CN106811135B - A kind of oily packet acidic ion liquid polishing fluid for KDP crystal - Google Patents
A kind of oily packet acidic ion liquid polishing fluid for KDP crystal Download PDFInfo
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- CN106811135B CN106811135B CN201710017150.7A CN201710017150A CN106811135B CN 106811135 B CN106811135 B CN 106811135B CN 201710017150 A CN201710017150 A CN 201710017150A CN 106811135 B CN106811135 B CN 106811135B
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- 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
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The present invention provides a kind of oily packet acidic ion liquid polishing fluids for KDP crystal, and the polishing fluid is by oil phase, dispersion phase solvent, acidic ion liquid（AIL）, surfactant and cosurfactant composition.Under the action of surfactant and cosurfactant, AIL solution is covered by as dispersed phase in oil phase, forms oily packet 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 chemically react with surface bulge position, realize the selective removal on surface.The AIL/O polishing fluids for KDP crystal of the present invention, simple, property is prepared to stablize, the characteristics of having considered the response characteristic and chemical Mechanical Polishing Technique of KDP crystal, both had the highly selective of microemulsion deliquescence polishing, the advantages of being compatible with organic acid/caustic corrosion polishing again, fly-cutting knife mark can effectively be weakened, reduce surface roughness, and surface noresidue.
Description
Technical field
The invention belongs to the cross-application fields of Ultra-precision Turning and functionalization microemulsion reaction methods, and in particular to one kind is used for
The oily packet acidic ion liquid polishing fluid of KDP crystal.
Background technology
Potassium dihydrogen phosphate（KDP）Crystal is a kind of very excellent optical crystal to grow up the 1940s, is
It is currently the only available for the non-thread of the laser freuqency doubling of the light path systems such as ICF, light laser weapon, Electro-optical Modulation and photoelectric switching device
Property optical material.It is high to the surface quality requirements of KDP crystal in engineer application, 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 have soft crisp, easy deliquescence, to temperature in itself
The features such as degree variation sensitivity and anisotropy, it is acknowledged as one of most unmanageable optical element.It is this kind of soft for KDP crystal
It is extremely difficult to obtain super-smooth surface for crisp material.The ultraprecise processing method master of comparative maturity in domestic and international project application at present
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, it can be in crystal table
Face generates periodical Microscale waveness（Fly-cutting knife mark）And sub-surface damage, high power laser light effect under easily generate damage and
It destroys.Although MRF can cut down the Microscale waveness of SPDT technologies generation, the micro-nanos such as iron powder can be generated in plane of crystal
The insertion 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 novel ultra-smooth of crisp deliquescent crystal, low damage, " soft polishing " technology of low defect are imperative.
Chemically mechanical polishing is a kind of surface polishing technique highly developed in semicon industry, it can realize work
Planarization in the full-scale range of part, there are technical advantages in terms of super-smooth surface is prepared.In chemically mechanical polishing, polishing
Liquid is one of core of entire technical matters, and physicochemical properties decide 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 library
The patent of liquid ", Patent No. CN00910010268.2, the patent select 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, can realize that the selectivity of plane of crystal uniformly removes.But due to water
Very big to the deliquescent effect intensity of KDP crystal, the removal rate of plane of crystal deliquescence microcell is uncontrollable during polishing, it is easy to
Surface generates small etch pit, and polishing removal fine degree is low.The method defect of deliquescence polishing principles based on microemulsion, mainly
It is attributed to：（1）Though water core size is Nano grade in W/O microemulsions, the deliquescent effect intensity of each water verification KDP crystal
It is uncontrollable, and during CMP, due to the participation of mechanism, the deliquescent effect that can further expand in microcell is strong
Degree eventually results in chemical machinery removal precision and is difficult to control, and removal rate can only be controlled in 100 nanometer level, KDP planes of crystal
Etch pit is easily generated, Precision Machining is difficult to realize.（2）Deliquescent effect forms KDP aqueous solutions on KDP quartz crystals surface, by
In KDP aqueous solutions in organic solvent（Oil phase）In solubility it is very low, inevitably KDP planes of crystal generate residual simultaneously
Recrystallization, leads to remained on surface KDP crystallites, influences surface quality.
