CN114317132B - Lithium tantalate cleaning agent containing nano colloid particles, preparation method and application - Google Patents
Lithium tantalate cleaning agent containing nano colloid particles, preparation method and application Download PDFInfo
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- CN114317132B CN114317132B CN202111664983.5A CN202111664983A CN114317132B CN 114317132 B CN114317132 B CN 114317132B CN 202111664983 A CN202111664983 A CN 202111664983A CN 114317132 B CN114317132 B CN 114317132B
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- 239000002245 particle Substances 0.000 title claims abstract description 154
- 239000000084 colloidal system Substances 0.000 title claims abstract description 105
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 55
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 55
- 238000004140 cleaning Methods 0.000 claims abstract description 141
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 129
- 239000000463 material Substances 0.000 claims abstract description 58
- 239000003381 stabilizer Substances 0.000 claims abstract description 55
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 53
- 125000002091 cationic group Chemical group 0.000 claims abstract description 43
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 39
- 239000012498 ultrapure water Substances 0.000 claims abstract description 39
- 239000003463 adsorbent Substances 0.000 claims abstract description 36
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 32
- 239000004094 surface-active agent Substances 0.000 claims abstract description 17
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 15
- 239000000080 wetting agent Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 65
- 238000003756 stirring Methods 0.000 claims description 49
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 229920002125 Sokalan® Polymers 0.000 claims description 14
- 239000004584 polyacrylic acid Substances 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 229920001577 copolymer Polymers 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920001444 polymaleic acid Polymers 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 21
- 235000012431 wafers Nutrition 0.000 description 68
- -1 cationic alkyl glycosides Chemical class 0.000 description 22
- 230000008569 process Effects 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 238000001514 detection method Methods 0.000 description 12
- 238000005498 polishing Methods 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 7
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000002131 composite material Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 229910052733 gallium Inorganic materials 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- 229910052746 lanthanum Inorganic materials 0.000 description 7
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 150000001768 cations Chemical class 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000000693 micelle Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 5
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- 230000003749 cleanliness Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
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- 229920001223 polyethylene glycol Polymers 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- MRUAUOIMASANKQ-UHFFFAOYSA-O carboxymethyl-[3-(dodecanoylamino)propyl]-dimethylazanium Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC(O)=O MRUAUOIMASANKQ-UHFFFAOYSA-O 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 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 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 229940075468 lauramidopropyl betaine Drugs 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- IHJUECRFYCQBMW-UHFFFAOYSA-N 2,5-dimethylhex-3-yne-2,5-diol Chemical compound CC(C)(O)C#CC(C)(C)O IHJUECRFYCQBMW-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
- 229910008051 Si-OH Inorganic materials 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 125000001204 arachidyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
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- 239000002738 chelating agent Substances 0.000 description 2
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- 150000002367 halogens Chemical group 0.000 description 2
- OIOJYJPDWYGJQB-UHFFFAOYSA-N hex-1-yne-1,3-diol Chemical compound CCCC(O)C#CO OIOJYJPDWYGJQB-UHFFFAOYSA-N 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012434 nucleophilic reagent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 description 2
- 235000011181 potassium carbonates Nutrition 0.000 description 2
- 235000011118 potassium hydroxide Nutrition 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000005956 quaternization reaction Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000010897 surface acoustic wave method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LXOFYPKXCSULTL-UHFFFAOYSA-N 2,4,7,9-tetramethyldec-5-yne-4,7-diol Chemical compound CC(C)CC(C)(O)C#CC(C)(O)CC(C)C LXOFYPKXCSULTL-UHFFFAOYSA-N 0.000 description 1
- XPFCZYUVICHKDS-UHFFFAOYSA-N 3-methylbutane-1,3-diol Chemical compound CC(C)(O)CCO XPFCZYUVICHKDS-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 241001089723 Metaphycus omega Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006664 bond formation reaction Methods 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 229940031728 cocamidopropylamine oxide Drugs 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 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
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- 150000008131 glucosides Chemical group 0.000 description 1
- 238000005858 glycosidation reaction Methods 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 125000002960 margaryl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([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])C([H])([H])[H] 0.000 description 1
- 125000003136 n-heptyl 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])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 125000001196 nonadecyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([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])[H] 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002958 pentadecyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 239000011736 potassium bicarbonate Substances 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
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Landscapes
- Cleaning Or Drying Semiconductors (AREA)
- Detergent Compositions (AREA)
Abstract
The invention provides a cleaning agent for cleaning the surface of a lithium tantalate wafer, and a preparation method and application thereof, wherein the cleaning agent comprises nano colloid particles, and also relates to the preparation method, the preparation method and the application of the nano colloid particles, wherein the nano colloid particles comprise nano silicon dioxide, a cationic colloid stabilizer and a silicon dioxide adsorbent, and the cleaning agent comprises the nano colloid particles, a pH regulator, a surfactant, a wetting agent and ultrapure water. The nano colloid particles have excellent stability, particle cleaning and particle redeposition resisting effects, can stop the occurrence of broken pieces, are particularly suitable for cleaning the surface of a soft and brittle material, especially a lithium tantalate wafer, and have wide application prospect and industrial use value.
Description
Technical Field
The invention relates to a cleaning agent for cleaning the surface of a soft and brittle material, a preparation method and application thereof, in particular to a lithium tantalate cleaning agent containing nano colloid particles, a preparation method and application thereof, the nano colloid particles and a preparation method thereof, and a cleaning method for cleaning the surface of the soft and brittle material by using the cleaning agent, belonging to the field of novel cleaning agents and the technical field of soft and brittle material surface treatment.
Background
Lithium tantalate (LiTaO) 3 Hereinafter, also referred to as "LT") crystal is a typical single crystal "soft and brittle" material having a mohs hardness of 5.5 to 6, and having excellent piezoelectric, pyroelectric, acousto-optic, electro-optic and other effects, and thus becomes a surface acoustic wave (SAW: surface acoustic wave) the device, the optical communication, the laser and the photoelectronic fields, and the device can be widely applied to filters, sensors, high-speed communication devices, frequency doubling devices and the like on civil photoelectric products in national defense industries such as aviation, aerospace and the like. SAW under 5G standard cannot be used by other more advantageous products especially in the field of high frequency elastic wave devicesThe crystal with the highest optical performance and the best comprehensive index is found so far, and is one of the main alternative materials of optical silicon which is currently accepted as an optoelectronic age.
With the progress of technology and the improvement of technical requirements, in recent years, the market demand for LT has increased significantly, and has progressed in demand toward the requirements of large size, high thinness, no damage, ultra-high-cleanliness surfaces, and the like.
