CN106811135A - A kind of oily bag acidic ion liquid polishing fluid for KDP crystal - Google Patents
A kind of oily bag acidic ion liquid polishing fluid for KDP crystal Download PDFInfo
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- CN106811135A CN106811135A CN201710017150.7A CN201710017150A CN106811135A CN 106811135 A CN106811135 A CN 106811135A CN 201710017150 A CN201710017150 A CN 201710017150A CN 106811135 A CN106811135 A CN 106811135A
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- ion liquid
- acidic ion
- polishing
- polishing fluid
- kdp crystal
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- 238000005498 polishing Methods 0.000 title claims abstract description 80
- 239000013078 crystal Substances 0.000 title claims abstract description 54
- 239000012530 fluid Substances 0.000 title claims abstract description 38
- 239000007788 liquid Substances 0.000 title claims abstract description 36
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 29
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 239000004064 cosurfactant Substances 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 26
- 150000002500 ions Chemical class 0.000 claims description 26
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 22
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- 229910019142 PO4 Inorganic materials 0.000 claims description 13
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 12
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 9
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 8
- 239000010452 phosphate Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000000263 2,3-dihydroxypropyl (Z)-octadec-9-enoate Substances 0.000 claims description 6
- RZRNAYUHWVFMIP-GDCKJWNLSA-N 3-oleoyl-sn-glycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-GDCKJWNLSA-N 0.000 claims description 6
- RZRNAYUHWVFMIP-UHFFFAOYSA-N monoelaidin Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-UHFFFAOYSA-N 0.000 claims description 6
- 229940093609 tricaprylin Drugs 0.000 claims description 6
- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 claims description 6
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims description 6
- -1 1- hexyl -3- methylimidazole hexafluorophosphates Chemical class 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 239000003495 polar organic solvent Substances 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- AJTWAFXXIGBVRF-UHFFFAOYSA-N pyridine;sulfo hydrogen sulfate Chemical compound C1=CC=NC=C1.OS(=O)(=O)OS(O)(=O)=O AJTWAFXXIGBVRF-UHFFFAOYSA-N 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000004530 micro-emulsion Substances 0.000 abstract description 21
- 239000000126 substance Substances 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 150000007524 organic acids Chemical class 0.000 abstract description 6
- 238000005520 cutting process Methods 0.000 abstract description 5
- 238000007521 mechanical polishing technique Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000003746 surface roughness Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000003518 caustics Substances 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 36
- 239000013504 Triton X-100 Substances 0.000 description 13
- 229920004890 Triton X-100 Polymers 0.000 description 13
- 238000004140 cleaning Methods 0.000 description 7
- IDOQDZANRZQBTP-UHFFFAOYSA-N 2-[2-(2,4,4-trimethylpentan-2-yl)phenoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=CC=C1OCCO IDOQDZANRZQBTP-UHFFFAOYSA-N 0.000 description 6
- 229920004929 Triton X-114 Polymers 0.000 description 6
- 230000006378 damage Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RVEJOWGVUQQIIZ-UHFFFAOYSA-N 1-hexyl-3-methylimidazolium Chemical compound CCCCCCN1C=C[N+](C)=C1 RVEJOWGVUQQIIZ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- GCFHZZWXZLABBL-UHFFFAOYSA-N ethanol;hexane Chemical compound CCO.CCCCCC GCFHZZWXZLABBL-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 150000007530 organic bases Chemical class 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 2
- WGVGZVWOOMIJRK-UHFFFAOYSA-N 1-hexyl-3-methyl-2h-imidazole Chemical compound CCCCCCN1CN(C)C=C1 WGVGZVWOOMIJRK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- VFNGKCDDZUSWLR-UHFFFAOYSA-L disulfate(2-) Chemical compound [O-]S(=O)(=O)OS([O-])(=O)=O VFNGKCDDZUSWLR-UHFFFAOYSA-L 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- FMYKJLXRRQTBOR-BZSNNMDCSA-N acetylleucyl-leucyl-norleucinal Chemical compound CCCC[C@@H](C=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](CC(C)C)NC(C)=O FMYKJLXRRQTBOR-BZSNNMDCSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 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
- C09G1/06—Other polishing compositions
- C09G1/14—Other polishing compositions based on non-waxy substances
- C09G1/18—Other polishing compositions based on non-waxy substances on other substances
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention provides a kind of oily bag acidic ion liquid polishing fluid for KDP crystal, the polishing fluid is by oil phase, dispersion phase solvent, acidic ion liquid(AIL), surfactant and cosurfactant composition.In the presence of surfactant and cosurfactant, AIL solution is covered by oil phase as dispersed phase, forms oily bag acidic ion liquid microemulsion(AIL/O).In chemically mechanical polishing, AIL/O microemulsions are squeezed and rubbing action, and AIL molecules break through interfacial film and reach plane of crystal, and are chemically reacted with rat position, realize the selective removal on surface.AIL/O polishing fluids for KDP crystal of the invention, prepare simple, stable in properties, the characteristics of having considered the response characteristic and chemical Mechanical Polishing Technique of KDP crystal, both possessed the high selectivity of microemulsion deliquescence polishing, the again compatible advantage of organic acid/caustic corrosion polishing, fly-cutting knife mark can effectively be weakened, surface roughness, and surface noresidue is reduced.
