CN115975711A - Dispersing property improving and foam type diamond wire silicon wafer cutting fluid reducing and preparation method thereof - Google Patents
Dispersing property improving and foam type diamond wire silicon wafer cutting fluid reducing and preparation method thereof Download PDFInfo
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- CN115975711A CN115975711A CN202211583159.1A CN202211583159A CN115975711A CN 115975711 A CN115975711 A CN 115975711A CN 202211583159 A CN202211583159 A CN 202211583159A CN 115975711 A CN115975711 A CN 115975711A
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- cutting fluid
- diamond wire
- silicon wafer
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000002173 cutting fluid Substances 0.000 title claims abstract description 92
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 80
- 239000010703 silicon Substances 0.000 title claims abstract description 80
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 66
- 239000010432 diamond Substances 0.000 title claims abstract description 66
- 239000006260 foam Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 36
- 239000000314 lubricant Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical class O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 29
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 29
- 239000002738 chelating agent Substances 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 26
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 26
- 150000002334 glycols Chemical class 0.000 claims abstract description 24
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 235000012431 wafers Nutrition 0.000 claims description 74
- 235000006708 antioxidants Nutrition 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 239000002518 antifoaming agent Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 26
- 229920000570 polyether Polymers 0.000 claims description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 24
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 22
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 230000000149 penetrating effect Effects 0.000 claims description 21
- 229920005862 polyol Polymers 0.000 claims description 19
- 150000003077 polyols Chemical class 0.000 claims description 19
- 238000001914 filtration Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- -1 polyoxypropylene Polymers 0.000 claims description 13
- 241001122767 Theaceae Species 0.000 claims description 12
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 12
- 235000013824 polyphenols Nutrition 0.000 claims description 12
- 229920001451 polypropylene glycol Polymers 0.000 claims description 12
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims description 10
- 230000002829 reductive effect Effects 0.000 claims description 8
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 7
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 7
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 4
- USYAMXSCYLGBPT-UHFFFAOYSA-L 3-carboxy-3-hydroxypentanedioate;tin(2+) Chemical compound [Sn+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O USYAMXSCYLGBPT-UHFFFAOYSA-L 0.000 claims description 4
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 4
- CRSBERNSMYQZNG-UHFFFAOYSA-N 1 -dodecene Natural products CCCCCCCCCCC=C CRSBERNSMYQZNG-UHFFFAOYSA-N 0.000 claims description 3
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 3
- 229930003268 Vitamin C Natural products 0.000 claims description 3
- 235000019262 disodium citrate Nutrition 0.000 claims description 3
- 239000002526 disodium citrate Substances 0.000 claims description 3
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 claims description 3
- 229940069096 dodecene Drugs 0.000 claims description 3
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 3
- 235000019154 vitamin C Nutrition 0.000 claims description 3
- 239000011718 vitamin C Substances 0.000 claims description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000391 magnesium silicate Substances 0.000 claims description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 2
- 235000019792 magnesium silicate Nutrition 0.000 claims description 2
- 238000007151 ring opening polymerisation reaction Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000013530 defoamer Substances 0.000 abstract description 3
- 238000005520 cutting process Methods 0.000 description 28
- 239000011863 silicon-based powder Substances 0.000 description 17
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000035699 permeability Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- 230000001050 lubricating effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- UWJDLABDOBGBFS-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;sodium Chemical compound [Na].[Na].OC(=O)CC(O)(C(O)=O)CC(O)=O UWJDLABDOBGBFS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 210000000056 organ Anatomy 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003254 anti-foaming effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- DTPCFIHYWYONMD-UHFFFAOYSA-N decaethylene glycol Polymers OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO DTPCFIHYWYONMD-UHFFFAOYSA-N 0.000 description 1
- 125000002704 decyl 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])* 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Landscapes
- Lubricants (AREA)
Abstract
The invention belongs to the technical field of diamond wire silicon wafer cutting fluid and preparation thereof, and particularly relates to foam type diamond wire silicon wafer cutting fluid capable of improving dispersibility and reducing foam and a preparation method thereof. The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is composed of the following raw materials in percentage by mass: 30-50% of lubricant, 1-5% of dispersant, 10-20% of penetrant, 0.5-5% of defoamer, 1-5% of chelating agent, 0.5-2% of antioxidant and the balance of deionized water; the dispersant is polyethylene glycol derivative containing quaternary ammonium salt, and the number average molecular weight of the dispersant is 500-700. The invention provides a diamond wire silicon wafer cutting fluid, which belongs to a low-foam cutting fluid and has the characteristic of high dispersibility; the invention also provides a preparation method of the composition.
