CN110295011A - A kind of polishing fluid for KDP crystal and preparation method thereof, application - Google Patents
A kind of polishing fluid for KDP crystal and preparation method thereof, application Download PDFInfo
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- CN110295011A CN110295011A CN201910645289.5A CN201910645289A CN110295011A CN 110295011 A CN110295011 A CN 110295011A CN 201910645289 A CN201910645289 A CN 201910645289A CN 110295011 A CN110295011 A CN 110295011A
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- polishing fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
- B24B57/02—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents
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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
- C09G1/04—Aqueous dispersions
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention discloses a kind of polishing fluid for KDP crystal and preparation method thereof, application, the polishing fluid is made of following volumes percent composition: polarity phase: 1~10%；Nonpolar phase: 30%~55%；Surplus is solvent pairs phase.Polishing liquid and preparation method thereof of the invention is simple, property is stablized, effectively removing for fly-cutting knife mark can be realized in (1~2.5kPa) under lower polish pressure, the problems such as higher polish pressure may bring sub-surface damage is avoided, and surface of polished roughness obtains a degree of improvement.Polishing fluid ingredient is common organic reagent and does not chemically react with KDP, polishing fluid does not use amphiphilic surfactant, it only needs to carry out simple surface washing using one of the component of polishing fluid (solvent pairs phase) after polishing, surface cleaning can be realized, any impurity residual will not be generated on surface.
Description
Technical field
The present invention relates to Ultra-precision Turning microemulsion polishing fluid technical fields, and in particular to a kind of throwing for KDP crystal
Light liquid and preparation method thereof, application.
Background technique
Potassium dihydrogen phosphate (KDP) crystal is a kind of very good nonlinear optical element, is currently the only can be used for
The nonlinear optical material of the laser freuqency doublings of the light path systems such as ICF, light laser weapon, Electro-optical Modulation and photoelectric switching device.Work
It is high to the surface quality requirements of KDP crystal in Cheng Yingyong, as ultra-smooth, free of surface defects, unstressed remaining and free from admixture are residual
It stays, the limit of intimate material processing.However KDP crystalline material itself have it is soft it is crisp, it is easy deliquesce, it is sensitive to temperature change and
The features such as anisotropy, so that processing KDP crystal has extremely strong challenge.Single-point diamond fly-cutting (SPDT) technology is at present
It uniquely can satisfy the KDP crystals for ultra-precision processing technology of engineering application requirement, LLNL National Laboratory, the U.S. and China Ha Er
The units such as shore polytechnical university have made certain gains in the field.Although lower rough surface can be obtained using SPDT technology
Degree, but periodical Microscale waveness (fly-cutting knife mark) and sub-surface damage can be generated in plane of crystal, make in high power laser light
Damage and destruction are easy to produce under.Therefore, the surface Research on Post-processing Techniques of KDP crystal has important grind after development fly-cutting
Study carefully value and application prospect.
Chemically mechanical polishing is a kind of surface polishing technique highly developed in semicon industry, it can be realized work
Planarization in the full-scale range of part, there are technical advantages in terms of preparing super-smooth surface.In chemically mechanical polishing, polishing
Liquid is one of the core of entire technical matters, and physicochemical properties directly affect the precision level of chemically mechanical polishing, if
Traditional polishing fluid is selected, will cause the atomization of KDP plane of crystal or damage.Therefore, design is suitble to soft crisp, deliquescent crystal special
It is the basis for carrying out the mechanical polishing of KDP crystal chemistry with polishing fluid.
Summary of the invention
The purpose of the present invention is to provide a kind of polishing fluid for KDP crystal, it can not only realize that traditional Water-In-Oil is micro-
Lotion deliquesces the effect of polishing, simultaneously as being free of surfactant, can be effectively prevented from after polishing due to surfactant
Remain bring surface aggravation deliquescence and secondary pollution.
Moreover, it relates to the preparation method and application of above-mentioned polishing fluid.
The present invention is achieved through the following technical solutions:
A kind of polishing fluid for KDP crystal, the polishing fluid are made of following volumes percent composition:
Polarity phase: 1~10%；
Nonpolar phase: 30%~55%；
Surplus is solvent pairs phase.
" 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 oily 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, when passing through polishing polishing pad with
The removal of plane of crystal is realized in rubbing action between crystal.
Through applicant study in find, using water-in-oil microemulsion containing surfactant as polishing fluid, surface of polished
Activating agent is easily adhered to plane of crystal, clean it is relatively difficult, it is amphipathic due to surfactant, KDP table can be further exacerbated by
The deliquescence in face deteriorates surface quality.
Therefore, applicant carries out experimental study to the component of polishing fluid, under the premise of being free of surfactant, sets again
The formula of polishing fluid is counted, applicant is had found by long-term experiment:
It mutually combines specific polarity phase, nonpolar phase and solvent pairs according to a certain percentage, similar oil packet can be formed
The monodisperse system of water microemulsion.Water can still exist in the form of nanosized liquid droplets in the polishing fluid of the type, and due to not
It is applicable in traditional surfactant, the interfacial film in the microemulsion between polarity phase and nonpolar phase is easier to deform or be destroyed,
Therefore we (1~2.5kPa) effectively removing for fly-cutting knife mark can be realized under lower polish pressure, avoid compared with
The problems such as high polish pressure possible sub-surface damage, surface of polished roughness obtains a degree of improvement.
