CN111763478B - Chemical polishing solution for KDP crystal, preparation method and polishing method - Google Patents

Chemical polishing solution for KDP crystal, preparation method and polishing method Download PDF

Info

Publication number
CN111763478B
CN111763478B CN202010704951.2A CN202010704951A CN111763478B CN 111763478 B CN111763478 B CN 111763478B CN 202010704951 A CN202010704951 A CN 202010704951A CN 111763478 B CN111763478 B CN 111763478B
Authority
CN
China
Prior art keywords
polishing
solution
organic acid
kdp
surfactant
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010704951.2A
Other languages
Chinese (zh)
Other versions
CN111763478A (en
Inventor
董会
潘金龙
王英英
叶作彦
王利利
李晓媛
叶敏恒
秦代成
高伟
黄姝珂
王超
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Mechanical Manufacturing Technology of CAEP
Original Assignee
Institute of Mechanical Manufacturing Technology of CAEP
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Mechanical Manufacturing Technology of CAEP filed Critical Institute of Mechanical Manufacturing Technology of CAEP
Priority to CN202010704951.2A priority Critical patent/CN111763478B/en
Publication of CN111763478A publication Critical patent/CN111763478A/en
Application granted granted Critical
Publication of CN111763478B publication Critical patent/CN111763478B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The invention discloses a chemical polishing solution for KDP crystals, a preparation method and a polishing method. The polishing solution consists of vegetable oil, organic acid, ionic liquid, surfactant and cosurfactant, and is a novel completely anhydrous microemulsion. The polishing solution disclosed by the invention is simple in preparation method, stable in property and simple in use method, and can be used for uniformly and controllably removing the surface of a KDP crystal; the polishing solution is an organic solution completely free of solid particles, and after polishing, the surface of the KDP crystal can be cleaned by rinsing the surface of the KDP crystal by using a matched organic solvent, so that secondary damage to the surface of the KDP crystal cannot be caused. The novel chemical polishing solution and the polishing method thereof have the advantages of high-point selective removal characteristic of microemulsion and stress-free processing of chemical polishing, can improve the surface quality of KDP crystals, and do not introduce new stress damage.