Description
Technical Field
The invention belongs to the technical field of diamond wire silicon wafer cutting fluid and preparation thereof, and particularly relates to a foam type diamond wire silicon wafer cutting fluid capable of improving dispersibility and reducing foam and a preparation method thereof.
Background
At present, the silicon wafer cutting process mainly comprises two modes of free abrasive mortar cutting and diamond wire cutting, compared with the traditional free abrasive mortar cutting, the diamond wire cutting has the advantages of high cutting speed (4-5 times of cutting speed), high wafer yield (the wafer yield of the silicon wafer exceeds 15-20%), energy conservation (two thirds of consumed water and electricity is reduced), small pollution and the like, so that the production cost of silicon wafer production enterprises can be greatly reduced, the photovoltaic installation yield is improved, and the diamond wire cutting process is gradually and widely applied by the industry. With the rapid development of the photovoltaic industry, the demand of silicon wafers as basic materials is increased, the important process of silicon wafer processing is slicing, the defects of silicon wafer stress, surface layer and subsurface layer damage, edge breakage and the like generated during slicing can seriously affect the conversion efficiency of the photovoltaic cell, and the performance of the cutting fluid is one of the key factors influencing the cutting efficiency and quality of the silicon wafers.
The diamond wire cutting fluid should have the following effects: (1) lubrication: the cutting fluid should timely penetrate into the wire mesh and the silicon wafer, and a layer of lubricating protective film is formed between the wire mesh and the scraps, so that the cutting resistance is reduced, and the damage, the wire mark and the hidden crack caused by the diamond wire are reduced; (2) cooling effect: the high heat generated by cutting is partially taken away by the cutting fluid, and most of the rest heat is absorbed by the crystalline silicon, so that local silicon chip deformation can be caused by high temperature, and therefore, the cutting fluid needs to have good heat transfer and cooling performance; (3) dispersing action: silicon powder cuttings formed by cutting need to be dispersed in time, and the silicon chips are prevented from being aggregated to form clusters, so that the silicon chips are scratched and even wire meshes are broken; (4) cleaning action: a large amount of scraps and silicon powder generated in the cutting process are easy to form adhesion agglomeration, so that the scraps can be wrapped by cutting liquid, and the scraps are easy to fall off and clean; (5) The cutting fluid also has the capabilities of rust prevention and bacteriostasis, and production interruption caused by corrosion of equipment in the long-term use process is avoided.
Just as above, because the linear velocity of the diamond is increased in multiples, the amount of the cut silicon powder is also increased in multiples, and if the silicon powder is not wetted and dispersed in time, the silicon powder is gathered on the surface of the silicon wafer to cause scratching of the silicon wafer and even breakage of a wire mesh, so that the requirement on the dispersibility of the cutting fluid is higher. In addition, a large amount of foam is often generated when the silicon wafer is cut and cleaned, cutting efficiency is seriously influenced, cutting liquid is excessively consumed, cost is increased, mechanical equipment is damaged along with the lapse of time, and the mechanical life is shortened.
Disclosure of Invention
The invention aims to solve the technical problem of providing a diamond wire silicon wafer cutting fluid, belonging to a low-foam cutting fluid with high dispersibility; the invention also provides a preparation method of the composition.
The invention relates to a silicon wafer cutting fluid for improving dispersibility and reducing foam type diamond wires, which is prepared from the following raw materials in percentage by mass:
the balance of deionized water;
the dispersant is polyethylene glycol derivative containing quaternary ammonium salt, and the number average molecular weight of the polyethylene glycol derivative is 500-700, preferably 500, 600 and 700.
The lubricant is a mixed compound of trans-block polyether polyol 1740 and trans-block polyether polyol 1720 in a weight ratio of 1/2-2/1.
The cloud point of a 1% aqueous solution of trans-block polyether polyol 1740 is 50. + -. 2 ℃ and the cloud point of a 1% aqueous solution of trans-block polyether polyol 1720 is 35. + -. 2 ℃.