The present invention differs not the improvement degree of surface of polished roughness compared with the polishing fluid containing surfactant
Greatly, and the degree of scatter of polishing fluid can equally reach nanoscale (polishing fluid is complete agranular type polishing fluid), but due to this
Invention be free of surfactant, only with short chain alcohol as solvent pairs phase, not will lead to polishing fluid be attached to KDP plane of crystal with
And cause KDP crystal to deliquesce, and polishing fluid ingredient is common organic reagent, it is anti-that with KDP crystal chemistry will not occur for polishing fluid
It answers, only needs to carry out simple surface washing using one of the component of polishing fluid (solvent pairs phase) after polishing, surface can be realized
Cleaning will not generate any impurity residual on surface, not will lead to secondary damage and secondary pollution.Apparently, the application
KDP plane of crystal has glossiness after polishing, and since there are apparent tables after the polishing of the polishing fluid containing surfactant
Face activating agent residual, the decline of KDP plane of crystal glossiness.
Further, polarity Xiang Weishui or inorganic salt solution.
For the difference according to initial roughness, controlled material removal rate.
Further, nonpolar phase is one of n-hexane, hexamethylene, terpane, isoamyl alkyl acetates.
Further, solvent pairs is mutually one of ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol.
A kind of preparation method of such as polishing fluid, comprising the following steps:
1), nonpolar phase is mutually pressed with solvent pairs to certain volume ratio mixing, stir evenly to form mixed solvent；
2) polarity phase, is added dropwise according to volume ratio in the mixed solvent, stands obtain polishing fluid after mixing evenly.
Preparation method step of the present invention is simple, easy to operate, and property is stablized, and the polishing fluid of preparation is in lower throwing
Effectively removing for fly-cutting knife mark can be realized in (1~2.5kPa) under light pressure, and Asia may be brought by avoiding higher polish pressure
The problems such as surface damage.
Further, the preparation environment temperature of polishing fluid is 20 DEG C~35 DEG C, and relative humidity is 30%~50%, and air pressure is
Normal pressure.
A kind of application of such as polishing fluid, the polishing fluid is for soft crisp deliquescent crystal surface polishings such as KDP crystal.
Further, the concrete application process of the polishing fluid:
Plane of crystal is polished using precision polishing machine, the polishing fluid is used in polishing process, after polishing, directly
It uses the solvent pairs phase reagent in polishing fluid to rinse polishing sample surfaces as cleaning solution, is then dried up with clean dried gas.
Compared with prior art, the present invention having the following advantages and benefits:
1, the present invention is designed as basic point of departure with the polishing fluid of surfactant-free class microemulsion, has developed better than tradition
The novel polishing liquid system of water-in-oil microemulsion can realize the throwing for deliquescing polishing removal fly-cutting knife mark under lower polish pressure
Light effect, and avoid using traditional amphiphilic surfactant, surface of polished cleaning is more easier, and will not generate surface
Organic substance residues.
2, polishing fluid of the present invention is complete agranular type polishing fluid, and preparation is simple, property is stablized.During the polishing process
By the deliquescent effect of the polishing fluid, controlled etching can be realized, KDP plane of crystal residue is simple organic molten after polishing
Agent will not be chemically reacted with KDP crystal, can easily realize KDP by using the solvent pairs phase organic solvent of response
Plane of crystal cleaning, will not cause secondary damage to KDP plane of crystal.
Detailed description of the invention
Attached drawing described herein is used to provide to further understand the embodiment of the present invention, constitutes one of the application
Point, do not constitute the restriction to the embodiment of the present invention.In the accompanying drawings:
Fig. 1 is using the KDP plane of crystal electron-microscope scanning figure after the polishing of tradition W/O microemulsion；
Fig. 2 is using the KDP plane of crystal electricity for impregnating primary (10min) after the polishing of tradition W/O microemulsion using isopropanol
Scarnning mirror figure；
Fig. 3 be using after the polishing of tradition W/O microemulsion using impregnating in isopropanol after (10min/ times, 3 times) three times in preventing
KDP plane of crystal electron-microscope scanning figure after placing 2 weeks in damp cabinet；
Fig. 4 is the KDP plane of crystal electron-microscope scanning figure after the class microemulsion polishing using surfactant-free；
Fig. 5 is brilliant using the KDP of isopropanol immersion primary (10min) after being polished using the class microemulsion of surfactant-free
Body surface face electron-microscope scanning figure；
Fig. 6 be after the class microemulsion polishing using surfactant-free using impregnate in isopropanol three times (10min/ times, 3
It is secondary) after placed in moisture-resistant cabinet 2 weeks after KDP plane of crystal electron-microscope scanning figure.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below with reference to embodiment and attached drawing, to this
Invention is described in further detail, and exemplary embodiment of the invention and its explanation for explaining only the invention, are not made
For limitation of the invention.
