CN115386297A - Polishing solution for wafer polishing and preparation method thereof - Google Patents
Polishing solution for wafer polishing and preparation method thereof Download PDFInfo
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- CN115386297A CN115386297A CN202210884062.8A CN202210884062A CN115386297A CN 115386297 A CN115386297 A CN 115386297A CN 202210884062 A CN202210884062 A CN 202210884062A CN 115386297 A CN115386297 A CN 115386297A
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- 238000005498 polishing Methods 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 35
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 11
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 239000003607 modifier Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- YOCIJWAHRAJQFT-UHFFFAOYSA-N 2-bromo-2-methylpropanoyl bromide Chemical compound CC(C)(Br)C(Br)=O YOCIJWAHRAJQFT-UHFFFAOYSA-N 0.000 claims description 6
- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims description 6
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 6
- 239000006061 abrasive grain Substances 0.000 claims description 6
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 6
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 6
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 claims description 6
- 229940045803 cuprous chloride Drugs 0.000 claims description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- 238000001035 drying Methods 0.000 description 9
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 230000032798 delamination Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 238000002390 rotary evaporation Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000000502 dialysis Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention relates to a polishing solution for wafer polishing and a preparation method thereof, wherein the polishing solution comprises polishing powder, deionized water, an oxidant, a dispersant and a pH regulator, and the preparation method comprises the following steps: adding an oxidant into deionized water according to the weight percentage, then adding polishing powder and a dispersing agent, adding the deionized water to the required volume, adjusting the pH value to 4-6 by using a pH regulator, and magnetically stirring for 10min to obtain the polishing solution. The prepared polishing powder is not easy to agglomerate, the processed surface is not easy to scratch, the total contact area of the polishing powder and the wafer is high, and the polishing efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of polishing, and particularly relates to a polishing solution for wafer polishing and a preparation method thereof.
Background
Silicon carbide (SiC), the most representative third generation wide bandgap semiconductor material, has the characteristics of wide bandgap, high critical breakdown electric field, high thermal conductivity, high carrier saturation mobility, low relative dielectric constant, and high temperature resistance, and is considered as an ideal material for high temperature and high frequency optoelectronic devices. Since the quality of the SiC wafer surface has a critical effect on the performance of its devices, there are stringent requirements on its processing surface quality in applications. Currently, chemical mechanical polishing is one of the most effective processing methods for obtaining ultra-smooth damage-free SiC wafer surfaces.
The polishing solution is the core of the chemical mechanical polishing technology and plays a decisive role in the chemical action and the mechanical action in the chemical mechanical polishing process. Generally, the polishing solution comprises polishing powder, deionized water, an oxidizing agent and a dispersing agent. When the polishing solution is prepared, the suspension property plays a decisive role in the quality of the polishing solution, and if the suspension property is poor, the polished particles are easy to agglomerate. The agglomerated polishing powder is equivalent to increase the particle size of the polishing particles, which in turn causes scratches on the processed surface, and the agglomeration of the polishing particles causes a decrease in the total contact area between the polishing particles and the glass surface, which reduces the polishing efficiency.
Disclosure of Invention
In order to solve the technical problems mentioned in the background art, the invention provides a polishing solution for wafer polishing and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a polishing solution for wafer polishing comprises polishing powder, deionized water, an oxidizing agent, a dispersing agent and a pH regulator;
the polishing powder is prepared by the following steps:
adding abrasive particles into toluene, performing ultrasonic dispersion for 10-20min, adding a modifier and tetrahydrofuran, stirring and dispersing for 1h at the temperature of 20 ℃, adding trifluoroacetic acid, continuously stirring for 20-24h, performing centrifugal separation, performing centrifugal washing by using toluene, and finally drying at the temperature of 120 ℃ under vacuum to obtain the polishing powder. The modifier is subjected to sol-gel reaction on the surface of the abrasive particle under the catalysis of trifluoroacetic acid, the modifier is grafted on the surface of the polymer, namely a layer of polymer is covered on the surface of the abrasive particle, and the dispersibility of the prepared polishing powder is improved by modifying the surface of the abrasive particle.