The dispersant is an intermediate generated by ring-opening polymerization of N, N' -dimethylethanolamine as an initiator and ethylene oxide under the action of a catalyst potassium hydroxide, and is desalted by a magnesium silicate adsorbent and finally neutralized with acetic acid to generate the polyethylene glycol derivative containing quaternary ammonium salt. The quaternary ammonium salt has the formula R 1 R 2 R 3 NX, wherein R 1 And R 2 Are all-CH 3 Structure R 3 Is- (CH) 2 )-O-(CH 2 -CH 2 -O) n-H structure, X is CH 3 CH 2 COO - Structure).
The penetrating agent is one or more of isomeric octanol polyoxyethylene ether, isomeric decanol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether.
The defoaming agent is one or more of polyoxypropylene ether, GPES type stearate polyoxyethylene polyoxypropylene glycerol ether and dodecene glycol polyether.
The chelating agent is one or more of disodium EDTA, tetrasodium EDTA, and disodium citrate.
The antioxidant is water soluble antioxidant, and comprises one or more of vitamin C, tea polyphenols, and disodium stannous citrate.
The preparation method of the foam type diamond wire silicon wafer cutting fluid capable of improving the dispersibility and reducing the foam type diamond wire silicon wafer cutting fluid comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35-40 ℃ while stirring;
(2) Sequentially adding a lubricant, a dispersing agent, a penetrating agent, a defoaming agent, a chelating agent and an antioxidant into a reaction kettle, stirring for 1-2 h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
The lubricant added in the formula is a compound of trans-block polyether polyol 1740 and 1720 mixed according to the weight ratio of 1/2-2/1, and the compound has excellent low foaming property and lubricating property and is good in compound property with other formula products. The trans-block polyether polyol 1740 is preferably produced by Shanghai east Chemicals, inc. Trans-block polyether polyol 1720 is preferably manufactured by Shanghai east Chemicals, inc.
The dispersing agent in the formula of the invention adopts the polyethylene glycol derivative containing quaternary ammonium salt, and is adsorbed on the surface of the cut silicon powder, the dispersibility of the silicon powder in the cutting liquid is greatly improved due to electrostatic repulsion acting force and steric hindrance effect, and the quaternary ammonium salt contained in the polyethylene glycol derivative not only has high-efficiency bactericidal performance, but also has low toxicity and no irritation to human organs and skin.
The penetrant in the formula disclosed by the invention is preferably the isomeric alcohol polyoxyethylene ether, so that the penetrant has excellent permeability and emulsibility, and has low foam height and poor foam stability compared with the traditional fatty alcohol polyoxyethylene ether penetrant.
The defoamer in the formula of the invention is preferably polyoxypropylene ether, which can play long-term defoaming and foam inhibiting roles in the formula of the cutting fluid, the cutting fluid does not adopt the existing modified silicon polyether defoaming agent because silicon spots are easily generated on the surface of a silicon wafer.
The chelating agent in the formula is one or more of EDTA disodium, EDTA tetrasodium and citric acid disodium, and iron ions generated in the diamond wire cutting process are removed in the use process of the cutting fluid, so that the pollution to the surface of the silicon wafer is further reduced.
Compared with the prior art, the invention has the beneficial effects that:
(1) The cutting fluid disclosed by the invention takes the trans-block polyether 1740/1720 compound as a lubricant, the cutting fluid permeates into a cutting gap in the diamond wire cutting process, 1740/1720 precipitates and adheres between a wire mesh and a silicon wafer and between the wire mesh and silicon powder due to high temperature generated by high-speed friction, a reversible lubricating film is formed on the surface, the cutting resistance is reduced, the damage degree of a cutting wire and the silicon wafer is greatly reduced, and the compound lubricant has excellent low foamability and defoaming property and can reduce the generation of foams.
(2) According to the formula of the cutting fluid, the polyethylene glycol derivative containing quaternary ammonium salt is used as a dispersing agent, the cutting fluid rapidly permeates into a cutting gap in the cutting process, the polyethylene glycol derivative is rapidly adsorbed on the surface of silicon powder by using hydrogen bonds and other acting forces, the silicon powder is dispersed in time due to the dual functions of electrostatic repulsion acting force and steric hindrance effect, aggregation of the silicon powder is prevented, and the quaternary ammonium salt contained in the polyethylene glycol derivative has high-efficiency sterilization performance, low toxicity and no irritation to human organs and skin.