Embodiment 1:
The polishing fluid of preparation is used for KDP polishing crystal, detailed process are as follows:
1), the acquisition of initial surface: using the KDP crystal of the Ф 50mm of single-point diamond fly-cutting as polished crystal, table
Surface roughness is 3.5nm；
2), prepared by polishing fluid: nonpolar phase (hexamethylene) is mixed according to certain volume ratio with solvent pairs phase (isopropanol)
It closes, after magnetic agitation is uniform, the polarity phase (water) of certain volume, final system cyclohexane, isopropyl is added dropwise in the mixed solvent
Alcohol, water volume ratio be 36:604, stand, seal up for safekeeping spare after mixing evenly；In order to compare polishing fluid of the present invention and traditional oils packet
The advantage of water microemulsion, we are with the oil that the ratio of oily phase (decyl alcohol), surfactant (TX-100) and water is that 36:60:4 is formed
Packet water microemulsion polishing fluid as a control group；
3), polishing experiments: the precise polished machine of PM6 is used, polishing fluid of the invention and traditional W/O microemulsion is respectively adopted
KDP crystal after two pieces of fly-cuttings is polished, polish pressure 2kPa, master revolving speed 60rpm, fixture revolving speed 60rpm, in the same direction
Rotation, polishing time 5min；
4) it is cleaned after, polishing: using solvent pairs phase (isopropanol) reagent as cleaning solution, rinsing sample surfaces after polishing, so
10min is impregnated in cleaning solution afterwards, is dried up with clean dried gas.
Under the polishing condition of the present embodiment, using the class microemulsion of surfactant-free of the invention as polishing fluid
When, the thickness removal rate of KDP crystal is 56nm/min, and after polishing and cleaning, the surface roughness of sample is 2.9nm.Using pair
When according to group W/O microemulsion as polishing fluid, the thickness removal rate of KDP crystal is 189nm/min, after polishing and cleaning, sample
Surface roughness is 3.2nm.
As shown in figs 1 to 6, using traditional containing surfactant W/O microemulsion polishing after, observed on surface compared with
More greasy dirt areas, after carrying out soaking and washing using demulsifier isopropanol, it is lesser liquid film that greasy dirt region is destroyed by isopropanol, after
Continuous soaking and washing drying and with (relative humidity 30%) in moisture-resistant cabinet, surface can gradually appear a large amount of solid fine grain, surface light
Brightness decline.
After the class microemulsion polishing of object surfactant of the invention, organic reagent shape is substantially not visible on surface
At greasy dirt area, using in isopropanol cleaning process, surface there is no significant change, will not generate in placement process solid
Body crystal grain.
Embodiment 2- embodiment 17 is obtained by orthogonal experiment:
Embodiment 2- embodiment 17 is based on embodiment 1, the difference from embodiment 1 is that:
Nonpolar phase, solvent phase are different with the volume ratio of polarity phase, and polish pressure is different.
The specific difference of embodiment 1- embodiment 17 and polishing effect are as shown in table 1: table 1
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (8)
1. a kind of polishing fluid for KDP crystal, which is characterized in that the polishing fluid is made of following volumes percent composition:
Polarity phase: 1~10%；
Nonpolar phase: 30%~55%；
Surplus is solvent pairs phase.
2. a kind of polishing fluid for KDP crystal according to claim 1, which is characterized in that the polarity Xiang Weishui or
Inorganic salt solution.
3. a kind of polishing fluid for KDP crystal according to claim 1, which is characterized in that the nonpolar phase is positive
One of hexane, hexamethylene, terpane, isoamyl alkyl acetates.
4. a kind of polishing fluid for KDP crystal according to claim 1, which is characterized in that the solvent pairs Xiang Weiyi
One of alcohol, normal propyl alcohol, isopropanol, n-butanol.
5. a kind of preparation method of the polishing fluid as described in claim any one of 1-4, which comprises the following steps:
1), nonpolar phase is mutually pressed with solvent pairs to certain volume ratio mixing, stir evenly to form mixed solvent；
2) polarity phase, is added dropwise according to volume ratio in the mixed solvent, stands obtain polishing fluid after mixing evenly.
6. the preparation method of polishing fluid according to claim 5, which is characterized in that the preparation environment temperature of the polishing fluid is
20 DEG C~35 DEG C, relative humidity is 30%~50%, and air pressure is normal pressure.
7. a kind of application of the polishing fluid as described in claim any one of 1-4, which is characterized in that the polishing fluid is for soft crisp easy
Deliquesce plane of crystal polishing.
8. the application of polishing fluid according to claim 7, which is characterized in that the concrete application process of the polishing fluid:
Plane of crystal is polished using precision polishing machine, the polishing fluid is used in polishing process, after polishing, directly with throwing
Solvent pairs phase reagent in light liquid rinses polishing sample surfaces as cleaning solution, is then dried up with clean dried gas.
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| CN201910645289.5A CN110295011B (en) | 2019-07-17 | 2019-07-17 | Polishing solution for KDP crystal and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112139859A (en) * | 2020-09-21 | 2020-12-29 | 大连理工大学 | Method for anhydrous polishing of KDP crystal |
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