Description
Technical field
The invention belongs to Ultra-precision Turning and the cross-application field of functionalization microemulsion reaction methods, and in particular to one kind is used for
The oily bag acidic ion liquid polishing fluid of KDP crystal.
Background technology
Potassium dihydrogen phosphate(KDP)Crystal is a kind of very excellent optical crystal for growing up the forties in 20th century, is
The non-thread of the currently the only laser freuqency doubling, Electro-optical Modulation and photoelectric switching device that can be used for the light path systems such as ICF, light laser weapon
Property optical material.Surface quality requirements in engineer applied to KDP crystal are high, such as ultra-smooth, free of surface defects, unstressed residual
Remaining and free from admixture residual etc., the limit of intimate material processing.However, KDP crystalline materials are in itself with soft crisp, easy deliquescence, to temperature
The features such as degree sensitive and anisotropy, it is acknowledged as one of most unmanageable optical element.It is this kind of for KDP crystal soft
Crisp material, obtains super-smooth surface extremely difficult.The ultraprecise processing method master of comparative maturity in current domestic and international project application
If single-point diamond fly-cutting(SPDT)Technology and Technique of Magnetorheological Finishing(MRF), U.S. LLNL laboratories and China Harbin
The units such as polytechnical university have made certain gains in the field.But, KDP crystal is processed using SPDT technologies, can be in crystal table
Face produces periodicity Microscale waveness(Fly-cutting knife mark)And sub-surface damage, high power laser light effect under easily produce damage and
Destruction.Although MRF can cut down the Microscale waveness of SPDT technologies generation, the micro-nanos such as iron powder can be produced in plane of crystal
The embedded phenomenon of grain, in addition, the cleaning at plane of crystal magnetorheological residual night is also current a great problem.Development is soft for KDP etc.
The new ultra-smooth of crisp deliquescent crystal, low damage, low defect " soft polishing " technology it is imperative.
Chemically mechanical polishing is a kind of surface polishing technique highly developed in semicon industry, and it can realize work
, there is technical advantage in terms of super-smooth surface is prepared in the planarization in the full-scale scope of part.In chemically mechanical polishing, polishing
Liquid is one of core of whole technical matters, and its physicochemical properties decides the precision level of chemically mechanical polishing, if choosing
With traditional polishing fluid, KDP planes of crystal can be caused to be atomized or damage.Currently for the chemistry of the soft crisp deliquescent crystal such as KDP
Mechanical polishing, it is main using based on Water-In-Oil(W/O)The deliquescence polishing principles of microemulsion and the chemical attack based on organic acid/base
Polishing.