Further, the abrasive particles are Al 2 O 3 、CeO 2 Wherein the abrasive grains have a grain size in the range of 30-500nm.
Further, the amount ratio of the abrasive particles, the modifier and trifluoroacetic acid is 1g:0.5g:50mg.
Further, the oxidizing agent is hydrogen peroxide.
Further, the pH regulator is nitric acid.
Further, the modifier is prepared by the following steps:
step one, mixing a branched monomer and dichloromethane at the temperature of 0 ℃, then adding triethylamine and 4-dimethylaminopyridine, then dropwise adding 2-bromoisobutyryl bromide, controlling the dropwise adding speed in the dropwise adding process, keeping the temperature not to exceed 5 ℃, keeping the temperature unchanged after the dropwise adding is finished, stirring for 2 hours, then heating to 20 ℃, continuously stirring for reaction for 16 hours, filtering after the reaction is finished, removing the solvent from the obtained filtrate by rotary evaporation, and drying in vacuum to obtain a modified monomer; hydroxyl in the branched monomer reacts with 2-bromoisobutyryl bromide to obtain a modified monomer, and the modified monomer and methyl (3-isopropoxy silicon) propyl acrylate undergo a free radical polymerization reaction under the combined catalysis of pyridine, cuprous bromide and cuprous chloride to obtain the modifier.
And secondly, under the condition of nitrogen protection, adding a modified monomer and methyl (3-isopropoxy silicon-based) propyl acrylate into anisole, adding pyridine, stirring and dispersing, then adding cuprous bromide and cuprous chloride, stirring and dispersing, heating to 80 ℃, stirring and reacting for 5 hours, decompressing and concentrating after the reaction is finished to remove the solvent, precipitating with acetonitrile, and drying in vacuum to obtain the modifier. The modifier has certain amphipathy, after the abrasive particles are treated, the modifier is subjected to organic-inorganic hybrid treatment, has the performances of amphipathy and abrasive particle fixation, has a branched structure in the modifier, utilizes the characteristics of good solubility, low viscosity, molecular chains which are not easy to tangle and the like of the hyperbranched polymer, is matched with the organic nonionic dispersant, has good dispersion stability in polishing solution, has good antioxidant stability and has better suspension property.
Further, in the first step, the dosage ratio of the branched monomer, triethylamine, 4-dimethylamino pyridine and 2-bromoisobutyryl bromide is 1g:0.5mL:50mg:0.5g.
Further, in the second step, the dosage ratio of the modified monomer, methyl (3-isopropoxysilyl) propyl acrylate, pyridine, cuprous bromide and cuprous chloride is 1g:0.5g:50mg:10mg:20mg.
Further, the branched monomer is prepared by the following steps:
under the protection of nitrogen, mixing 0.5g of ethylenediamine and 6mL of ethanol, mixing 3g of polypropylene glycol diglycidyl ether (Mn = 500) and 3g of polyethylene glycol diglycidyl ether (Mn = 640) in ethanol, then dropwise adding the mixture into the ethylenediamine, stirring and reacting for 24 hours at the temperature of 25 ℃, after the reaction is finished, distilling under reduced pressure to remove the ethanol, adding n-hexane, stirring and dispersing, and standing to remove the supernatant liquid to obtain the hyperbranched polyetheramine;
mixing hyperbranched polyetheramine, epoxy cage-like silsesquioxane and ethanol, stirring and dispersing, heating and refluxing for reaction for 24 hours under the protection of nitrogen, dialyzing for 72 hours (the molecular weight cut-off is 9 kD) in THF after the reaction is finished, removing redundant solvent by rotary evaporation after the dialysis is finished, and drying in vacuum to obtain the branched monomer. The polyether amine has good hydrophilicity, the cage-shaped silsesquioxane has good chemical inertness, low surface energy and good stability, and the cage-shaped silsesquioxane and the polyether amine are used as raw materials to prepare the branching monomer by introducing the epoxy cage-shaped silsesquioxane.
