CN115895356B - Protective material for silicon wafer cutting and preparation method thereof - Google Patents
Protective material for silicon wafer cutting and preparation method thereof Download PDFInfo
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- 230000001681 protective effect Effects 0.000 title claims abstract description 55
- 239000000463 material Substances 0.000 title claims abstract description 47
- 238000005520 cutting process Methods 0.000 title claims abstract description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 42
- 239000010703 silicon Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 14
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- 238000000034 method Methods 0.000 claims abstract description 7
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
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- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 4
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
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- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims description 3
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- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 claims description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 2
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- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
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- 229920005591 polysilicon Polymers 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
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- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 1
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- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention provides a protective material for silicon wafer cutting and a preparation method thereof, and relates to the technical field of wafer cutting protection. The protective material for silicon wafer cutting comprises the following raw materials in parts by weight: 30-40 parts of water-soluble resin, 0.5-1 part of carbon nano tube, 7-12 parts of aromatic carboxylic anhydride, 3-8 parts of long-chain polyunsaturated fatty acid, 0.2-1 part of wetting agent, 0.1-1 part of defoamer, 10-20 parts of organic solvent and 40-60 parts of water. The protective material for silicon wafer cutting can rapidly form a film on the surface of a wafer, has high strength after film formation, has good heat resistance, can effectively prevent condensed silicon vapor or other scraps generated in the processing process from being deposited on the surface of a chip during wafer processing, improves the quality and reliability of products, and has good film removing property.
Description
Technical Field
The invention relates to the technical field of wafer cutting protection, in particular to a protective material for silicon wafer cutting and a preparation method thereof.
Background
Wafer refers to a silicon wafer used in the manufacture of a silicon semiconductor integrated circuit, and wafer dicing is a key process in the packaging process of the integrated circuit, and mainly, the whole wafer is divided into single chips according to the size of the chips by external force.
With the development and progress of technology, the current wafer dicing has been changed from the original simple blade dicing to the laser dicing, and the contact dicing is improved to the non-contact dicing. The laser cutting can greatly reduce the mechanical and stress damage to the chip in the cutting process, improves the product yield, and has become the mainstream in the current wafer cutting. Most of semiconductor chips are silicon chips, silicon is a brittle material, the strength of the chips can be influenced by corner fracture, the surface smoothness can be easily damaged in the cutting process, the pollution can be caused to the subsequent process, and in order to avoid the problems, a layer of protective film is required to be arranged in the wafer cutting process, so that a certain protective effect is achieved, and the subsequent trouble is avoided.
Researchers find that most of the wafer dicing protective solutions in the market can improve the dicing efficiency and stability of the wafer to a certain extent and avoid the problem of chipping or cracking and thermal stress, but many of the heat resistance in the protective solutions are not ideal, so that the research on the aspect is an important development direction of the industry in order to further widen the variety of the wafer dicing protective materials with heat resistance in the market.
Disclosure of Invention
In order to solve the problems that most of the wafer cutting protection liquids on the market at present in the background technology can improve the cutting efficiency and stability of wafers to a certain extent and avoid the problems of cutting chips or cracks and thermal stress, but a lot of heat resistance in the protection liquids is not ideal, the protection material for silicon wafer cutting provided by the invention has good film forming property and good heat resistance.
The specific scheme is as follows:
the protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 30-40 parts of water-soluble resin, 0.5-1 part of carbon nano tube, 7-12 parts of aromatic carboxylic anhydride, 3-8 parts of long-chain polyunsaturated fatty acid, 0.2-1 part of wetting agent, 0.1-1 part of defoamer, 10-20 parts of organic solvent and 40-60 parts of water.
The water-soluble resin is one or more of polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide, polyacrylic acid and polyethyleneimine.
In carrying out the above embodiment, it is preferable that the molecular weight of the water-soluble resin is more than 20000.