" a kind of non-water base polishing without abrasive for soft crisp deliquescent crystal entitled disclosed in Chinese patent literature storehouse
The patent of liquid ", Patent No. CN00910010268.2, the patent is from alcohol or ester as oil phase, high-carbon fatty alcohol polyoxyethylene
The nonionic surfactants such as ether are prepared for the microemulsion of Water-In-Oil as surface reactive material.The microemulsion is by deliquescent effect
Nano grade is narrowed down to, for the polishing of KDP crystal, it is possible to achieve the selectivity of plane of crystal is uniformly removed.But due to water
Deliquescent effect intensity to KDP crystal is very big, and the clearance of plane of crystal deliquescence microcell is uncontrollable during polishing, it is easy to
Surface produces small etch pit, and polishing removal fine degree is low.The method defect of the deliquescence polishing principles based on microemulsion, mainly
It is attributed to:(1)Though W/O microemulsion reclaimed water cores size is Nano grade, each water checks the deliquescent effect intensity of KDP crystal
It is uncontrollable, and during CMP, due to the participation of mechanism, the deliquescent effect that further can expand in microcell is strong
Degree, eventually results in chemical machinery removal precision and is difficult to control to, and clearance can only be controlled in 100 nanometer level, KDP planes of crystal
Etch pit is easily produced, Precision Machining is difficult to.(2)Deliquescent effect forms the KDP aqueous solution on KDP quartz crystals surface, by
In the KDP aqueous solution in organic solvent(Oil phase)In solubility it is very low, inevitably KDP planes of crystal produce residual simultaneously
Recrystallization, causes remained on surface KDP crystallites, influences surface quality.
It is entitled disclosed in Chinese patent literature storehouse that " anhydrous polishing without abrasive is used in soft crisp deliquescent crystal chemically mechanical polishing
The patent of liquid ", Patent No. CN102660198 A, the patent be prepared for it is a kind of by organic corrosion agent, organic corrosion inhibitor,
The anhydrous agranular type polishing fluid of surfactant, organic pH value regulator and organic solvent composition, it is to avoid deliquescence polishing
Plane of crystal problems of crack.But the polishing fluid of composition mode is used, there is static corrosion effect, and to table during polishing
The poor selectivity in face site, directly affects final quality of finish.For the chemical etch polishing based on organic acid/base, must
Polishing fluid must further be reduced to the static corrosion of KDP crystal and the high selectivity of polishing fluid is improved.
From the above analysis, chemical Mechanical Polishing Technique is expected to realize in theory ultra-smooth, the ultra-clean of KDP crystal
Surface Machining target, but the chemical etch polishing that the deliquescence for being currently based on microemulsion polishes theoretical and organic acid/base is theoretical
There is a problem that being difficult to overcome.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of oily bag acidic ion liquid polishing for KDP crystal
Liquid.
Oily bag acidic ion liquid polishing fluid for KDP crystal of the invention, is characterized in:Described polishing fluid each group
Point mass percent be:
Oil phase:25%~60%;
Dispersion phase solvent:10%~15%;
Acidic ion liquid:5%~15%;
Surfactant:15%~45%;
Cosurfactant:5%~15%.
Described oil phase be non-polar organic solvent, hexamethylene, n-hexane, glyceryl monooleate, olein or
One kind in tricaprylin.
Described dispersion phase solvent is ethanol, isopropanol or 1- hexyl -3- methylimidazole hexafluorophosphates([Hmim]PF6)
In one kind.
Described acidic ion liquid is bis-trifluoromethylsulfoandimide(TFSI), caprolactam phosphate([NHCH]
H2PO4), N, N '-dimethylformamide phosphate([DMFH]H2PO4), 1- butyl -3- methylimidazolium hydrogen sulphate salt([Bmim]
HSO4)Or pyridine disulfate([Py]HSO4)In one kind.
Described surfactant is in NPE, alkyl polyoxyethylene ether or AEO
One kind.
Described cosurfactant is the one kind in n-butanol, n-amyl alcohol, n-hexyl alcohol or n-octyl alcohol.
The preparation environment temperature of described polishing fluid is 20 DEG C ~ 25 DEG C, and relative humidity is 30% ~ 50%, and air pressure is normal pressure.