The current LT wafer production process is a "cut-grind-polish" process where the cut is made by grinding, the free abrasive is used to grind, and the polish is made by acid etching. However, LT crystals have various problems in cutting, grinding, polishing, etc. due to their physical properties such as strong anisotropy and soft and brittle properties, for example: 1. as a typical soft and brittle material, LT crystals are prone to defects such as cracks, edge chipping, subsurface damage, and the like during grinding and polishing; 2. because of low hardness, the LT crystal is easy to scratch the processing surface by impurity particles such as abrasive materials and damage such as abrasive particle embedding, and is difficult to eliminate in the subsequent cleaning process; 3. the LT material has a pyroelectric effect, and the temperature of the working environment is increased to cause the discharge phenomenon of the wafer to cause fragmentation; 4. process stability and continued processing efficiency during continued processing of LT wafers remain to be improved.
The existence of these problems places stringent and diverse specifications on the cleaning process after LT grinding and/or polishing: 1. physical cleaning parameters (ultrasonic frequency, solution fluctuation, rinsing strength, etc.) of the cleaning process need to be controlled gently to reduce LT fragmentation; 2. particles embedded in the surface of a wafer in the grinding process of LT are required to have good cleaning and removing effects; 3. the cleaning temperature is controlled within 40 ℃ to avoid chip cracking caused by the pyroelectric phenomenon of the chip.
However, the cleaning method for lithium tantalate wafers has been mainly limited to the prior art cleaning method, i.e., soaking, ultrasonic treatment, etc. are generally adopted, but there are problems that particles embedded in the grinding and/or polishing process cannot be cleaned, and the breakage rate of LT in cleaning still needs to be further reduced, etc. There are few cleaning methods that are more efficient and meet the above-mentioned needs. The only slight modifications or similar methods are as follows:
CN103603054a discloses a method for preparing lithium tantalate wafer, wherein the cleaning method of the lithium carbonate wafer is specifically as follows: ultrasonically cleaning the lithium tantalate substrate with an aqueous acetone solution at a first cleaning temperature for a second time; ultrasonically cleaning the lithium tantalate substrate with an absolute ethyl alcohol aqueous solution at a second cleaning temperature for a third time, wherein the first and second cleaning temperatures are 80 ℃, the second time is 20-30 minutes, the third time is 20-30 minutes, then washing the lithium tantalate wafer with deionized water for 30 seconds to 1 minute, and drying the washed lithium tantalate wafer at 50-60 ℃ for 1-2 minutes.
CN109988509a discloses a lithium tantalate reducing sheet polishing solution, a preparation method and application thereof, wherein the reducing sheet polishing solution comprises the following components in percentage by weight: 35-65% of liquid phase carrier, 15-60% of silicon dioxide particles, less than or equal to 20% of oxidant and 0.005-20% of nucleophilic reagent. The lithium tantalate reducing sheet polishing solution overcomes the defects in the prior art, and the preparation method is simple and efficient. In addition, the polishing liquid is reasonably combined by a specific nucleophilic reagent and an oxidizing reagent, so that the polishing quality and the polishing rate of the polishing liquid are greatly improved.
CN103878145a discloses a method for cleaning a gallium lanthanum silicate wafer similar to a lithium tantalate wafer, comprising the steps of: megasonic cleaning is carried out on the gallium lanthanum silicate wafer by using a cleaning liquid consisting of phosphoric acid, hydrogen peroxide and deionized water; rinsing and spin-drying the cleaned gallium lanthanum silicate wafer; then cleaning the gallium lanthanum silicate wafer by megasonic cleaning liquid consisting of ammonia water, hydrogen peroxide and deionized water; rinsing and spin-drying the cleaned gallium lanthanum silicate wafer; and (5) putting the wafer subjected to rinsing and spin-drying into a baking oven for baking. The cleaning method can compress the time of an acid cleaning process and prolong the time of an alkaline cleaning process, and simultaneously replaces the traditional ultrasonic cleaning with more effective megasonic cleaning, so that the cleaning problem of the gallium lanthanum silicate wafer after the cutting treatment is solved, the cleanliness of the surface of the gallium lanthanum silicate wafer is improved, and a better cleaning effect is achieved.
As described above, there are few reports on a novel cleaning method for lithium tantalate wafers, and therefore, development of a novel cleaning agent and a novel cleaning method for soft and brittle materials, particularly lithium tantalate wafers, is a technical difficulty in the field at present. The invention aims at providing a novel lithium tantalate wafer cleaning agent capable of meeting the technical requirements and trends, and the key and technical innovation points of the novel lithium tantalate wafer cleaning agent are mainly characterized by a novel nano colloid particle, so that a plurality of excellent technical effects are achieved through the use of the nano colloid particle, breakthrough progress is made in the field, and the novel lithium tantalate wafer cleaning agent has great promotion and improvement effects on the surface cleaning of soft and brittle materials, particularly lithium tantalate wafers.
Disclosure of Invention
The present inventors have made extensive and intensive studies to solve the problems and to satisfy the requirements and trends of the prior art LT wafer cleaning techniques as described above, and to develop a novel environment-friendly cleaning solution, a preparation method and a cleaning process, thereby developing and obtaining a nano colloidal particle suitable for cleaning a surface of a soft and brittle material, particularly an LT wafer, a preparation method and use thereof, and various technical schemes such as a cleaning agent containing the nano colloidal particle and a cleaning method of an LT wafer, and thus completing the present invention.
It should be noted that, in the present invention, unless otherwise specified, reference to the specific meaning of "comprising" as defined and described by the composition includes both the open meaning of "comprising", "including" and the like, and the closed meaning of "consisting of …", "consisting of …" and the like.
Specifically, the invention specifically comprises the following technical schemes.
[ first technical means ]
In a first aspect, an aspect of the present invention is to provide a nano-colloidal particle which is particularly suitable for surface cleaning of fragile materials, especially LT wafers.
In the nano-colloidal particles of the present invention, the nano-colloidal particles include nano-silica, a silica adsorbent (hereinafter, sometimes referred to as "adsorbent"), and a cationic colloidal stabilizer.
In the nano-colloidal particles of the present invention, the particle size of the nano-silica may be, for example, 1 to 100nm, for example, any two values of 1nm, 5nm, 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, and may be, for example, 5 to 90nm, 10 to 80nm, 20 to 70nm, 30 to 60nm, etc., preferably 20 to 60nm.
In the nano-colloidal particles of the present invention, the cationic colloidal stabilizer is a cationic ammonium oligomer of the following formula (1):
wherein:
r is H or C 6-20 An alkyl group;
n is a degree of polymerization selected from integers from 5 to 50;
x is halogen.
Among the cationic colloidal stabilizers of formula (1) above, cationic alkyl glycosides, which are a class of oligomers already known, are commercially available in a variety of forms, which may be a single component of various cationic alkyl glycosides having different alkyl groups R or a mixture of any of a variety of types.
