to the PEG-800 is (0.2-0.5): 1.
2. the high-polishing-degree CMP polishing liquid according to claim 1, wherein: the abrasive is silica sol.
3. The high-polishing-degree CMP polishing liquid according to claim 1, wherein: the surfactant is a cationic surfactant.
4. A method for preparing a high-polishing CMP slurry according to any of claims 1 to 3, comprising the steps of: after the grinding material and the water are mixed uniformly, the water-soluble cyclodextrin and the polyethylene glycol are sequentially added and mixed uniformly, and then the pH regulator and the surfactant are added and mixed uniformly to prepare the CMP polishing solution with high polishing degree.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109251678A (en) * 2017-07-13 2019-01-22 安集微电子科技（上海）股份有限公司 A kind of chemical mechanical polishing liquid
CN110003798A (en) * 2019-05-20 2019-07-12 广东惠尔特纳米科技有限公司 A kind of polishing fluid and its preparation method and application

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US9505952B2 (en) * 2015-03-05 2016-11-29 Cabot Microelectronics Corporation Polishing composition containing ceria abrasive

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109251678A (en) * 2017-07-13 2019-01-22 安集微电子科技（上海）股份有限公司 A kind of chemical mechanical polishing liquid
CN110003798A (en) * 2019-05-20 2019-07-12 广东惠尔特纳米科技有限公司 A kind of polishing fluid and its preparation method and application

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