Further, the mass ratio of the hyperbranched polyetheramine to the epoxy cage-like silsesquioxane is 9:1.
further, the dispersing agent belongs to an organic nonionic dispersing agent, and specifically is alkylphenol polyethenoxy ether. The nonionic dispersant is not easy to be adsorbed on the surface of an object to be polished and is easy to clean; the stability is good without being influenced by pH value; has good wetting, diffusing, solubilizing and antistatic capabilities.
A preparation method of polishing solution for wafer polishing comprises the following steps:
adding an oxidant into deionized water according to the weight percentage, then adding polishing powder and a dispersing agent, adding deionized water to the required volume, adjusting the pH value to 4-6 by using a pH regulator, and magnetically stirring for 10min to obtain the polishing solution.
Furthermore, the weight percentage of the oxidant is 10-30%, the weight percentage of the polishing powder is 5-10%, the weight percentage of the dispersant is 5-10%, and the balance is deionized water.
The invention has the beneficial effects that:
in order to solve the problem of poor suspension property of the polishing solution, the polishing powder is prepared, abrasive particles are treated, a self-made modifier generates a sol-gel reaction on the surfaces of the abrasive particles under the catalysis of trifluoroacetic acid to obtain the polishing powder, and the stability of the polishing solution is improved after modification.
The modifier has certain amphipathy, has the performances of amphipathy and solid abrasive particles after being treated by organic-inorganic hybridization, and has good dispersion stability in a polishing solution by matching with an organic nonionic dispersant. The polishing powder prepared by the invention is not easy to agglomerate, and the processed surface is not easy to scratch; the dispersibility of the polishing powder is good, the total contact area of the polishing powder and the wafer is increased, and the polishing efficiency is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a branched monomer:
under the protection of nitrogen, mixing 0.5g of ethylenediamine and 6mL of ethanol, mixing 3g of polypropylene glycol diglycidyl ether (Mn = 500) and 3g of polyethylene glycol diglycidyl ether (Mn = 640) in ethanol, then dropwise adding the mixture into the ethylenediamine, stirring and reacting for 24 hours at the temperature of 25 ℃, after the reaction is finished, distilling under reduced pressure to remove the ethanol, adding n-hexane, stirring and dispersing, and standing to remove the supernatant liquid to obtain the hyperbranched polyetheramine;
mixing 9g of hyperbranched polyetheramine, 1g of epoxy cage-like silsesquioxane and 50mL of ethanol, stirring and dispersing, heating and refluxing for reaction for 24h under the protection of nitrogen, dialyzing for 72h (the molecular weight cutoff is 9 kD) in tetrahydrofuran after the reaction is finished, removing redundant solvent by rotary evaporation after the dialysis is finished, and drying in vacuum to obtain the branched monomer.
Example 2
Preparing a modifier:
step one, mixing the branched monomer prepared in the example 1 with dichloromethane at the temperature of 0 ℃, then adding triethylamine and 4-dimethylamino pyridine, then dropwise adding 2-bromoisobutyryl bromide, controlling the dropwise adding speed in the dropwise adding process, keeping the temperature not more than 5 ℃, keeping the temperature unchanged after the dropwise adding is finished, stirring for 2 hours, then heating to 20 ℃, continuously stirring for reaction for 16 hours, filtering after the reaction is finished, removing the solvent from the obtained filtrate by rotary evaporation, and drying in vacuum to obtain a modified monomer; wherein the dosage ratio of the branched monomer, triethylamine, 4-dimethylamino pyridine and 2-bromoisobutyryl bromide is 1g:0.5mL:50mg:0.5g.