It is entitled disclosed in Chinese patent literature library that " soft crisp deliquescent crystal chemically-mechanicapolish polishes anhydrous polishing without abrasive
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 adjusting agent and organic solvent composition avoids deliquescence polishing
Plane of crystal problems of crack.But the polishing fluid of composition mode is used, there are static corrosion effect, and to table during polishing
The poor selectivity in face site directly affects final quality of finish.It, must for the chemical etch polishing based on organic acid/base
Polishing fluid must further be reduced to the static corrosion of KDP crystal and improve the highly selective of polishing fluid.
From the above analysis, chemical Mechanical Polishing Technique is expected to realize in theory ultra-smooth, the ultra-clean of KDP crystal
Surface editing objective, but it is theoretical currently based on the theoretical chemical etch polishing with organic acid/base of deliquescence polishing of microemulsion
There is be difficult to overcome the problems, such as.
Invention content
The technical problems to be solved by the invention are to provide a kind of oily packet acidic ion liquid for KDP crystal and polish
Liquid.
The oily packet acidic ion liquid polishing fluid for KDP crystal of the present invention, its main feature is that：The polishing fluid each group
Point mass percent be：
Oil phase：25%~60%；
Disperse phase solvent：10%~15%；
Acidic ion liquid：5%~15%；
Surfactant：15%~45%；
Cosurfactant：5%~15%.
The oil phase be non-polar organic solvent, hexamethylene, n-hexane, glyceryl monooleate, olein or
One kind in tricaprylin.
The dispersion phase solvent is ethyl alcohol, isopropanol or 1- hexyl -3- methylimidazole hexafluorophosphates（[Hmim]PF6）
In one kind.
The 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.
The surfactant is in nonylphenol polyoxyethylene ether, alkyl polyoxyethylene ether or fatty alcohol polyoxyethylene ether
One kind.
The cosurfactant is one kind in n-butanol, n-amyl alcohol, n-hexyl alcohol or n-octyl alcohol.
The preparation environment temperature of the polishing fluid is 20 DEG C ~ 25 DEG C, and relative humidity is 30% ~ 50%, and air pressure is normal pressure.
The polishing fluid of the present invention is oily packet acidic ion liquid microemulsion, considered KDP crystal response characteristic and
The characteristics of chemical Mechanical Polishing Technique, overcomes current KDP crystal deliquescence polishing water-in-oil microemulsion and organic acid/alkalization
The defects of etch polishing liquid and deficiency, while had both highly selective and organic acid/caustic corrosion polishing of microemulsion deliquescence polishing
Complete anhydrous feature, be a kind of more advanced polishing fluid.The present invention by being coated to active constituent acidic ion liquid,
And the multi- scenarios method mechanism of chemically mechanical polishing is combined, with Chemical Kinetics control is basic point of departure on interface, to acid
Property the release of ionic liquid, interface interaction form and Chemical Kinetics carry out interface regulation and control, react the removal in microcell
KDP can be realized by the organic solvent to match in more controllable precise, the remaining organic solution of KDP planes of crystal after polishing
Plane of crystal cleans, and secondary damage will not be caused to KDP planes of crystal, finally realizes the point-by-point controllable removal of KDP crystal.
Specific embodiment
With reference to embodiment, the present invention will be described in detail.
The oily packet acidic ion liquid polishing fluid for KDP crystal of the present invention, the mass percent of each component are：
Oil phase：25%~60%；
Disperse phase solvent：10%~15%；
Acidic ion liquid：5%~15%；
Surfactant：15%~45%；
Cosurfactant：5%~15%.
The oil phase be non-polar organic solvent, hexamethylene, n-hexane, glyceryl monooleate, olein or
One kind in tricaprylin.
The dispersion phase solvent is ethyl alcohol, isopropanol or 1- hexyl -3- methylimidazole hexafluorophosphates（[Hmim]PF6）
In one kind.
The 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.