In carrying out the above embodiments, it is preferable that the carbon nanotubes have an average diameter of 5 to 30nm and a specific surface area of 200 to 350 m/g.
In carrying out the above embodiment, preferably, the aromatic carboxylic anhydride is one or more of trimellitic anhydride, pyromellitic anhydride, and biphenyltetracarboxylic dianhydride.
In practicing the above embodiments, the long chain polyunsaturated fatty acid is preferably one or more of omega-3 fatty acid, linoleic acid, eicosapentaenoic acid, docosahexaenoic acid.
In carrying out the above embodiment, preferably, the wetting agent is one or more of sulfonate, phosphate, monolauryl sulfate and dodecyl polyoxyethylene ether.
In carrying out the above embodiments, preferably, the antifoaming agent is one or more of polysilicon, siloxane, and polysiloxane.
In carrying out the above embodiment, preferably, the organic solvent is one or more of ethanol, n-propanol, isopropanol, propylene glycol methyl ether, ethylene glycol propyl ether, propyl formate, n-butyl acetate, and ethyl propionate.
The invention also provides a preparation method of the protective material for silicon wafer cutting, which comprises the following steps: adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoamer, organic solvent and water into a mixing container with a stirrer according to the proportion, stirring at the speed of 300-700rpm for 1.5-2.5h at normal temperature, and obtaining the protective material for silicon wafer cutting.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the protective material for silicon wafer cutting, the carbon nano tubes are added in raw material components, and a large number of physical crosslinking points can be formed between the carbon nano tubes and the water-soluble resin matrix, so that the heat resistance of the resin is improved, and meanwhile, the toughness of the resin is further enhanced; in addition, the carbon nano tube has stronger adsorption performance, thereby improving the adsorption of the protective material, and small molecular substances generated in the wafer cutting process can be adsorbed by the protective film formed by the protective material.
2. According to the protective material for silicon wafer cutting, the aromatic carboxylic anhydride is added into the raw material components, so that the heat resistance of the protective material is further improved, however, research and development personnel find that the film forming property is reduced due to the introduction of the aromatic carboxylic anhydride, and the adverse effect of the aromatic carboxylic anhydride on the film forming property of the protective material can be eliminated due to the addition of the long-chain polyunsaturated fatty acid, and through the synergistic effect of the aromatic carboxylic anhydride and the long-chain polyunsaturated fatty acid, the heat resistance of the protective material can be improved, and meanwhile, the film forming property of the protective material can also be improved.
3. The protective material for silicon wafer cutting can rapidly form a film on the surface of a wafer, has high strength after film formation, has good heat resistance, can effectively prevent condensed silicon vapor or other scraps generated in the processing process from being deposited on the surface of a chip during wafer processing, improves the quality and reliability of products, and has good film removing property.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The reagents of the examples and comparative examples are described below:
water-soluble resin: polyvinyl alcohol, guangzhou co-brightness chemical;
carbon nanotubes: korean LG;
aromatic carboxylic anhydride: trimellitic anhydride, northeast Cao Huaxue;
long chain polyunsaturated fatty acids: omega-3 fatty acids, shandong is looking for chemical industry;
wetting agent: monolauryl sulfate, a marchantia grosvenorii organism;
defoaming agent, polysiloxane and Shandong energy-accumulating chemical industry;
organic solvent, n-propanol, jinan Xueshun chemical industry.
It should be noted that, in the examples, specific techniques or conditions are not noted, and the reagents or apparatuses used, which are carried out according to techniques or conditions described in the literature in the field or according to the specifications of the products, are conventional products commercially available, and are not noted to manufacturers.
Example 1
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 30 parts of water-soluble resin, 1 part of carbon nano tube, 12 parts of aromatic carboxylic anhydride, 8 parts of long-chain polyunsaturated fatty acid, 1 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 60 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoaming agent, organic solvent and water into a reaction kettle, stirring at the speed of 300rpm for 2.5 hours at room temperature, filtering after stirring uniformly, and obtaining the protective material for cutting silicon wafers.