The synthesis methods of the cationic alkyl glycoside can be generally three methods: 1. one-step method, synthesizing epichlorohydrin and a glucoside unit in one step; 2. glycosidation and quaternization are carried out; 3. etherification followed by quaternization is described in various prior art such as "Sexiqiang et al, synthesis and use of cationic alkyl glycosides, progress in fine petrochemical engineering, volume 12, 11 th, 2011", etc., and will not be described in detail herein.
In the cationic colloidal stabilizer of the above formula (1), "2nX - "means 2N halide anions corresponding to 2N cations contained in N repeating units.
In the cationic colloidal stabilizer of the above formula (1), R may be C 6-20 Alkyl groups, e.g. can beN-hexyl, n-heptyl, n-octyl, n-nonyl, n-decyl, n-undecyl, n-dodecyl, n-tridecyl, n-tetradecyl, n-pentadecyl, n-hexadecyl, n-heptadecyl, n-octadecyl, n-nonadecyl or n-eicosyl, as well as branched alkyl groups which may be any of the above, i.e., branched hexyl, branched heptyl, branched octyl, branched nonyl, branched decyl, branched undecyl, branched dodecyl, branched tridecyl, branched tetradecyl, branched pentadecyl, branched hexadecyl, branched heptadecyl, branched octadecyl, branched nonadecyl or branched eicosyl.
In the cationic colloidal stabilizer of the above formula (1), X is halogen, and may be F, cl, br or I, for example.
In the nano-colloidal particles of the present invention, the silica adsorbent is any one or a mixture of any more of polyacrylic acid, polymaleic acid, acrylic acid-maleic acid copolymer or acrylic acid-styrene copolymer.
The molecular weight of the silica adsorbent is not particularly limited, and may be, for example, 2000 to 20000 (i.e., selected from the group consisting of 2000, 3000, 4000, 5000, 6000, 7000, 8000, 9000, 10000, 11000, 12000, 13000, 14000, 15000, 16000, 17000, 18000, 19000, 20000, and the like, and may be, for example, 2000 to 20000, 5000 to 15000, 8000 to 12000, and the like, and further may be, for example, 2000 to 3000, 5000 to 15000, 8000 to 12000, and the like, and it is a common technical means for polymerization in the polymer field, and it is not described in detail herein.
As an illustrative example, the structure of the nano-colloid particle is shown in the following formula (2):
in the nano colloidal particles of the formula (2), the colloidal stabilizer is a cationic colloidal stabilizer of the formula (1), the silica adsorbent is polyacrylic acid, dashes at two ends of the cationic colloidal stabilizer refer to connection positions of repeating units in the colloidal stabilizer, and n has the same definition as the above.
In the nano-colloidal particles of formula (2), it is noted that the dotted line represents an ionic bond, i.e. the hydroxyl oxyanion of the polyacrylic acid is ionically bonded to the N cation of the cationic colloidal stabilizer compound of formula (1), since the hydroxyl group is preferably bonded to the strong cation N + And (3) combining. It should also be noted that other oxyhydrogen anions and strong cations N are not shown for simplicity only + The long-dashed lines combined, but in practice in the nano-colloidal particles, most or even all of the oxyhydrogen anions are associated with strong cations N + Binding is by ionic bond formation.
The nano colloid particles have good colloid stability, have excellent cleaning effect when being used for cleaning the surface of a soft and brittle material such as a lithium tantalate wafer, can be used in the technical field of cleaning the surface of the soft and brittle material, and have good application prospect.
[ second technical means ]
In a second aspect, an aspect of the present invention is to provide a use of the above-mentioned nano-colloidal particles for cleaning the surface of a brittle material.
The nano colloid particles can be applied to surface cleaning of lithium tantalate wafers on the surfaces of soft and brittle materials due to the unique structure and cleaning mechanism.
Third technical means ]
In a third aspect, the present invention provides a method for preparing the above-mentioned nano-colloidal particles.
The preparation method comprises the following steps:
A. weighing 5-15 parts of nano silicon dioxide, 0.01-1 part of cationic colloid stabilizer, 0.5-4 parts of silicon dioxide adsorbent and 75-95 parts of ultrapure water according to parts by mass, and dividing the ultrapure water into two equal parts for later use;
B. adding the nano silicon dioxide into the first part of ultrapure water under stirring, adding the silicon dioxide adsorbent under stirring, and continuing stirring for 30-60 minutes to serve as an agent I for standby;
C. adding the cationic colloid stabilizer into the second part of ultrapure water under stirring, and keeping stirring until the colloid stabilizer is fully swelled to serve as a II agent for standby;
D. slowly adding the agent II while stirring the agent I at 25 ℃, continuously stirring until the agent is sufficiently uniform, and standing for 5-10 hours to obtain the nano colloid particles.
In the preparation method of the nano colloidal particles, the nano silica, the colloid stabilizer and the silica adsorbent in the step A are the corresponding nano silica, colloid stabilizer and silica adsorbent in the first technical scheme.
For example, in the method for preparing the nano colloidal particles, the particle size of the nano silica is 1 to 100nm, for example, may be in the range of any two values of 1nm, 5nm, 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, and may be exemplified by 5 to 90nm, 10 to 80nm, 20 to 70nm, 30 to 60nm, etc., preferably 20 to 60nm.
For another example, the cationic colloidal stabilizer and the silica adsorbent are also described in the first technical scheme, and for brevity, description will not be repeated, and specific description and various limitations can be referred to the first technical scheme, and no further description will be made here.
In the preparation method of the nano colloid particle, in the step A, the nano silicon dioxide is 5-15 parts by mass, for example, 5 parts, 7 parts, 9 parts, 11 parts, 13 parts or 15 parts.
In the preparation method of the nano colloid particle, in the step a, the cationic colloid stabilizer may be 0.01-1 part by mass, for example, 0.01 part, 0.02 part, 0.05 part, 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part or 1 part.
In the preparation method of the nano colloid particle, in the step A, the silica adsorbent is 0.5-4 parts by mass, for example, 0.5 parts, 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts or 4 parts.
In the preparation method of the nano colloid particles, in the step A, the ultrapure water is 75-95 parts by mass, for example, 75 parts, 80 parts, 85 parts, 90 parts or 95 parts.
The ultrapure water is deionized water with the resistance of more than or equal to 18MΩ.
In the production method of the present invention, the stirring speed in the step B is not particularly limited as long as the nanosilica and the silica adsorbent can be sufficiently mixed, and may be, for example, 40 to 150rpm, and further may be, for example, 40rpm, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm, 100rpm, 110rpm, 120rpm, 130rpm, 140rpm or 150rpm.
In the production method of the present invention, the stirring speed in the step C is not particularly restricted so long as the cationic colloidal stabilizer can be sufficiently stirred in ultrapure water to be completely swollen, and may be, for example, 40 to 150rpm, further, for example, 40rpm, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm, 100rpm, 110rpm, 120rpm, 130rpm, 140rpm or 150rpm. The stirring time is determined according to the complete swelling, and the stirring can be stopped or continued for 5-10 minutes as long as the cationic colloidal stabilizer is fully swelled, and the skilled person can make appropriate selections and determinations after reading the preparation method, and detailed description thereof is omitted here.