Polishing fluid of the invention is oily bag acidic ion liquid microemulsion, considered KDP crystal response characteristic and
The characteristics of chemical Mechanical Polishing Technique, overcome current KDP crystal deliquescence polishing water-in-oil microemulsion and organic acid/alkalization is learned
The defect and deficiency of etch polishing liquid, while having had high selectivity and organic acid/caustic corrosion polishing that microemulsion deliquescence is polished concurrently
Complete anhydrous feature, be a kind of more advanced polishing fluid.The present invention is coated by active component acidic ion liquid,
And the multi- scenarios method mechanism for chemically-mechanicapolish polishing is combined, basic point of departure is controlled to Chemical Kinetics on interface, to acid
The release of property ionic liquid, interface interaction form and Chemical Kinetics carry out interface regulation and control, react the removal in microcell
More controllable precise, the organic solution of KDP planes of crystal residual after polishing, KDP is capable of achieving by the organic solvent for matching
Plane of crystal is cleaned, and secondary damage will not be caused to KDP planes of crystal, finally realizes the controllable removal of pointwise of KDP crystal.
Specific embodiment
The present invention is described in detail with reference to embodiment.
Oily bag acidic ion liquid polishing fluid for KDP crystal of the invention, the mass percent of each component is:
Oil phase:25%~60%;
Dispersion phase solvent:10%~15%;
Acidic ion liquid:5%~15%;
Surfactant:15%~45%;
Cosurfactant:5%~15%.
Described oil phase be non-polar organic solvent, hexamethylene, n-hexane, glyceryl monooleate, olein or
One kind in tricaprylin.
Described dispersion phase solvent is ethanol, isopropanol or 1- hexyl -3- methylimidazole hexafluorophosphates([Hmim]PF6)
In one kind.
Described acidic ion liquid is bis-trifluoromethylsulfoandimide(TFSI), caprolactam phosphate([NHCH]
H2PO4), N, N '-dimethylformamide phosphate([DMFH]H2PO4), 1- butyl -3- methylimidazolium hydrogen sulphate salt([Bmim]
HSO4)、)Or pyridine disulfate([Py]HSO4)In one kind.
Described surfactant is in NPE, alkyl polyoxyethylene ether or AEO
One kind.
Described cosurfactant is one kind of n-butanol, n-amyl alcohol, n-hexyl alcohol or n-octyl alcohol.
The preparation environment temperature of described polishing fluid is 20 DEG C ~ 25 DEG C, and relative humidity is 30% ~ 50%, and air pressure is normal pressure.
Polishing fluid of the invention is oily bag acidic ion liquid microemulsion, with oil phase, acidic ion liquid, surfactant
It is technological means with the quasi- ternary phase diagrams of cosurfactant, is drawn by phasor, obtains the single-phase of oily bag acidic ion liquid
Micro-emulsion region.The polishing fluid of different ratio is screened in Monophase microemulsion area, machine light is thrown using chemical machinery and is realized polishing fluid pair
The polishing of KDP crystal.
Embodiment 1
The present embodiment is implemented according to following steps:
(1)The acquisition of initial surface:KDP crystal with 35 mm × 35 mm of single-point diamond fly-cutting is polished crystal;
(2)The preparation of oily bag acidic ion liquid microemulsion:Oil phase is hexamethylene, and dispersion phase solvent is isopropanol, acid ion
Liquid is bis-trifluoromethylsulfoandimide(TFSI), surfactant is Triton X-100(Triton X-100), help
Surfactant is n-octyl alcohol;During preparation, TFSI is well mixed with isopropanol, is added dropwise to n-hexane, Triton X-
100 and n-octyl alcohol mixed solution in, wherein the mass percent of each component be 45:10:5:32:8, the microemulsion is labeled as A
Polishing fluid;
(3)Chemically mechanical polishing experiment:Using chemical-mechanical polishing mathing, the polishing experiments of KDP crystal, wherein A polishing fluids are carried out
Rate of addition be 10 ml/min, polish pressure is 2.5 KPa, the rpm of master rotating speed 60, holds thing ring rotating speed for 60 rpm, is thrown
The min of light time 10.
(4)Cleaned after polishing:Successively using isopropanol, n-hexane as cleaning fluid, after auxiliary mega sonic wave is polished
Cleaning, is then dried up with clean dried gas.