And secondly, under the condition of nitrogen protection, adding a modified monomer and methyl (3-isopropoxy silicon-based) propyl acrylate into anisole, adding pyridine, stirring and dispersing, then adding cuprous bromide and cuprous chloride, stirring and dispersing, heating to 80 ℃, stirring and reacting for 5 hours, decompressing and concentrating after the reaction is finished to remove the solvent, precipitating with acetonitrile, and drying in vacuum to obtain the modifier. Wherein the dosage ratio of the modified monomer, methyl (3-isopropoxy silicon) propyl acrylate, pyridine, cuprous bromide and cuprous chloride is 1g:0.5g:50mg:10mg:20mg.
Example 3
The polishing powder is prepared by the following steps:
adding abrasive particles into toluene, performing ultrasonic dispersion for 10min, then adding the modifier prepared in example 2 and tetrahydrofuran, stirring and dispersing for 1h at the temperature of 20 ℃, then adding trifluoroacetic acid, continuing stirring for 20h, performing centrifugal separation, performing centrifugal washing by using toluene, and finally drying at the temperature of 120 ℃ under vacuum to obtain the polishing powder. Wherein the abrasive grains are Al 2 O 3 The grain size of the abrasive grains is 30-500nm. The using ratio of the abrasive particles to the modifier to the trifluoroacetic acid is 1g:0.5g:50mg.
Example 4
The polishing powder is prepared by the following steps:
and (3) adding the abrasive particles into toluene, performing ultrasonic dispersion for 20min, then adding the modifier prepared in the example 2 and tetrahydrofuran, stirring and dispersing for 1h at the temperature of 20 ℃, then adding trifluoroacetic acid, continuing stirring for 24h, performing centrifugal separation, performing centrifugal washing by using toluene, and finally drying at the temperature of 120 ℃ under a vacuum condition to obtain the polishing powder. Wherein the abrasive particles are CeO 2 The grain size of the abrasive grains is 30-500nm. The using ratio of the abrasive particles to the modifier to the trifluoroacetic acid is 1g:0.5g:50mg.
Example 5
A preparation method of polishing solution for wafer polishing comprises the following steps:
adding hydrogen peroxide into deionized water according to the weight percentage, then adding the polishing powder and alkylphenol polyethenoxy ether prepared in the embodiment 3, adding deionized water to the required volume, adjusting the pH value to 6 by nitric acid, and magnetically stirring for 10min to obtain the polishing solution. Wherein, the weight percentage of the hydrogen peroxide is 10 percent, the weight percentage of the polishing powder is 5 percent, the weight percentage of the alkylphenol polyethenoxy ether is 5 percent, and the rest is deionized water.
Example 6
A preparation method of polishing solution for wafer polishing comprises the following steps:
adding hydrogen peroxide into deionized water according to the weight percentage, then adding the polishing powder and alkylphenol polyethenoxy ether prepared in the embodiment 4, adding deionized water to the required volume, adjusting the pH value to 4 by nitric acid, and magnetically stirring for 10min to obtain the polishing solution. Wherein, the weight percentage of the hydrogen peroxide is 15 percent, the weight percentage of the polishing powder is 10 percent, the weight percentage of the alkylphenol polyethenoxy ether is 10 percent, and the rest is deionized water.
Example 7
A preparation method of polishing solution for wafer polishing comprises the following steps:
adding hydrogen peroxide into deionized water according to the weight percentage, then adding the polishing powder and alkylphenol polyoxyethylene ether prepared in the embodiment 4, adding deionized water to the required volume, adjusting the pH value to 4 by nitric acid, and magnetically stirring for 10min to obtain the polishing solution. Wherein, the weight percentage of the hydrogen peroxide is 30 percent, the weight percentage of the polishing powder is 10 percent, the weight percentage of the alkylphenol polyethenoxy ether is 10 percent, and the rest is deionized water.
Comparative example 1
The polishing powder of example 5 was replaced with Al 2 O 3 The particle size range is 30-500nm, and the rest raw materials and the preparation process are kept unchanged.
Comparative example 2
The polishing powder of example 7 was replaced with CeO 2 The particle size range is 30-500nm, and the rest raw materials and the preparation process are kept unchanged.