In the production method of the present invention, the stirring speed in the step D is not particularly limited as long as the agent I and the agent II can be sufficiently stirred uniformly, and may be, for example, 40 to 150rpm, and further may be, for example, 40rpm, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm, 100rpm, 110rpm, 120rpm, 130rpm, 140rpm or 150rpm. The stirring time is not particularly restricted so long as the agent I and the agent II can be sufficiently stirred uniformly, and a person skilled in the art can make appropriate selections and determinations after reading the present preparation method, and detailed description thereof will not be given here.
Fourth technical means ]
In a fourth aspect, the invention provides a cleaning agent for cleaning the surface of a soft and brittle material, and a preparation method of the cleaning agent.
The soft and brittle material, especially lithium tantalate wafer, is generally applied in a plurality of high-tech fields, and has extremely high technical requirements and demands on particle removal degree, surface cleanliness and the like, as described above.
The cleaning agent can be used for the cleaning procedure after grinding or polishing of the soft and brittle materials, so as to remove surface particles, greasy dirt, dust, fingerprints and other pollutants.
The cleaning agent for cleaning the surface of the soft and brittle material comprises the nano colloid particles.
The cleaning agent for cleaning the surface of the soft and brittle material comprises a pH regulator, a surfactant, a wetting agent and ultrapure water in addition to the nano colloid particles.
The cleaning agent for cleaning the surface of the soft and brittle material according to the present invention comprises, as an example, 5 to 10 parts by mass of nano colloid particles, 5 to 15 parts by mass of a pH regulator, 0.1 to 0.5 part by mass of a surfactant, 2 to 12 parts by mass of a wetting agent, and 75 to 95 parts by mass of ultrapure water.
Still further, the nano-colloid particles may be 5 to 10 parts by mass, for example, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts.
Still further, the pH adjuster is 5 to 15 parts by mass, for example, 5 parts, 7 parts, 9 parts, 11 parts, 13 parts, or 15 parts.
Still further, the surfactant is 0.1 to 0.5 parts by mass, and for example, may be 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, or 0.5 parts.
Still further, the wetting agent is 2 to 12 parts by mass, for example, may be 2 parts, 4 parts, 6 parts, 8 parts, 10 parts or 12 parts.
Further, the ultrapure water is 75 to 95 parts by mass, and for example, 75 parts, 80 parts, 85 parts, 90 parts or 95 parts by mass.
Wherein, the pH regulator can be any one or a mixture of any plurality of sodium carbonate, potassium carbonate, sodium bicarbonate, KOH, naOH or potassium bicarbonate.
Wherein the surfactant can be any one of lauramidopropyl betaine, cocamidopropyl amine oxide or acetylenic diol surfactant.
Among them, lauramidopropyl betaine and cocoamidopropyl amine oxide are well known surfactants and commercially available from various sources, and will not be described in detail herein.
Among them, the acetylenic diol type surfactant is also a well-known surfactant, and may be, for example, dimethylhexyne diol (i.e., 2, 5-dimethyl-3-hexyne-2, 5-diol), 1-hexyne-1, 3-diol, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, etc., which are readily commercially available from various sources and will not be described in detail herein.
Wherein the wetting agent is a small molecular polyol or polyether alcohol, for example, the small molecular polyol can be any one or a combination of any of glycerol, neopentyl glycol, diethylene glycol, triethylene glycol, ethylene glycol, isoprene glycol and propylene glycol; for example, the polyether alcohol may be any one or a combination of polyethylene glycol (e.g., polyethylene glycol 400, polyethylene glycol 600, etc.), polyethylene glycol monomethyl ether (e.g., polyethylene glycol monomethyl ether 2000, etc.).
Wherein the ultrapure water is deionized water with the resistance of more than or equal to 18MΩ.
The preparation method of the cleaning agent for cleaning the surface of the soft and brittle material comprises the following steps:
a1: respectively weighing nano colloid particles, a pH regulator, a surfactant, a wetting agent and ultrapure water in parts by mass;
b1: adding each component into a container, and stirring at the stirring speed of 300-1000rpm for 1-2 hours at normal temperature to obtain the cleaning agent.
Wherein, each component in the step A1 is specifically described above, and will not be described in detail herein.
Wherein the stirring speed in step B1 is 300-1000rpm, and may be 300rpm, 400rpm, 500rpm, 600rpm, 700rpm, 800rpm, 900rpm or 1000rpm, for example.
Wherein, the stirring time in the step B1 is 1-2 hours, for example, 1 hour, 1.5 hours or 2 hours.
According to the cleaning agent for cleaning the surface of the soft and brittle material, the cleaning agent has excellent surface cleaning effect and performance due to the inclusion of the unique nano colloid particles, is particularly suitable for cleaning the surface of the soft and brittle material, particularly the surface of a lithium tantalate wafer, has simple cleaning steps and small waste liquid amount, realizes green and environment-friendly cleaning treatment, and has good industrialized application potential and value.
[ fifth technical means ]
In a fifth aspect, the present invention provides a method for cleaning a surface of a brittle material.
According to the surface cleaning method of the soft and brittle material, the cleaning agent is used, and the components, the content and the like of the cleaning agent are as described in the fourth technical scheme, and are not repeatedly cited and described herein.
According to the surface cleaning method of the soft and brittle material, the surface cleaning method comprises the following steps:
s1: adding the cleaning agent into a cleaning tank, and then placing the soft and brittle material to be cleaned into the cleaning tank;
s2: opening ultrasonic waves to carry out ultrasonic cleaning; preferably, the ultrasonic current is 1.5-2.5A when the ultrasonic cleaning is carried out, and the ultrasonic cleaning time is 5-10 minutes;
s3: and taking the soft and brittle material out of the cleaning tank, cleaning the soft and brittle material with ultrapure water for 2-3 times, and finally drying the soft and brittle material in vacuum to finish the cleaning method.
According to the surface cleaning method of the soft and brittle material, the soft and brittle material in the step S1 is as described above, especially a lithium tantalate wafer.
According to the surface cleaning method of the soft and brittle material, the ultrasonic current in the step S2 is preferably 1.5-2.5A, for example, 1.5A, 2A or 2.5A; the ultrasonic cleaning time is preferably 5 to 10 minutes, and may be, for example, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, or 10 minutes. Of course, the ultrasonic current can be increased or decreased appropriately according to the actual situation (such as serious dirt on the surface of the soft and brittle material), and the cleaning time can be prolonged or shortened.
According to the surface cleaning method of the soft and brittle material, the ultrapure water in the step S3 is deionized water with the resistance of more than or equal to 18MΩ.