(3) In the formula of the cutting fluid, the isomeric alcohol polyoxyethylene ether is used as a penetrating agent, so that the cutting fluid has excellent permeability and emulsibility, and has low foam height, poor foam stability and higher defoaming speed compared with the traditional fatty alcohol polyoxyethylene ether penetrating agent.
(4) The lubricant, the penetrating agent, the dispersant and the defoaming agent in the formula of the cutting fluid are all polyethers, the compatibility is good, and the prepared cutting fluid has strong stability.
Detailed Description
The present invention is further illustrated by the following examples. The following raw material reagents are all commercially available products.
Example 1
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is composed of the following raw materials in percentage by mass:
lubricant: trans-block polyether polyol 1740 and 1720 mixed 1/1 by weight ratio, 35%;
dispersing agent: a polyethylene glycol derivative containing a quaternary ammonium salt, the number average molecular weight of which is 500,2.5%;
penetrant: isomeric decyl alcohol polyoxyethylene ether, 20%;
defoaming agent: polyoxypropylene ether, 2%;
chelating agent: disodium EDTA, 2.5%;
antioxidant: 1.0% of tea polyphenol;
deionized water: 37 percent; the sum of the total amount of all the components is 100 percent.
The preparation method of the foam type diamond wire silicon wafer cutting fluid capable of improving the dispersibility and reducing the foam type diamond wire silicon wafer cutting fluid comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 1h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Example 2
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer consists of the following raw materials in percentage by mass:
lubricant: a 1/1 mixed 1/1 blend of trans-block polyether polyols 1740 and 1720;
dispersing agent: a polyethylene glycol derivative containing a quaternary ammonium salt, the number average molecular weight of which is 500,2.5%;
penetrant: isomeric decyl alcohol polyoxyethylene ether, 16%;
defoaming agent: 1% of polyoxypropylene ether and 1% of dodecene glycol polyether;
chelating agent: tetrasodium EDTA, 1%;
antioxidant: disodium stannous citrate, 2.0%;
deionized water: 36.5 percent; the sum of the total amount of all the components is 100 percent.
The preparation method of the foam type diamond wire silicon wafer cutting fluid capable of improving the dispersibility and reducing the foam type diamond wire silicon wafer cutting fluid comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 40 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 2 hours, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Example 3
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is composed of the following raw materials in percentage by mass:
lubricant: trans-block polyether polyol 1740 and 1720, mixed 1/1 weight ratio, 45%;
dispersing agent: a polyethylene glycol derivative containing a quaternary ammonium salt, the number average molecular weight of which is 500,3%;
and (3) penetrant: isomeric dodecyl alcohol polyoxyethylene ether, 15%;
defoaming agent: GPES type stearate polyoxyethylene polyoxypropylene glycerol ether, 2%;
chelating agent: disodium EDTA, 2%;
antioxidant: 0.5 percent of vitamin C, 0.5 percent of tea polyphenol and 0.5 percent of disodium stannous citrate;
deionized water: 31.5 percent; the sum of the total amount of all the components is 100 percent.
The preparation method of the silicon wafer cutting fluid for improving the dispersibility and reducing the foam type diamond wire comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 1.5 hours, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Example 4
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is composed of the following raw materials in percentage by mass:
lubricant: trans-block polyether polyol 1740 and 1720, mixed at a 1/1 weight ratio, 50%;
dispersing agent: a polyethylene glycol derivative containing a quaternary ammonium salt, the number average molecular weight of which is 500,1%;
penetrant: 6% of isomeric tridecanol polyoxyethylene ether and 6% of isomeric tridecanol polyoxyethylene ether;
defoaming agent: polyoxypropylene ether, 2%;
chelating agent: disodium EDTA, 2.5%;
antioxidant: 1.5 percent of tea polyphenol;
deionized water: 31 percent; the sum of the total amount of all the components is 100 percent.