Under the polishing condition, after polishing and completing cleaning, the surface roughness of sample is 1.96 nm.
Embodiment 2
The present embodiment is implemented according to following steps:
(1)The acquisition of initial surface:KDP crystal with 35 mm × 35 mm of single-point diamond fly-cutting is polished crystal;
(2)The preparation of oily bag acidic ion liquid microemulsion:Oil phase is hexamethylene, and dispersion phase solvent is [Hmim] PF6, it is acid from
Sub- liquid is caprolactam phosphate([NHCH]H2PO4), surfactant is Triton X-100(Triton X-
100), cosurfactant is n-hexyl alcohol;During preparation, caprolactam phosphate is well mixed with ethanol, is added dropwise to ring
In the mixed solution of hexane, Triton X-100 and n-hexyl alcohol, wherein the mass percent of each component is 50:10:5:
30:5, the microemulsion is labeled as B polishing fluids;
(3)Chemically mechanical polishing experiment:Using chemical-mechanical polishing mathing, the polishing experiments of KDP crystal, wherein B polishing fluids are carried out
Rate of addition be 10 ml/min, polish pressure is 2.5 KPa, the rpm of master rotating speed 60, holds thing ring rotating speed for 60 rpm, is thrown
The min of light time 10.
(4)Cleaned after polishing:Successively using isopropanol, n-hexane as cleaning fluid, after auxiliary mega sonic wave is polished
Cleaning, is then dried up with clean dried gas.
Under the polishing condition, after polishing and completing cleaning, the surface roughness of sample is 2.18 nm.
Remaining embodiment is essentially identical with the implementation method of embodiment 1 and embodiment 2, differs primarily in that matching somebody with somebody for microemulsion
Fang Butong;In polishing process, polishing fluid rate of addition, polish pressure, master rotating speed, hold thing ring rotating speed keep it is constant.Specifically
Embodiment experimental result be summarised in table 1.
The IL/O polishing fluids of table 1. are constituted and polishing experiments acetonideexample
| Embodiment | Oil phase | Dispersion phase solvent | AIL | Surfactant | Cosurfactant | Each component mass percent | Roughness after polishing |
| 3 | Hexamethylene | Isopropanol | TFSI | Triton X-100 | N-octyl alcohol | 45:10:5:30:10 | 2.06 |
| 4 | Hexamethylene | Isopropanol | TFSI | Triton X-100 | N-octyl alcohol | 45:15:5:30:5 | 1.73 |
| 5 | Hexamethylene | Isopropanol | TFSI | Triton X-100 | N-octyl alcohol | 40:10:5:30:15 | 1.85 |
| 6 | N-hexane | Ethanol | Triton X-114 | N-hexyl alcohol | 50:15:5:24:6 | 2.18 | |
| 7 | N-hexane | Ethanol | Triton X-114 | N-hexyl alcohol | 45:20:5:24:6 | 2.23 | |
| 8 | N-hexane | Ethanol | Triton X-114 | N-hexyl alcohol | 35:30:5:24:6 | 2.47 | |
| 9 | Glyceryl monooleate | Triton X-114 | N-butanol | 30:15:15:32:8 | 2.04 | ||
| 10 | Glyceryl monooleate | Triton X-114 | N-butanol | 30:20:10:32:8 | 1.82 | ||
| 11 | Glyceryl monooleate | Triton X-114 | N-butanol | 30:25:5:32:8 | 1.96 | ||
| 12 | Olein | Isopropanol | Triton X-100 | N-octyl alcohol | 30:10:5:45:10 | 2.29 | |
| 13 | Olein | Isopropanol | Triton X-100 | N-octyl alcohol | 30:10:5:40:15 | 2.58 | |
| 14 | Olein | Isopropanol | Triton X-100 | N-octyl alcohol | 30:10:5:35:20 | 2.87 | |
| 15 | Tricaprylin | Ethanol | Triton X-100 | N-amyl alcohol | 60:5:5:24:6 | 3.15 | |
| 16 | Tricaprylin | Ethanol | Triton X-100 | N-amyl alcohol | 40:15:5:32:8 | 2.72 | |
| 17 | Tricaprylin | Ethanol | Triton X-100 | N-amyl alcohol | 35:20:5:32:8 | 2.31 |
The description for more than applying example is more specific, detailed, but can not be therefore understands that being the limitation to this patent scope, it should be pointed out that
It is that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, some deformations can also be made
And improvement, these belong to protection scope of the present invention.