Example 2
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 0.5 part of carbon nano tube, 7 parts of aromatic carboxylic anhydride, 8 parts of long-chain polyunsaturated fatty acid, 1 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 60 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoaming agent, organic solvent and water into a reaction kettle, stirring at the speed of 700rpm for 1.5h at room temperature, filtering after stirring uniformly, and obtaining the protective material for silicon wafer cutting.
Example 3
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 1 part of carbon nano tube, 12 parts of aromatic carboxylic anhydride, 3 parts of long-chain polyunsaturated fatty acid, 0.2 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 60 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoaming agent, organic solvent and water into a reaction kettle, stirring at 400rpm for 1.5h at room temperature, filtering after stirring uniformly to obtain the protective material for silicon wafer cutting.
Example 4
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 1 part of carbon nano tube, 12 parts of aromatic carboxylic anhydride, 8 parts of long-chain polyunsaturated fatty acid, 1 part of wetting agent, 0.1 part of defoamer, 10 parts of organic solvent and 60 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoaming agent, organic solvent and water into a reaction kettle, stirring at 600rpm for 2h at room temperature, stirring uniformly, and filtering to obtain the protective material for silicon wafer cutting.
Example 5
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 1 part of carbon nano tube, 12 parts of aromatic carboxylic anhydride, 8 parts of long-chain polyunsaturated fatty acid, 0.2-1 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 40 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoaming agent, organic solvent and water into a reaction kettle, stirring at the speed of 700rpm for 2 hours at normal temperature, uniformly stirring, and filtering to obtain the protective material for silicon wafer cutting.
Comparative example 1
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 12 parts of aromatic carboxylic anhydride, 8 parts of long-chain polyunsaturated fatty acid, 0.2-1 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 40 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoamer, organic solvent and water into a reaction kettle, stirring at the speed of 700rpm for 2 hours at normal temperature, uniformly stirring, and filtering to obtain the protective material for silicon wafer cutting.
Comparative example 2
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 1 part of carbon nano tube, 8 parts of long-chain polyunsaturated fatty acid, 0.2-1 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 40 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, long-chain polyunsaturated fatty acid, wetting agent, defoamer, organic solvent and water into a reaction kettle, stirring at the speed of 700rpm for 2 hours at normal temperature, uniformly stirring, and filtering to obtain the protective material for silicon wafer cutting.
Comparative example 3
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 1 part of carbon nano tube, 12 parts of aromatic carboxylic anhydride, 0.2-1 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 40 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, wetting agent, defoamer, organic solvent and water into a reaction kettle, stirring at the speed of 700rpm for 2 hours at normal temperature, uniformly stirring, and filtering to obtain the protective material for silicon wafer cutting.
Comparative example 4
The protective material for silicon wafer cutting comprises the following raw materials in parts by mass: 40 parts of water-soluble resin, 1 part of carbon nano tube, 0.2-1 part of wetting agent, 1 part of defoamer, 20 parts of organic solvent and 40 parts of water.
According to the proportion, the preparation method comprises the following steps:
adding water-soluble resin, carbon nano tube, wetting agent, defoaming agent, organic solvent and water into a reaction kettle, stirring at the speed of 700rpm for 2 hours at normal temperature, uniformly stirring, and filtering to obtain the protective material for silicon wafer cutting.
The performances of the wafer cutting protection liquids obtained in examples 1 to 5 and comparative examples 1 to 4 were tested experimentally to verify the beneficial effects of the invention, and the specific tests are as follows:
1. film forming property test after the wafer cutting protective liquid of the above examples and comparative examples was obtained, the protective liquid was spin-uniformly coated on a glass slide, heated to about 110 ℃ for about 3 to 5 minutes, and observed whether the protective film was dried or not, and whether cracking was present or not.