The preparation method of the foam type diamond wire silicon wafer cutting fluid capable of improving the dispersibility and reducing the foam type diamond wire silicon wafer cutting fluid comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 1h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Example 5
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer consists of the following raw materials in percentage by mass:
lubricant: trans-block polyether polyol 1740 and 1720, mixed 1/1 weight ratio, 45%;
dispersing agent: a polyethylene glycol derivative containing a quaternary ammonium salt, the number average molecular weight of which is 500,5%;
penetrant: 15% of isomeric octanol polyoxyethylene ether;
defoaming agent: polyoxypropylene ether, 2%;
chelating agent: disodium EDTA, 5%;
antioxidant: 1.0% of tea polyphenol;
deionized water: 27%; the sum of the total amount of all the components is 100 percent.
The preparation method of the silicon wafer cutting fluid for improving the dispersibility and reducing the foam type diamond wire comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 1h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Example 6
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is composed of the following raw materials in percentage by mass:
lubricant: trans-block polyether polyol 1740 and 1720, mixed at a 1/1 weight ratio, 30%;
dispersing agent: polyethylene glycol derivatives containing quaternary ammonium salt, the number average molecular weight is 700,3%;
and (3) penetrant: isomeric dodecyl alcohol polyoxyethylene ether, 10%;
defoaming agent: 5% of polyoxypropylene ether;
chelating agent: 1% of EDTA disodium and 1% of citric acid disodium;
antioxidant: 0.5% of tea polyphenol;
deionized water: 49.5 percent; the sum of the total amount of all the components is 100 percent.
The preparation method of the foam type diamond wire silicon wafer cutting fluid capable of improving the dispersibility and reducing the foam type diamond wire silicon wafer cutting fluid comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 1h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Example 7
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is composed of the following raw materials in percentage by mass:
lubricant: trans-block polyether polyol 1740 and 1720, 1/2 mixed formulation by weight ratio, 45%;
dispersing agent: a polyethylene glycol derivative containing a quaternary ammonium salt, the number average molecular weight of which is 600,3%;
penetrant: isomeric dodecyl alcohol polyoxyethylene ether, 15%;
defoaming agent: polyoxypropylene ether, 0.5%;
chelating agent: disodium citrate, 3.5%;
antioxidant: 1.5 percent of tea polyphenol;
deionized water: 31.5 percent; the sum of the total amount of all the components is 100 percent.
The preparation method of the foam type diamond wire silicon wafer cutting fluid capable of improving the dispersibility and reducing the foam type diamond wire silicon wafer cutting fluid comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 1h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Example 8
The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is composed of the following raw materials in percentage by mass:
lubricant: a 2/1 mixed blend of trans-block polyether polyols 1740 and 1720;
dispersing agent: a polyethylene glycol derivative containing a quaternary ammonium salt, the number average molecular weight of which is 500,2.5%;
penetrant: isomeric decyl alcohol polyoxyethylene ether, 18%;
defoaming agent: polyoxypropylene ether, 2%;
chelating agent: disodium EDTA, 2.5%;
antioxidant: 1.0% of tea polyphenol;
deionized water: 39 percent; the sum of the total amount of all the components is 100 percent.
The preparation method of the foam type diamond wire silicon wafer cutting fluid capable of improving the dispersibility and reducing the foam type diamond wire silicon wafer cutting fluid comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35 ℃ while stirring;
(2) And sequentially adding the lubricant, the dispersing agent, the penetrating agent, the defoaming agent, the chelating agent and the antioxidant into the reaction kettle, stirring for 1h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
Comparative example 1
A diamond wire silicon wafer cutting fluid comprises the following raw materials: 45% of lubricant (1740 and 1720 mass ratio of 1/1), 3% of dispersant (polyethylene glycol 500), 15% of penetrating agent (isomeric dodecyl alcohol polyoxyethylene ether), 2% of defoaming agent (polyoxypropylene ether), 2% of chelating agent (EDTA disodium), 1.5% of antioxidant (tea polyphenol) and 31.5% of deionized water. The sum of the total amount of all the components is 100 percent.
The preparation method comprises the following steps:
(1) Adding deionized water into a reaction kettle according to a certain proportion, and heating to 35 ℃ while stirring;
(2) Sequentially adding a lubricant, a dispersing agent, a penetrating agent, a defoaming agent, a chelating agent and an antioxidant into the reaction kettle, stirring for 1 hour, and filtering to obtain the silicon wafer cutting fluid.