Claims (7)
1. a kind of oily bag acidic ion liquid polishing fluid for KDP crystal, it is characterised in that:Described polishing fluid each component
Mass percent is:
Oil phase:25%~60%;
Dispersion phase solvent:10%~15%;
Acidic ion liquid:5%~15%;
Surfactant:15%~45%;
Cosurfactant:5%~15%.
2. the oily bag acidic ion liquid polishing fluid for KDP crystal according to claim 1, it is characterised in that:It is described
Oil phase be non-polar organic solvent, hexamethylene, n-hexane, glyceryl monooleate, olein or tricaprylin
In one kind.
3. the oily bag acidic ion liquid polishing fluid for KDP crystal according to claim 1, it is characterised in that:It is described
Dispersion phase solvent be ethanol, isopropanol or 1- hexyl -3- methylimidazole hexafluorophosphates in one kind.
4. the oily bag acidic ion liquid polishing fluid for KDP crystal according to claim 1, it is characterised in that:It is described
Acidic ion liquid be bis-trifluoromethylsulfoandimide, caprolactam phosphate, N, N '-dimethylformamide phosphate, 1- fourths
One kind in base -3- methylimidazolium hydrogen sulphates salt or pyridine disulfate.
5. the oily bag acidic ion liquid polishing fluid for KDP crystal according to claim 1, it is characterised in that:It is described
Surfactant be the one kind in NPE, alkyl polyoxyethylene ether or AEO.
6. the oily bag acidic ion liquid polishing fluid for KDP crystal according to claim 1, it is characterised in that:It is described
Cosurfactant be the one kind in n-butanol, n-amyl alcohol, n-hexyl alcohol or n-octyl alcohol.
7. the oily bag acidic ion liquid polishing fluid for KDP crystal according to claim 1, it is characterised in that:It is described
Polishing fluid preparation environment temperature be 20 DEG C ~ 25 DEG C, relative humidity be 30% ~ 50%, air pressure is normal pressure.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110295011A (en) * | 2019-07-17 | 2019-10-01 | 中国工程物理研究院机械制造工艺研究所 | A kind of polishing fluid for KDP crystal and preparation method thereof, application |
| CN110405543A (en) * | 2019-08-05 | 2019-11-05 | 衢州学院 | Ferrite substrate polishing method adopting acidic polishing solution and metal-based polishing disk |
| CN111136812A (en) * | 2019-12-11 | 2020-05-12 | 中国工程物理研究院机械制造工艺研究所 | Combined processing method of phosphorus germanium zinc crystal |
| CN111763478A (en) * | 2020-07-21 | 2020-10-13 | 中国工程物理研究院机械制造工艺研究所 | Chemical polishing solution for KDP crystal, preparation method and polishing method |
| CN112213173A (en) * | 2020-09-29 | 2021-01-12 | 山东大学 | KH (KH-wall building block)2PO4Method for generating clear dislocation etch pit on crystal {101} crystal face |
| CN114561643A (en) * | 2022-03-16 | 2022-05-31 | 四川大学 | A kind of aluminum chemical polishing liquid and polishing method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060183654A1 (en) * | 2005-02-14 | 2006-08-17 | Small Robert J | Semiconductor cleaning using ionic liquids |
| CN101422744A (en) * | 2008-12-10 | 2009-05-06 | 云南民族大学 | Ion super strong acid and synthesis method thereof |
| CN101481586A (en) * | 2009-01-20 | 2009-07-15 | 大连理工大学 | Nonaqueous non-abrasive polishing solution for soft, crisp and deliquescent crystal |
| CN101536171A (en) * | 2006-11-08 | 2009-09-16 | 圣劳伦斯纳米科技有限公司 | Chemical mechanical polishing of moisture sensitive surfaces and compositions therefor |