2. After the wafer cutting protection liquid of the embodiment and the comparative example is obtained, the protection liquid is uniformly coated on a glass slide in a rotating way, and is heated to about 110 ℃ for about 3-5 minutes, so that a water-soluble protection film is formed on the surface of a silicon wafer by the protection liquid; each of the examples and comparative examples was baked in an oven at 300℃and 400℃for 30 minutes, respectively, and the state of the protective film was observed.
The test results are shown in Table 1:
TABLE 1
As can be seen from the test results of the points shown in Table 1, comparative example 1 was inferior in heat resistance test results to examples 1, which were shown to be dark yellow at 300℃and dark brown at 400℃as compared with examples 1 to 5, in which the raw material components were absent carbon nanotubes, indicating that the protective liquid was not resistant to high temperature. The invention is proved to be capable of forming a large number of physical crosslinking points with the water-soluble resin matrix by utilizing the carbon nano tube, thereby improving the heat resistance of the resin.
On the one hand, comparative example 3, which lacks long-chain polyunsaturated fatty acids in the raw material components, was found to have a poor film-forming effect and to exhibit cracking, compared with examples 1 to 5; for this purpose, comparative example 2 was designed, which contains long-chain polyunsaturated fatty acids and lacks aromatic carboxylic acid anhydrides, and which has good film formation compared with comparative example 3; in addition, comparative example 4, which does not contain a long-chain polyunsaturated fatty acid or an aromatic carboxylic anhydride, has a good film-forming effect as compared with comparative example 3. It was found from a series of comparisons that the incorporation of aromatic carboxylic anhydrides resulted in a decrease in film forming properties, whereas the addition of long chain polyunsaturated fatty acids eliminated the adverse effect of the aromatic carboxylic anhydrides on the film forming properties of the protective materials.
On the other hand, it was found that the heat resistance of comparative example 3 was due to comparative examples 2 and 4. This proves that the addition of the aromatic carboxylic anhydride further improves the heat resistance of the protective material.
From this, it is found that the synergistic effect of the long-chain polyunsaturated fatty acid and the aromatic carboxylic anhydride can improve the heat resistance of the protective material and the film forming property.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (4)
1. The protective material for silicon wafer cutting is characterized by comprising the following raw materials in parts by weight: 30-40 parts of water-soluble resin, 0.5-1 part of carbon nano tube, 7-12 parts of aromatic carboxylic anhydride, 3-8 parts of long-chain polyunsaturated fatty acid, 0.2-1 part of wetting agent, 0.1-1 part of defoamer, 10-20 parts of organic solvent and 40-60 parts of water;
the carbon nanotubes have an average diameter of 5-30nm and 200m 2 /g-350m 2 Specific surface area/g;
the molecular weight of the water-soluble resin is more than 20000, and the water-soluble resin is polyvinyl alcohol;
the long chain polyunsaturated fatty acid is an omega-3 fatty acid;
the aromatic carboxylic anhydride is one or more of trimellitic anhydride, pyromellitic anhydride and biphenyl tetracarboxylic dianhydride;
the organic solvent is one or more of ethanol, n-propanol, isopropanol, propylene glycol methyl ether, ethylene glycol propyl ether, propyl formate, n-butyl acetate and ethyl propionate.
2. The protective material for silicon wafer dicing of claim 1, wherein the wetting agent is one or more of sulfonate, phosphate, monolauryl sulfate, and dodecyl polyoxyethylene ether.
3. The protective material for silicon wafer dicing of claim 1, wherein the antifoaming agent is one or more of polysilicon and siloxane.
4. A method for preparing a protective material for silicon wafer dicing according to any one of claims 1 to 3, characterized by comprising the steps of: adding water-soluble resin, carbon nano tube, aromatic carboxylic anhydride, long-chain polyunsaturated fatty acid, wetting agent, defoamer, organic solvent and water into a mixing container with a stirrer according to the proportion, stirring at the speed of 300-700rpm at normal temperature for 1.5-2.5-h, and obtaining the protective material for silicon wafer cutting.
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