In the cleaning method of the present invention, since the cleaning agent containing the unique nano-colloid particles is used, an excellent cleaning effect is obtained, and the subsequent cleaning test is specifically seen, which will not be described in detail herein.
As described above, the present invention provides a nano-colloidal particle, a preparation method and use thereof, a cleaning agent containing the nano-colloidal particle, a preparation method of the cleaning agent, a cleaning method for cleaning a surface of a soft and brittle material using the cleaning agent, etc., and these technical schemes have the following principles and advantages:
1. the nano-silica, the silica adsorbent and the cationic colloid stabilizer are creatively used to obtain the nano-colloid particles with unique structures, which are amphiphilic supermolecular systems, can be used in various cleaning environments (such as acidity, neutrality or alkalinity) to maintain excellent stability, can be used in surface cleaning of various soft and brittle materials, and can obtain excellent surface ultra-high-cleanliness cleaning effect.
2. Compared with the traditional organic solvent or surfactant-containing cleaning process, the nano colloid particles can reduce the use amount of the solvent, greatly shorten the cleaning time (how long the prior art is usually 30-60 minutes or even longer), are environment-friendly, have little waste liquid production and greatly reduce the waste liquid treatment cost; and various particle impurities can be effectively removed, and the cleaning efficiency and the yield are greatly improved.
3. The cleaning method has mild cleaning process parameters and simple operation, can effectively reduce the fragmentation rate and reduce the production cost of the LT process.
4. The nano colloid particles do not contain metal ions and traditional chelating agents, and because the molecular structure of the silicon dioxide adsorbent contains a large number of carboxylic acid groups, the silicon dioxide adsorbent has high-efficiency chelation effect on the metal ions, and the complexation of impurity metal ions attached to the surface of the soft and brittle material can be realized without adding additional chelating agents. Moreover, the nano colloid ion has good water solubility and strong chelating ability, and has good cleaning effect on the surface of a soft and brittle material with serious surface metal pollution and the surface of a material with extremely low requirement on the residual metal after cleaning.
5. When the cationic colloidal stabilizer and the silica adsorbent are used, dynamic balance change can be generated under the comprehensive dilution effect of the pH regulator, the surfactant, the wetting agent and the water molecules, the modified nano silica can be exposed from colloid particles and directly contacted with the surface of a cleaning material, so that weak van der Waals friction effect is generated between the modified nano silica and impurities such as particles adsorbed on the surface of a soft and brittle material, the pollutants on the surface of the material are quickly and fully combined with silica molecules, and the effect of eluting the particles from the surface of the material is achieved.
6. Aiming at the defects that the lithium tantalate wafer is easy to adsorb dirt such as particles, dust and the like in the air or solution medium environment where the manufacturing process is located, and the dirt on the surface of the lithium tantalate material is not easy to remove or is sticky back, the cationic colloid stabilizer used in the invention can carry out cationization modification on the surface of the lithium tantalate wafer in the cleaning process to form a layer of molecular-grade antistatic protective film, so that tiny dust or particles in the environment are prevented from being adsorbed on the surface of the wafer again, the surface of the lithium tantalate wafer is kept clean, and the conventional and necessary complex cleaning treatment is not needed again in the application of the subsequent manufacturing process.
7. When the cleaning agent containing the nano colloid particles is used for cleaning, high temperature and long-time ultrasonic operation are not needed, so that the occurrence of broken pieces is avoided, and the cleaning agent has remarkable large-scale and industrialized significance for improving the yield of products and reducing the cost.
Therefore, the nano colloid particles and the cleaning liquid containing the same have excellent cleaning effect in a plurality of technical fields, especially the surface cleaning field of soft and brittle materials, are more environment-friendly, have very small environment-friendly pressure, are more friendly to the operation requirements of operators and the operation environment, and have good large-scale industrial application values.
Drawings
FIG. 1 is a schematic diagram of the principle of formation of the nano-colloid particles according to the present invention.
The specific forming principle is as follows:
the first stage: the silica nanopowder (represented by spheres in fig. 1) is combined with the hydrophobic groups in the silica adsorbent to form a micelle structure in which the nanosilica micropowder is encapsulated: the hydrophilic groups in the adsorbent are outwards, so that the silicon dioxide molecules which are insoluble in water per se are dispersed in water in the form of micelles (see big spheres indicated by the first arrow, the outer layer of which is outwards hydrophilic groups, and the inner layer of which is hydrophobic groups combined with silicon dioxide).
And a second stage: after the cationic colloid stabilizer is added, a large amount of hydrophilic N cations contained in the molecular structure of the colloid stabilizer can be further combined with hydrophilic groups outwards on the surface of the micelle around the micelle, so that a space network structure is formed, aggregation (i.e. aggregation) or damage between the micelle and the micelle caused by molecular motion is avoided, and the stability of the nano colloid particles is ensured.
Fig. 2 is an infrared spectrogram of nano silica powder, a composite obtained after nano silica is compounded with polyacrylic acid, and finally obtained nano colloid particle N1 in nano colloid particle preparation example 1, wherein: a is an infrared spectrogram of nano silicon dioxide powder, b is an infrared spectrogram of a compound obtained after the nano silicon dioxide is compounded with polyacrylic acid, and c is an infrared spectrogram of a finally obtained nano colloid particle N1.
Wherein the complex of nano silica and polyacrylic acid (i.e. B) is the complex obtained in step B (i.e. agent I) in preparation example 1 of nano colloid particles.
FIG. 3 shows TEM micro morphology of the composite (i.e., agent I) obtained in step B of nano-colloidal particle preparation example 1 and the finally obtained nano-colloidal particle N1 after standing for 1 day and 30 days, wherein: 3 (1) is the morphology of the composite or the nano-colloid particle N1 after standing for 1 day (only one is listed because the two are highly similar), 3 (2) is the TEM microstructure of the composite after standing for 30 days, and 3 (3) is the TEM microstructure of the nano-colloid particle N1 after standing for 30 days.
Fig. 4 is a graph of particle residue detection after cleaning a polished lithium tantalate wafer using the prior art and the cleaning method of the present invention, respectively.
Wherein, the left graph is a particle residue detection graph after cleaning using the prior art cleaning method, and the right graph is a particle residue detection graph after cleaning using Q1 using the cleaning method of the present invention.
FIG. 5 is a graph of AOI particle residue detection after polishing lithium tantalate wafers with different cleaners and after standing in an air environment for different times, respectively, using the cleaning method of the present invention to examine the respective anti-particle redeposition properties.
Wherein, upper left and upper left are AOI particle residue detection contrast graphs of placing 1h after cleaning and 24h after cleaning with Q1, respectively, lower left and lower right are AOI particle residue detection contrast graphs of placing 1h after cleaning and 24h after cleaning with DQ1, respectively.
Detailed Description
The present invention will be described in detail by way of specific examples, but the purpose and purpose of these exemplary embodiments are merely to illustrate the present invention, and are not intended to limit the actual scope of the present invention in any way.