The samples prepared in example 5 to example 7 and comparative example 1 to comparative example 2 were subjected to the test; the pressure during polishing was 300g/cm 2 The rotation speed of the polishing disk is 70r/min, the flow rate of polishing solution is 4mL/min, the temperature is 25-30 ℃, and the time is 60min.
Surface roughness Ra test: under the same conditions, the measurement was performed by using a coarseness gauge.
Polishing rate test: the polishing rate can be calculated by the change in the quality of the silicon carbide wafer before and after polishing, i.e., polishing rate = removal amount before and after polishing/polishing time.
The test results are shown in table 1 below:
TABLE 1
| Example 5 | Example 6 | Example 7 | Comparative example 1 | Comparative example 2 | |
| Roughness/nm | 0.05 | 0.04 | 0.04 | 3 | 2 |
| Removal Rate/(nm/min) | 280 | 300 | 300 | 220 | 200 |
| Standing for 72h | Without delamination | Without delamination | Without delamination | Delamination of layers | Delamination of layers |
The polishing solution is prepared by processing the polishing powder, and the prepared polishing solution has good storage stability and high polishing efficiency according to test data.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only, and it will be appreciated by those skilled in the art that various modifications, additions and substitutions can be made to the embodiments described without departing from the scope of the invention as defined in the appended claims.
Claims (9)
1. The polishing solution for wafer polishing is characterized by comprising polishing powder, deionized water, an oxidizing agent, a dispersing agent and a pH regulator;
the polishing powder is prepared by the following steps:
step one, mixing a branched monomer and dichloromethane at the temperature of 0 ℃, then adding triethylamine and 4-dimethylaminopyridine, then dropwise adding 2-bromoisobutyryl bromide, controlling the dropwise adding speed in the dropwise adding process, keeping the temperature not to exceed 5 ℃, keeping the temperature unchanged after the dropwise adding is finished, stirring for 2 hours, then heating to 20 ℃, and continuing stirring for reacting for 16 hours to obtain a modified monomer;
step two, under the condition of nitrogen protection, adding a modified monomer and methyl (3-isopropoxy silicon-based) propyl acrylate into anisole, adding pyridine, stirring and dispersing, then adding cuprous bromide and cuprous chloride, stirring and dispersing, heating to 80 ℃, stirring and reacting for 5 hours to obtain a modifier;
and step three, adding abrasive particles into toluene, performing ultrasonic dispersion for 10-20min, then adding a modifier and tetrahydrofuran, stirring and dispersing for 1h at the temperature of 20 ℃, then adding trifluoroacetic acid, and continuing stirring for 20-24h to obtain the polishing powder.
2. The polishing solution as set forth in claim 1, wherein the branched monomer is prepared by the steps of:
mixing hyperbranched polyetheramine, epoxy cage-like silsesquioxane and ethanol, stirring and dispersing, and heating and refluxing for reaction for 24 hours under the condition of nitrogen protection to obtain a branched monomer.
3. The polishing solution for polishing a wafer according to claim 1, wherein said abrasive grains are Al 2 O 3 、CeO 2 Wherein the abrasive grains have a grain size in the range of 30-500nm.
4. The polishing solution as set forth in claim 1 wherein the oxidizing agent is hydrogen peroxide.
5. The polishing solution as set forth in claim 1, wherein the pH adjusting agent is nitric acid.
6. The polishing solution for polishing a wafer according to claim 1, wherein the dispersant is an organic nonionic dispersant.
7. The polishing solution for wafer polishing according to claim 2, wherein the mass ratio of the hyperbranched polyetheramine to the epoxy cage-like silsesquioxane is 9:1.
8. the method of claim 1, comprising the steps of:
adding an oxidant into deionized water according to the weight percentage, then adding polishing powder and a dispersing agent, adding deionized water to the required volume, adjusting the pH value to 4-6 by using a pH regulator, and magnetically stirring for 10min to obtain the polishing solution.
9. The method of claim 8, wherein the oxidizer is 10-30 wt%, the polishing powder is 5-10 wt%, the dispersant is 5-10 wt%, and the balance is deionized water.
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