Comparative example 2
A diamond wire silicon wafer cutting fluid comprises the following raw materials: 45% of lubricant (1740-1720 mass ratio of 1/1), 3% of dispersant (polyethylene glycol derivative containing quaternary ammonium salt and with number average molecular weight of 500), 15% of penetrating agent (isomeric dodecyl alcohol polyoxyethylene ether), 2% of chelating agent (EDTA disodium), 1.5% of antioxidant (tea polyphenol) and 33.5% of deionized water. The sum of the total amount of all the components is 100 percent.
The preparation method comprises the following steps:
(1) Adding deionized water into a reaction kettle according to a certain proportion, and heating to 35 ℃ while stirring;
(2) Sequentially adding a lubricant, a dispersing agent, a penetrating agent, a chelating agent and an antioxidant into the reaction kettle, stirring for 1 hour, and filtering to obtain the silicon wafer cutting fluid.
Comparative example 3
A diamond wire silicon wafer cutting fluid comprises the following raw materials: 45% of a lubricant (1720), 3% of a dispersant (a polyethylene glycol derivative containing quaternary ammonium salt and having a number average molecular weight of 500), 15% of a penetrating agent (isomeric decyl polyoxyethylene ether), 2% of a defoaming agent (polyoxypropylene ether), 2% of a chelating agent (EDTA disodium), 1.5% of an antioxidant (tea polyphenol) and 31.5% of deionized water. The sum of the total amount of all the components is 100 percent.
The preparation method comprises the following steps:
(1) Adding deionized water into a reaction kettle according to a certain proportion, and heating to 35 ℃ while stirring;
(2) Sequentially adding a lubricant, a dispersing agent, a penetrating agent, a defoaming agent, a chelating agent and an antioxidant into the reaction kettle, stirring for 1 hour, and filtering to obtain the silicon wafer cutting fluid.
Firstly, the performance parameters of the diamond wire silicon wafer cutting fluid prepared in the above examples 1-8 and comparative examples 1-4 are detected under the following detection conditions:
carrying out conductivity detection on the cutting fluid according to 1% diluent at 25 +/-1 ℃; the instrument and model number is S230SevenCompact conductivity meter.
Cutting fluid is mixed according to the proportion of 1:1000, performing COD detection on the diluted solution; instrument type 6B-300 water quality quick-measuring instrument
Detecting the wetting time of the cutting fluid at 25 +/-1 ℃ according to 0.1% of diluent; the method is a canvas settlement permeability test method.
Measuring the circulating foam height and defoaming time of the cutting fluid according to 0.5% of diluent, wherein the initial volume is 1000mL at 23 ℃ for 15 min; the instrument and the model are HCR-700 type metal cutting fluid anti-foaming determinator.
Measuring the suspension rate of cutting fluid and silicon powder at 25 +/-1 ℃ for 24h, wherein the mass ratio of the cutting fluid to the silicon powder is 1; the dispersibility is characterized by measuring the suspension capacity of the cutting liquid to the silicon powder, and the cutting liquid and the silicon powder are mixed according to the weight ratio of 1: after uniformly mixing in a mass ratio of 1, standing in a 100mL measuring cylinder, and recording the sedimentation height h of the silicon powder in the cutting fluid, wherein the suspension rate is = (100-h) × 100%/100.
The above detection results are shown in table 1.
TABLE 1 test results
Secondly, the diamond wire silicon wafer cutting fluids prepared in the above examples and comparative examples are diluted by 300 times with deionized water, and then silicon crystals of the same material are cut, and the detection results are shown in table 2.
Table 2 cutting data results
As can be seen from table 1, the cutting fluid using the polyethylene glycol derivative containing the quaternary ammonium salt as the dispersant has better dispersing effect than the polyethylene glycol dispersant, the effect of preventing silicon powder from aggregating on the silicon wafer is better, and the cutting fluid without the defoamer also has better foam inhibition and defoaming performance.
As can be seen from Table 2, the cutting fluid of the present invention has excellent permeability and lubricity, low occurrence of surface defects, and low wire breakage rate and cut-adding rate; compared with polyethylene glycol, the polyethylene glycol derivative containing quaternary ammonium salt has better dispersibility, improves the cleaning efficiency and reduces the dirty ratio. Since 1720 is less hydrophilic than 1740 itself, the staining rate is slightly higher than that of 1740/1720 mixed lubricants.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.