The surfactant is in nonylphenol polyoxyethylene ether, alkyl polyoxyethylene ether or fatty alcohol polyoxyethylene ether
One kind.
The cosurfactant is one kind of n-butanol, n-amyl alcohol, n-hexyl alcohol or n-octyl alcohol.
The preparation environment temperature of the polishing fluid is 20 DEG C ~ 25 DEG C, and relative humidity is 30% ~ 50%, and air pressure is normal pressure.
The polishing fluid of the present invention is oily packet acidic ion liquid microemulsion, with oil phase, acidic ion liquid, surfactant
Quasi- ternary phase diagrams with cosurfactant is technological means, is drawn by phasor, obtains the single-phase of oily packet acidic ion liquid
Micro-emulsion region.In the polishing fluid of Monophase microemulsion area screening different ratio, throw machine light using chemical machinery and realize 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：Using the KDP crystal of the mm of 35 mm of single-point diamond fly-cutting × 35 as polished crystalline substance
Body；
（2）The preparation of oily packet acidic ion liquid microemulsion：Oil phase is hexamethylene, and dispersion phase solvent is isopropanol, acid
Ionic liquid is bis-trifluoromethylsulfoandimide（TFSI）, surfactant is Triton X-100（Triton X-
100）, cosurfactant is n-octyl alcohol；During preparation, TFSI is uniformly mixed with isopropanol, be added dropwise to n-hexane,
In the mixed solution of Triton X-100 and n-octyl alcohol, wherein the mass percent of each component is 45:10:5:32:8, the micro emulsion
Liquid is labeled as A polishing fluids；
（3）Chemically mechanical polishing experiment：Using chemical-mechanical polishing mathing, the polishing experiments of KDP crystal are carried out, wherein A is thrown
The rate of addition of light liquid is 10 ml/min, and polish pressure is 2.5 KPa, 60 rpm of master rotating speed, and it is 60 to hold object ring rotating speed
Rpm, 10 min of polishing time.
（4）It is cleaned after polishing：Successively using isopropanol, n-hexane as cleaning solution, after mega sonic wave is assisted to be polished
Then cleaning is 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：Using the KDP crystal of the mm of 35 mm of single-point diamond fly-cutting × 35 as polished crystalline substance
Body；
（2）The preparation of oily packet acidic ion liquid microemulsion：Oil phase is hexamethylene, and dispersion phase solvent is [Hmim] PF6, acid
Property ionic liquid be caprolactam phosphate（[NHCH]H2PO4）, surfactant is Triton X-100（Triton
X-100）, cosurfactant is n-hexyl alcohol；During preparation, caprolactam phosphate with ethyl alcohol is uniformly mixed, is added dropwise to
In the mixed solution of hexamethylene, Triton X-100 and n-hexyl alcohol, wherein the mass percent of each component is 50:10:
5:30:5, which is labeled as B polishing fluids；
（3）Chemically mechanical polishing experiment：Using chemical-mechanical polishing mathing, the polishing experiments of KDP crystal are carried out, wherein B is thrown
The rate of addition of light liquid is 10 ml/min, and polish pressure is 2.5 KPa, 60 rpm of master rotating speed, and it is 60 to hold object ring rotating speed
Rpm, 10 min of polishing time.
（4）It is cleaned after polishing：Successively using isopropanol, n-hexane as cleaning solution, after mega sonic wave is assisted to be polished
Then cleaning is dried up with clean dried gas.
Under the polishing condition, after polishing and completing cleaning, the surface roughness of sample is 2.18 nm.
The embodiment of remaining embodiment and embodiment 1 and embodiment 2 is essentially identical, and the main distinction is matching for microemulsion
Fang Butong；In polishing process, polishing fluid rate of addition, master rotating speed, is held object ring rotating speed and is remained unchanged polish pressure.Specifically
Embodiment experimental result be summarised in table 1.