In all the following preparation examples, the ultrapure water used was deionized water having a resistance of not less than 18 M.OMEGA.and anions in all the cationic colloidal stabilizers were chloride anions.
Nano-colloid particle preparation example 1: preparation of nano-colloid particles
A. Weighing 10 parts of nano silicon dioxide (with the granularity of 20-60 nm), 0.5 part of a cationic colloid stabilizer compound of formula (1) (wherein R is lauryl, namely dodecyl, n is 20-30), 2.25 parts of silicon dioxide adsorbent polyacrylic acid (with the molecular weight of 8000-14000) and 85 parts of ultrapure water according to parts by mass, and dividing the ultrapure water into two equal parts (namely 42.5 parts by mass) for standby;
B. Adding the nano silicon dioxide into the first part of ultrapure water under stirring, adding the silicon dioxide adsorbent under stirring at 100rpm, and continuing stirring for 45 minutes to obtain an agent I for later use;
C. adding the cationic colloid stabilizer into the second part of ultrapure water under stirring, and keeping stirring at 100rpm until the colloid stabilizer is fully swelled to obtain a reagent II for later use;
D. slowly adding the agent II while stirring the agent I at 100rpm at 25 ℃, continuously stirring until the agent II is sufficiently uniform, and standing for 7.5 hours to obtain the nano colloid particle which is named as N1.
Nano-colloid particle preparation example 2: preparation of nano-colloid particles
A. Weighing 5 parts by mass of nano silicon dioxide (with the granularity of 20-60 nm), 1 part by mass of a cationic colloid stabilizer compound of formula (1) (wherein R is n-hexyl, n is 5-15), 0.5 part by mass of silicon dioxide adsorbent polymaleic acid (with the molecular weight of 3000-8000) and 95 parts by mass of ultrapure water respectively, and dividing the ultrapure water into two equal parts (namely 47.5 parts by mass) for later use;
B. adding the nano silicon dioxide into the first part of ultrapure water under stirring, adding the silicon dioxide adsorbent under stirring at 100rpm, and continuing stirring for 30 minutes to obtain an agent I for later use;
C. Adding the cationic colloid stabilizer into the second part of ultrapure water under stirring, and keeping stirring at 100rpm until the colloid stabilizer is fully swelled to obtain a reagent II for later use;
D. slowly adding the agent II while stirring the agent I at 100rpm at 25 ℃, continuously stirring until the agent II is sufficiently uniform, and standing for 10 hours to obtain the nano colloid particle which is named as N2.
Nano-colloid particle preparation example 3: preparation of nano-colloid particles
A. Weighing 15 parts of nano silicon dioxide (with the granularity of 20-60 nm), 0.1 part of a cationic colloid stabilizer compound of formula (1) (wherein R is normal eicosanyl, n is 35-50), 4 parts of a silicon dioxide adsorbent acrylic acid-maleic acid copolymer (with the molecular weight of 15000-20000) and 75 parts of ultrapure water respectively, and dividing the ultrapure water into two equal parts (namely, 37.5 parts by mass for later use;
B. adding the nano silicon dioxide into the first part of ultrapure water under stirring, adding the silicon dioxide adsorbent under stirring at 100rpm, and continuing stirring for 60 minutes to obtain an agent I for later use;
C. adding the cationic colloid stabilizer into the second part of ultrapure water under stirring, and keeping stirring at 100rpm until the colloid stabilizer is fully swelled to obtain a reagent II for later use;
D. Slowly adding the agent II while stirring the agent I at 100rpm at 25 ℃, continuously stirring until the agent II is sufficiently uniform, and standing for 7.5 hours to obtain the nano colloid particle which is named as N3.
Cleaning agent preparation example 1: preparation of cleaning agent
A1: the preparation method comprises the following steps of weighing the following components in parts by mass: 7.5 parts of nano colloid particles N1, 10 parts of pH regulator potassium carbonate, 0.3 part of surfactant lauramidopropyl betaine, 7 parts of wetting agent glycerol and 85 parts of ultrapure water;
b1: the respective components were added to a vessel and stirred at 650rpm for 1.5 hours at normal temperature to obtain a cleaning agent, which was designated as Q1.
Cleaning agent preparation example 2: preparation of cleaning agent
A1: the preparation method comprises the following steps of weighing the following components in parts by mass: 5 parts of nano colloid particles N2, 15 parts of pH regulator sodium bicarbonate, 0.1 part of surfactant 1-hexyne-1, 3-diol, 12 parts of wetting agent polyethylene glycol 400 and 75 parts of ultrapure water;
b1: the respective components were added to a vessel and stirred at a stirring speed of 300rpm for 2 hours at normal temperature, thereby obtaining a cleaning agent, which was designated as Q2.
Cleaning agent preparation example 3: preparation of cleaning agent
A1: the preparation method comprises the following steps of weighing the following components in parts by mass: 10 parts of nano colloid particles N3, 5 parts of pH regulator KOH, 0.5 part of surfactant cocoamidopropyl amine oxide, 2 parts of wetting agent polyethylene glycol monomethyl ether 2000 and 95 parts of ultrapure water;
B1: the respective components were added to a vessel and stirred at a stirring speed of 1000rpm for 1 hour at normal temperature, thereby obtaining a cleaning agent, which was designated as Q3.
Comparative cleaning agent preparation examples 1-3: preparation of comparative cleaning agent
Except for sequentially replacing the nano-colloid particles in step A1 of the detergent preparation examples 1-3 with the I-agent in step B of the nano-colloid particle preparation example 1, the I-agent in step B of the nano-colloid particle preparation example 2 and the I-agent in step B of the nano-colloid particle preparation example 3, respectively, the operations were unchanged, so that the detergent preparation examples 1-3 were repeatedly carried out, and the obtained detergents were sequentially named DQ1, DQ2 and DQ3.
That is, the preparation of the cleaning agent is carried out by using the agent I, and the cationic colloid stabilizer is not added.
Spectral characterization, stability testing and cleaning performance testing of nano-colloidal particles
I. Characterization by Infrared Spectroscopy
Characterizing the test object: nano-colloidal particles the nano-silica powder in step a of preparation example 1 (its infrared spectrum is a), the obtained complex of nano-colloidal particles and silica adsorbent polypropylene (i.e. agent I, its infrared spectrum is b), and finally obtained nano-colloidal particles N1 (its infrared spectrum is c).
The results are shown in FIG. 2:
1. 3421cm in b Spectrum -1 The nearby strong absorption peak is nano SiO 2 Stretching vibration peaks of-OH and O-H in upper association state, and in nano SiO 2 The absence of this peak in the a spectrum of the powder indicates that the silica powder, treated in step B with the adsorbent polyacrylic acid, has undergone hydration to form si—oh bonds, which is the onset of formation of the nano-colloidal particle structure. And the peak intensity in the b spectrum is significantly stronger than the peak intensity in the c spectrum. This is because of the passing ofAfter the step C treatment of the colloid stabilizer, the Si-OH is wrapped in the integral structure of the particle by the polyacrylic acid main chain and the colloid stabilizer, so that the peak intensity of the Si-OH in the C spectrum is weakened.