| CN102660198A (en) * | 2012-04-11 | 2012-09-12 | 南京航空航天大学 | Waterless abrasive-free polishing solution for chemical-mechanical polishing of flexible, crisp and deliquescent crystals |
| KR20130071089A (en) * | 2011-12-20 | 2013-06-28 | 주식회사 동진쎄미켐 | Chemical mechanical polishing slurry composition |
| CN103820079A (en) * | 2014-02-21 | 2014-05-28 | 无锡研奥电子科技有限公司 | Grinding composition used for gallium nitride material, and its preparation method |
-
2017
- 2017-01-11 CN CN201710017150.7A patent/CN106811135B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060183654A1 (en) * | 2005-02-14 | 2006-08-17 | Small Robert J | Semiconductor cleaning using ionic liquids |
| CN101536171A (en) * | 2006-11-08 | 2009-09-16 | 圣劳伦斯纳米科技有限公司 | Chemical mechanical polishing of moisture sensitive surfaces and compositions therefor |
| CN101422744A (en) * | 2008-12-10 | 2009-05-06 | 云南民族大学 | Ion super strong acid and synthesis method thereof |
| CN101481586A (en) * | 2009-01-20 | 2009-07-15 | 大连理工大学 | Nonaqueous non-abrasive polishing solution for soft, crisp and deliquescent crystal |
| KR20130071089A (en) * | 2011-12-20 | 2013-06-28 | 주식회사 동진쎄미켐 | Chemical mechanical polishing slurry composition |
| CN102660198A (en) * | 2012-04-11 | 2012-09-12 | 南京航空航天大学 | Waterless abrasive-free polishing solution for chemical-mechanical polishing of flexible, crisp and deliquescent crystals |
| CN103820079A (en) * | 2014-02-21 | 2014-05-28 | 无锡研奥电子科技有限公司 | Grinding composition used for gallium nitride material, and its preparation method |
Non-Patent Citations (3)
| Title |
|---|
| HUI DONG,ET AL.: "A Novel Water-in-Oil Microemulsion for KH2PO4 (KDP) Crystal Chemical Mechanical Polishing at Room Temperature", 《PROCEEDINGS OF OTA 2016-CONF.4 ADVANCED OPTICAL DESIGN AND MANUFACTURING TECHNOLOGIES》 * |
| 王碧玲: "KDP晶体无磨料水溶解抛光方法与加工机理", 《中国博士学位论文全文数据库》 * |
| 腾弘霓,等: "醇对非离子表面活性剂所形成微乳液的影响", 《吉林化工学院学报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110295011A (en) * | 2019-07-17 | 2019-10-01 | 中国工程物理研究院机械制造工艺研究所 | A kind of polishing fluid for KDP crystal and preparation method thereof, application |
| CN110295011B (en) * | 2019-07-17 | 2021-06-04 | 中国工程物理研究院机械制造工艺研究所 | Polishing solution for KDP crystal and preparation method and application thereof |
| CN110405543A (en) * | 2019-08-05 | 2019-11-05 | 衢州学院 | Ferrite substrate polishing method adopting acidic polishing solution and metal-based polishing disk |
| CN111136812A (en) * | 2019-12-11 | 2020-05-12 | 中国工程物理研究院机械制造工艺研究所 | Combined processing method of phosphorus germanium zinc crystal |
| CN111763478A (en) * | 2020-07-21 | 2020-10-13 | 中国工程物理研究院机械制造工艺研究所 | Chemical polishing solution for KDP crystal, preparation method and polishing method |
| CN111763478B (en) * | 2020-07-21 | 2021-11-02 | 中国工程物理研究院机械制造工艺研究所 | Chemical polishing solution for KDP crystal, preparation method and polishing method |
| CN112213173A (en) * | 2020-09-29 | 2021-01-12 | 山东大学 | KH (KH-wall building block)2PO4Method for generating clear dislocation etch pit on crystal {101} crystal face |
| CN114561643A (en) * | 2022-03-16 | 2022-05-31 | 四川大学 | A kind of aluminum chemical polishing liquid and polishing method thereof |
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