Claims (9)
1. The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer is characterized in that: the composite material is prepared from the following raw materials in percentage by mass:
the balance of deionized water;
the dispersant is a polyethylene glycol derivative containing quaternary ammonium salt, and the number average molecular weight of the polyethylene glycol derivative is 500-700.
2. The silicon wafer cutting fluid for improving the dispersibility and reducing the foam type diamond wire according to claim 1, which is characterized in that: the lubricant is a mixed compound of trans-block polyether polyol 1740 and trans-block polyether polyol 1720 in a weight ratio of 1/2-2/1.
3. The cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafers according to claim 2 is characterized in that: the cloud point of a 1% aqueous solution of trans-block polyether polyol 1740 is 50. + -. 2 ℃ and the cloud point of a 1% aqueous solution of trans-block polyether polyol 1720 is 35. + -. 2 ℃.
4. The cutting fluid for improving the dispersity and reducing the foam type diamond wire silicon wafers according to claim 1 is characterized in that: the dispersant is an intermediate generated by ring-opening polymerization of N, N' -dimethylethanolamine as an initiator and ethylene oxide under the action of a catalyst, and is desalted by a magnesium silicate adsorbent and finally neutralized with acetic acid to generate the polyethylene glycol derivative containing the quaternary ammonium salt.
5. The silicon wafer cutting fluid for improving the dispersibility and reducing the foam type diamond wire according to claim 1, which is characterized in that: the penetrating agent is one or more of isomeric octanol polyoxyethylene ether, isomeric decanol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether.
6. The silicon wafer cutting fluid for improving the dispersibility and reducing the foam type diamond wire according to claim 1, which is characterized in that: the defoaming agent is one or more of polyoxypropylene ether, GPES type stearate polyoxyethylene polyoxypropylene glycerol ether and dodecene glycol polyether.
7. The silicon wafer cutting fluid for improving the dispersibility and reducing the foam type diamond wire according to claim 1, which is characterized in that: the chelating agent is one or more of disodium EDTA, tetrasodium EDTA, and disodium citrate.
8. The cutting fluid for improving the dispersity and reducing the foam type diamond wire silicon wafers according to claim 1 is characterized in that: the antioxidant is water-soluble antioxidant, and comprises one or more of vitamin C, tea polyphenols, and disodium stannous citrate.
9. The preparation method of the foam type diamond wire silicon wafer cutting fluid with improved dispersibility and reduced foam type according to any one of claims 1 to 8, which is characterized by comprising the following steps: the method comprises the following steps:
(1) Adding deionized water into a reaction kettle according to the formula proportion, and heating to 35-40 ℃ while stirring;
(2) Sequentially adding a lubricant, a dispersing agent, a penetrating agent, a defoaming agent, a chelating agent and an antioxidant into a reaction kettle, stirring for 1-2 h, and filtering to obtain the cutting fluid for improving the dispersibility and reducing the foam type diamond wire silicon wafer.
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| CN113549488A (en) * | 2021-08-03 | 2021-10-26 | 江苏捷捷半导体新材料有限公司 | Large-size silicon wafer diamond wire cutting liquid |
| CN114164040A (en) * | 2021-12-15 | 2022-03-11 | 上海东大化学有限公司 | Low-foam environment-friendly fully-synthetic water-based cutting fluid and preparation method thereof |
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| CN101935576A (en) * | 2010-10-09 | 2011-01-05 | 辽宁奥克化学股份有限公司 | Cutting fluid with anti-oxidation performance, preparation method and application thereof |
| CN111116888A (en) * | 2019-12-20 | 2020-05-08 | 万华化学集团股份有限公司 | Quaternary ammonium salt type dispersing agent and preparation method thereof, and preparation method of inorganic modified polyether polyol |
| CN113549488A (en) * | 2021-08-03 | 2021-10-26 | 江苏捷捷半导体新材料有限公司 | Large-size silicon wafer diamond wire cutting liquid |
| CN114164040A (en) * | 2021-12-15 | 2022-03-11 | 上海东大化学有限公司 | Low-foam environment-friendly fully-synthetic water-based cutting fluid and preparation method thereof |
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