2. 803cm in the a-spectrum -1 The nearby weak absorption peak is the Si-O stretching vibration peak, whereas in b and c there is no such peak, because of SiO 2 Binding with adsorbent polyacrylic acid, thereby causing SiO 2 Due to the change of dipole moment of Si-O, the SiO is proved 2 And the colloidal adsorbent polyacrylic acid.
3. The spectrum c is compared with the spectrum b in the whole, at 1481.55cm -1 There is a distinct absorption peak, which is the quaternary ammonium salt-N (CH) in the cationic colloidal stabilizer 3 ) 3 Is a deformation absorption vibration peak of (2); and 1024.05cm -1 The absorption peak at the site is the-CH 2 -O-CH 2 (i.e. the-CH on the side chain of the six-membered ring of the glycoside) 2 -O-CH 2 ) Is a stretching vibration peak of (2); 1607cm in b-spectrum -1 The absorption peak at the point is the O-H bending vibration peak of the silica adsorbent polyacrylic acid after absorbing a small amount of water, compared with 1607cm in the c spectrum -1 The absorption peak at the site is significantly reduced. The reason is that after the treatment of the colloid stabilizer, the O-H bending vibration peak of the polyacrylic acid is wrapped in the integral structure of the particle by the colloid stabilizer, so that the peak intensity of the O-H in the c spectrum is weakened.
The infrared spectrum test was performed on the nano-silica used in nano-colloidal particle preparation examples 2 to 3, the agent I formed by the silica adsorbent (polymaleic acid and acrylic acid-maleic acid copolymer, respectively) and the nano-silica, and the final corresponding nano-colloidal particles obtained, and the change and trend of the corresponding spectrum peaks also prove the same results in the above examples 1 to 3, so that the list is not repeated.
II. Stability test of nano colloid particles
Fig. 2 is a TEM microstructure of the composite (i.e. agent I) obtained in step B of nano-colloidal particle preparation example 1 and the finally obtained nano-colloidal particle N1 after standing for 1 day, 30 days, wherein: 3 (1) is the morphology of the composite and the nano-colloid particle N1 after standing for 1 day (only one is listed because the two are highly similar), 3 (2) is the TEM micro morphology of the composite after standing for 30 days, and 3 (3) is the TEM micro morphology of the nano-colloid particle N1 after standing for 30 days.
It can be seen from this: the colloid particles of the agent I and the nano colloid particles N1 after standing for 1 day are ellipsoidal, uniformly distributed and have no agglomeration phenomenon. However, as the storage time increases, the agent I which is not treated by the cationic colloidal stabilizer in the step C is obviously polymerized in 30 days, so that the colloidal particles are obviously agglomerated and are not in an evenly distributed ellipsoidal structure. Compared with the prior art, after the cationic colloid stabilizer is added in the step C, the microcolloidal particle N1 is still highly stable even if being kept for 30 days, and almost no change (slight increase in granularity) is caused after being kept for 1 day, and the particle is still uniform ellipsoidal and no agglomeration is caused, so that the addition of the colloid stabilizer can greatly and remarkably improve the long-term stability of the nano colloid particle, and almost keep the original morphology unchanged.
The same stability tests were performed on the corresponding agents I and N2, N3 obtained in nano-colloidal particle preparations 2-3, and the TEM microcosmic morphology was highly similar to that of fig. 3, so that the list is not repeated.
III, cleaning Performance test of nano colloid particles
The polished lithium tantalate wafer was cleaned according to the prior art cleaning method according to CN103603054a, in particular according to example 3 thereof, without etching treatment, i.e. as follows:
A lithium tantalate substrate with a thickness of 55-65 μm is put on a wafer holder, the wafer holder containing the lithium tantalate substrate is firstly ultrasonically cleaned with acetone (mass fraction 99.5%) for 20-30 minutes (ultrasonic temperature 80 ℃), then with absolute ethyl alcohol (mass fraction 99.7%) for 20-30 minutes (ultrasonic temperature 80 ℃), and finally with deionized water for 20 minutes. And then the surface of the crystal is cleaned by deionized water in a mode of combining fast flushing and slow flushing, the flushing time is 30 seconds to 1 minute, and the wafer is manually flushed. Finally, the wafer is put into a drying box to be dried for 1 to 2 minutes at the temperature of 50 to 60 ℃.
The cleaning method of the invention uses the cleaning agent Q1 to clean, and comprises the following steps:
s1: adding a cleaning agent Q1 into a cleaning tank, and then placing a lithium tantalate wafer piece to be cleaned into the cleaning tank;
s2: opening ultrasonic, setting ultrasonic current to be 2A, and performing ultrasonic cleaning for 8 minutes;
s3: and taking out the lithium tantalate wafer from the cleaning tank, cleaning the lithium tantalate wafer with ultrapure water (the resistance is not less than 18MΩ) for 3 times, and finally drying the lithium tantalate wafer in vacuum to finish cleaning.
Each lithium tantalate wafer was subjected to particle residue detection after cleaning using AOI, which is an optical detection, the detection process being: by scanning the wafer with light of different wavelengths, substances not belonging to the material of the wafer bottom itself are displayed in a color pattern, i.e. inorganic particles and/or metal particles on the wafer surface.
The results are shown in FIG. 4, and can be seen in FIG. 4: after cleaning using the prior art cleaning method, more particulate impurities remain on the lithium tantalate wafer (see figure 4 left). After the cleaning agent is used for cleaning, the particle impurities on the lithium tantalate wafer are very few (see the right figure of the attached figure 4), and the cleaning effect is very excellent.
When cleaning is performed using the cleaning agents Q2 and Q3, the particle removal effect is highly similar to that of the right diagram of fig. 4, and thus the list is not repeated.
IV, surface anti-particle redeposition performance test of nano colloid particles
In order to examine the effect on the anti-redeposition properties of the surface due to the presence of the cationic colloidal stabilizer in the nano-colloidal particles of the present invention, the polished lithium tantalate wafers were cleaned using Q1 and DQ1, respectively, in the same manner as the cleaning operation in "III" above.
After the cleaning, the lithium tantalate wafer is placed in air with the cleanliness of ten thousand grades, and the AOI surface particle residue detection is carried out again after 1h and 24h respectively.
The results are shown in FIG. 5, wherein: the upper left is a particle residue detection graph after 1 hour of standing after cleaning with Q1, and the upper right is a particle residue detection graph after 24 hours of standing; the lower left is a graph of particle residue after 1 hour of standing after washing with DQ1, and the lower right is a graph of particle residue after 24 hours of standing.