1. IL/O polishing fluids of table form and polishing experiments acetonideexample
| Embodiment | Oil phase | Disperse 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 | Ethyl alcohol | [NHCH]H2PO4 | Triton X-114 | N-hexyl alcohol | 50:15:5:24:6 | 2.18 |
| 7 | N-hexane | Ethyl alcohol | [NHCH]H2PO4 | Triton X-114 | N-hexyl alcohol | 45:20:5:24:6 | 2.23 |
| 8 | N-hexane | Ethyl alcohol | [NHCH]H2PO4 | Triton X-114 | N-hexyl alcohol | 35:30:5:24:6 | 2.47 |
| 9 | Glyceryl monooleate | [Hmim]PF6 | [DMFH]H2PO4 | Triton X-114 | N-butanol | 30:15:15:32:8 | 2.04 |
| 10 | Glyceryl monooleate | [Hmim]PF6 | [DMFH]H2PO4 | Triton X-114 | N-butanol | 30:20:10:32:8 | 1.82 |
| 11 | Glyceryl monooleate | [Hmim]PF6 | [DMFH]H2PO4 | Triton X-114 | N-butanol | 30:25:5:32:8 | 1.96 |
| 12 | Olein | Isopropanol | [Bmim]HSO4 | Triton X-100 | N-octyl alcohol | 30:10:5:45:10 | 2.29 |
| 13 | Olein | Isopropanol | [Bmim]HSO4 | Triton X-100 | N-octyl alcohol | 30:10:5:40:15 | 2.58 |
| 14 | Olein | Isopropanol | [Bmim]HSO4 | Triton X-100 | N-octyl alcohol | 30:10:5:35:20 | 2.87 |
| 15 | Tricaprylin | Ethyl alcohol | [Py]HSO4 | Triton X-100 | N-amyl alcohol | 60:5:5:24:6 | 3.15 |
| 16 | Tricaprylin | Ethyl alcohol | [Py]HSO4 | Triton X-100 | N-amyl alcohol | 40:15:5:32:8 | 2.72 |
| 17 | Tricaprylin | Ethyl alcohol | [Py]HSO4 | Triton X-100 | N-amyl alcohol | 35:20:5:32:8 | 2.31 |
The description for applying example above is more specific, detailed, but cannot should refer to therefore understands that for the limitation to this patent range
Go out, for those of ordinary skill in the art, without departing from the inventive concept of the premise, can also make several
Modification and improvement, these belong to protection scope of the present invention.
Claims (2)
1. a kind of oily packet acidic ion liquid polishing fluid for KDP crystal, it is characterised in that：The polishing fluid each component
Mass percent is：
Oil phase：25%~60%；
Disperse phase solvent：10%~15%；
Acidic ion liquid：5%~15%；
Surfactant：15%~45%；
Cosurfactant：5%~15%；
The oil phase is non-polar organic solvent, and hexamethylene, n-hexane, glyceryl monooleate, olein or three are pungent
One kind in acid glyceride；
The dispersion phase solvent is one kind in ethyl alcohol, isopropanol or 1- hexyl -3- methylimidazole hexafluorophosphates；
The acidic ion liquid is bis-trifluoromethylsulfoandimide, caprolactam phosphate, N, N '-dimethylformamide phosphoric acid
One kind in salt, 1- butyl -3- methylimidazolium hydrogen sulphates salt or pyridine disulfate；
The surfactant is one in nonylphenol polyoxyethylene ether, alkyl polyoxyethylene ether or fatty alcohol polyoxyethylene ether
Kind；
The cosurfactant is one kind in n-butanol, n-amyl alcohol, n-hexyl alcohol or n-octyl alcohol.
2. the oily packet acidic ion liquid polishing fluid according to claim 1 for KDP crystal, it is characterised in that：It is described
Polishing fluid preparation environment temperature for 20 DEG C ~ 25 DEG C, relative humidity is 30% ~ 50%, and air pressure is normal pressure.
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| 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 |
| CN110405543B (en) * | 2019-08-05 | 2020-08-04 | 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 |
| 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 |
| CN114561643B (en) * | 2022-03-16 | 2023-03-17 | 四川大学 | Chemical polishing solution for aluminum material and polishing method thereof |
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