It is clear from this: 1. after 24 hours of standing with Q1 cleaning, the particles on the wafer surface were slightly increased compared to 1 hour of standing, and the surface cleanliness was not significantly changed (see upper left and upper right). 2. However, after 24 hours of rinsing with DQ1, the particles on the wafer surface are significantly increased compared with those after 1 hour of rinsing, and the surface cleanliness is significantly deteriorated, especially, the wafer surface has serious particle redeposition and adsorption aggregation phenomena (see lower left and lower right). 3. The anti-particle redeposition effect of Q1 was also significantly better than DQ1 after 1 hour of standing (see upper left versus lower left).
This demonstrates that the use of cationic colloidal stabilizers can achieve excellent anti-particle redeposition properties in addition to excellent wafer surface particle removal properties. The method is characterized in that the combination of the cationic colloid stabilizer and the colloid particles is a dynamic balance process, and in the process of the nano colloid particles playing a cleaning role, part of the cationic stabilizer is released, so that the surface of the lithium tantalate wafer can be cationized and modified in the cleaning process to form a layer of molecular-level antistatic protective film. The lithium tantalate wafer after cationic modification has antistatic property, so that tiny dust or particles in the environment can be effectively prevented from being adsorbed and accumulated on the surface of the wafer again.
When the test was performed using Q2-Q3 and DQ2-DQ3, the results are highly similar to FIG. 5 and therefore are not repeated.
V, lithium tantalate wafer fragment rate test
The respective chipping rates (including chipping, edge chipping, and any cases involving cracking or complete chipping) were examined by performing cleaning according to the prior art cleaning method and the inventive cleaning method in the above-described III, respectively, using 20 lithium tantalate wafers as a set of tests, and the results are shown in table 1 below.
TABLE 1
Therefore, the invention can clean at normal temperature without high temperature and ultrasonic operation without long time by using the cleaning agent containing unique nano colloid particles, thereby avoiding the occurrence of fragmentation, and having obvious industrial significance for improving the product yield and reducing the wafer production cost on a large scale.
As described above, the present invention provides a nano-colloidal particle, a method for preparing the same, a use thereof, a cleaning agent comprising the same, a method for preparing the same, a method for cleaning a surface of a soft and brittle material, particularly a lithium tantalate wafer using the same, etc., wherein the nano-colloidal particle forms a nano-colloidal particle having a unique structure through nano-silica, a silica adsorbent and a cationic colloidal stabilizer, has excellent stability, particle cleaning and anti-particle redeposition effects, is particularly suitable for surface cleaning of a soft and brittle material such as a lithium tantalate wafer, and can prevent occurrence of broken pieces, and has remarkable industrial significance.
It should be understood that these examples are for the purpose of illustrating the application only and are not intended to limit the scope of the application. Furthermore, it is to be understood that various changes, modifications and/or variations may be made by those skilled in the art after reading the technical content of the present application, and that all such equivalents are intended to fall within the scope of the present application as defined in the appended claims.
Claims (9)
1. A nano-colloidal particle comprising nano-silica, a silica adsorbent, and a cationic colloidal stabilizer;
the silicon dioxide adsorbent is any one or a mixture of any plurality of polyacrylic acid, polymaleic acid, acrylic acid-maleic acid copolymer or acrylic acid-styrene copolymer;
the cationic colloid stabilizer is a cationic ammonium oligomer of the following formula (1):
wherein:
r is H or C 6-20 An alkyl group;
n is a degree of polymerization selected from integers from 5 to 50;
x is halogen.
2. The nano-colloid particles according to claim 1, wherein: the granularity of the nano silicon dioxide is 1-100 nm.
3. The nano-colloidal particles according to claim 2, wherein: the granularity of the nano silicon dioxide is 20-60 nm.
4. Use of the nano-colloidal particles according to any of claims 1-3 for cleaning the surface of a soft and brittle material.
5. A method of preparing the nano-colloidal particles according to any one of claims 1 to 3, the method comprising the steps of:
A. weighing 5-15 parts of nano silicon dioxide, 0.01-1 part of cationic colloid stabilizer, 0.5-4 parts of silicon dioxide adsorbent and 75-95 parts of ultrapure water according to parts by mass, and dividing the ultrapure water into two equal parts for later use;
B. adding the nano silicon dioxide into the first part of ultrapure water under stirring, adding the silicon dioxide adsorbent under stirring, and continuing stirring for 30-60 minutes to serve as an agent I for standby;
C. adding the cationic colloid stabilizer into the second part of ultrapure water under stirring, and keeping stirring until the colloid stabilizer is fully swelled to serve as a II agent for standby;
D. slowly adding the agent II while stirring the agent I at 25 ℃, continuously stirring until the agent is sufficiently uniform, and standing for 5-10 hours to obtain the nano colloid particles.
6. A cleaning agent for cleaning the surface of a soft and brittle material, which comprises, by mass, 5-10 parts of the nano colloid particles according to any one of claims 1-3, 5-15 parts of a pH regulator, 0.1-0.5 part of a surfactant, 2-12 parts of a wetting agent and 75-95 parts of ultrapure water.
7. The method for preparing the cleaning agent as claimed in claim 6, comprising the steps of:
a1: respectively weighing nano colloid particles, a pH regulator, a surfactant, a wetting agent and ultrapure water in parts by mass;
b1: adding each component into a container, and stirring at the stirring speed of 300-1000 rpm for 1-2 hours at normal temperature to obtain the cleaning agent.
8. A surface cleaning method for a soft and brittle material, the surface cleaning method comprising the steps of:
s1: adding the cleaning agent according to claim 6 into a cleaning tank, and then placing the soft and brittle material to be cleaned into the cleaning tank;
s2: opening ultrasonic waves to carry out ultrasonic cleaning;
s3: and taking the soft and brittle material out of the cleaning tank, cleaning the soft and brittle material with ultrapure water for 2-3 times, and finally drying the soft and brittle material in vacuum to finish the cleaning method.
9. The surface cleaning method of claim 8, wherein: the soft and brittle material in step S1 is a lithium tantalate wafer.
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| CN103603054A (en) * | 2013-10-15 | 2014-02-26 | 电子科技大学 | Method for preparing lithium tantalite wafer |
| CN107345178A (en) * | 2017-07-07 | 2017-11-14 | 广州克思曼研磨科技有限公司 | A kind of nanometer cleaning-nursing liquid and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103603054A (en) * | 2013-10-15 | 2014-02-26 | 电子科技大学 | Method for preparing lithium tantalite wafer |
| CN107345178A (en) * | 2017-07-07 | 2017-11-14 | 广州克思曼研磨科技有限公司 | A kind of nanometer cleaning-nursing liquid and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 阳离子烷基糖昔的合成及应用;司西强 等;精细石油化工进展;第12卷(第11期);27-31 * |
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