Description

Chemical polishing solution for KDP crystal, preparation method and polishing method
Technical Field
The invention relates to the cross application field of functionalized microemulsion synthesis and ultra-precision machining, in particular to a chemical polishing solution for KDP crystals, a preparation method and a polishing method.
Background
Potassium dihydrogen phosphate (KDP) crystals are important optical elements (photoelectric switches and frequency doubling conversion devices) in inertial confinement nuclear fusion intense laser systems, and are recognized as optical materials which are extremely difficult to process due to the characteristics of softness, brittleness, deliquescence, sensitivity to temperature change, anisotropy and the like. The single-point diamond fly-cutting (SPDT) is the most main technical means of the KDP ultra-precision machining at present, due to the action of machining stress, the crystal lattice dislocation of the KDP surface can be caused, the single crystal structure is damaged, and a sub-surface damage layer is formed, so that the SPDT is an important reason for inducing the KDP crystal laser damage. Therefore, it is very important to explore the polishing and removing technology of the sub-surface damage layer of the KDP crystal after fly-cutting and improve the laser damage resistance of the KDP crystal.
Compared with the SPDT, the method has the advantages that the method becomes an important technical means for improving the laser damage resistance of the KDP crystal at present in order to effectively remove the sub-surface damage layer of the KDP crystal after fly-cutting. Magnetorheological polishing (MRF) and Chemical Mechanical Polishing (CMP) are currently the two leading polishing techniques. The MRF can effectively remove fly cutter lines and small-scale ripples and improve the surface shape precision, but the new subsurface damage caused by iron powder particle embedding and processing stress in the MRF restricts the further engineering application of the MRF. The CMP technology can effectively improve the surface roughness and remove fly-cutting knife lines; however, CMP is a process that takes advantage of processing stresses and still does not avoid the problem of sub-surface damage caused by forward pressure. More importantly, the polishing solution for polishing the KDP crystal is mainly aqueous polishing solution, and because the dissolution and recrystallization of the KDP crystal are reversible processes, the surface recrystallization cannot be avoided, and the formation of a smooth surface is not facilitated. Therefore, the research on novel water-free and stress-free KDP crystal surface polishing solution after fly-cutting and a corresponding polishing method thereof have important scientific research significance and engineering application value.
Chemical polishing is a classical stress-free surface polishing technology, is widely applied to surface processing of optical elements such as fused quartz and the like, and can effectively remove surface deposits, surface impurities and subsurface damage layers. The surface polishing is carried out in a chemical reaction mode, and the stress-free processing target of the surfaces of different materials can be realized theoretically. However, the conventional chemical polishing solution mainly adopts a dispersion form of a solution, which cannot accurately control the surface roughness and even deteriorates the surface roughness to different degrees. Therefore, special polishing liquid and polishing method need to be designed for processing surfaces with different materials and different roughness. However, no research report exists on a special polishing solution and a corresponding polishing method for KDP crystal chemical polishing at present.
Disclosure of Invention
The invention aims to solve the technical problem of providing a chemical polishing solution for KDP crystal, a preparation method and a polishing method, overcoming the defects and shortcomings of poor reaction controllability and no high-point selectivity of the traditional solution type polishing solution, realizing the controllability and the high-point selectivity of KDP crystal surface removal in a stress-free processing mode, and obtaining the KDP crystal with high surface quality.
The invention is realized by the following technical scheme:
in a first aspect, the invention provides a chemical polishing solution for KDP crystals, which is a functionalized microemulsion taking organic acid and ionic liquid as internal phases and consists of vegetable oil, organic acid, ionic liquid, surfactant and cosurfactant, wherein the components in percentage by mass are as follows:
vegetable oil: 20 to 65 percent;
surfactant (b): 36 to 56 percent;
cosurfactant: 9% -14%;
organic acid: 0.5 to 5 percent;
ionic liquid: 10% -25%;
the mass ratio of the surfactant to the cosurfactant is 4: 1;
the mass ratio range of the organic acid to the ionic liquid is as follows: 0.05 to 0.20.
The traditional chemical polishing solution mainly adopts a dispersion form of solution, so that the surface roughness cannot be accurately controlled, and even can be deteriorated to different degrees. Therefore, special polishing liquid and polishing method need to be designed for processing surfaces with different materials and different roughness. The invention designs a novel microemulsion of oil-packed organic acid-ionic liquid solution as the polishing solution of KDP crystal by comprehensively considering the chemical reaction characteristic of KDP crystal and the characteristics of chemical polishing technology. The polishing solution is a completely anhydrous chemical polishing solution, KDP crystal chemical polishing based on the polishing solution has surface high-point selectivity on the basis of stress-free processing, and is a more advanced polishing technology.
Specifically, the polishing solution is a functional microemulsion taking organic acid and ionic liquid as internal phases, and mainly comprises 20-60% of vegetable oil, 1-5% of organic acid, 10-30% of ionic liquid, 16-48% of surfactant and 4-12% of cosurfactant. The invention takes the chemical reaction kinetics control on a polishing interface as a basic starting point to coat the ionic liquid solution of the organic acid as an active ingredient, and because the micelle particles in the microemulsion are subjected to continuous Brownian motion and mutual collision, the ionic liquid solution of the organic acid is subjected to continuous mass transfer diffusion among different micelle particles. The special dispersion mode and mass transfer state of the organic acid solution in the microemulsion are utilized, and the advantage of a chemical polishing stress-free method is combined, so that the controllable chemical reaction of the KDP crystal surface high point is realized. The chemical polishing solution for the KDP crystal is a microemulsion which is completely anhydrous and particle-free, the microemulsion can uniformly remove the surface of the KDP crystal in a controllable manner in the polishing process, and the organic solution remained on the surface of the KDP crystal after polishing can be cleaned by rinsing with a matched organic solvent, so that the surface of the KDP crystal cannot be damaged secondarily.
Further, the vegetable oil is one of castor oil or epoxidized soybean oil.
Further, the surfactant is a nonionic surfactant polyethylene glycol octyl phenyl ether (TX-100).
Further, the cosurfactant is one of n-butyl alcohol or n-hexyl alcohol.
Further, the organic acid is bis (trifluoromethanesulfonimide) (TF)2NH)。
Further, the ionic liquid is 1-butyl-3-methylimidazole bistrifluoromethanesulfonylimide salt ([ Bmim)][TF2N]) 1-hexyl-3-methylimidazolium bistrifluoromethylsulfonyl imide salt ([ Hmim ]][TF2N]) Or 1-octyl-3-methylimidazolium bistrifluoromethylsulfonyl imide salt ([ Omim][TF2N]) One kind of (1).
Furthermore, the polishing solution is a novel anhydrous microemulsion and is suitable for chemical polishing of the KDP crystal surface after single-point diamond fly-cutting.
In a second aspect, the invention further provides a preparation method of the polishing solution, which comprises the following steps:
(1) adding organic acid with certain mass into the ionic liquid in a glove box, after the organic acid is fully dissolved, recording the obtained organic acid solution as a solution a, and taking out the solution a from the glove box for later use;
(2) fully mixing the surfactant and the cosurfactant according to the mass ratio of 4:1, and uniformly stirring to obtain a compound surfactant which is recorded as a solution b for later use;
(3) mixing the solution b and the vegetable oil according to a certain mass ratio, and fully and uniformly stirring at 200rpm to obtain a mixed solution, and recording the mixed solution as a solution c;
(4) dropwise adding a certain mass of the solution a into a ground triangular-conical flask filled with the solution c in the step (3), stirring at 200rpm for 2h (2 h), placing the triangular-conical flask in 37kHz ultrasonic waves for 30min, taking out, and standing for 12h (12 h) to obtain the anhydrous microemulsion type chemical polishing solution.
In a third aspect, the present invention also provides a polishing method of the polishing solution, including the steps of:
1) adding the chemical polishing solution for KDP crystal into a polytetrafluoroethylene polishing container;
2) after the KDP crystal is installed by a clamp, immersing the surface to be polished below the liquid level of the polishing solution, and carrying out chemical polishing;
3) the polishing environment temperature is 25 ℃, the relative humidity is 40%, the polishing liquid temperature is 25 ℃, and the polishing time is 10-90 minutes;
4) and sequentially rinsing the polished substrate by adopting absolute ethyl alcohol, isopropanol, acetone and normal hexane, blow-drying the surface by using high-purity nitrogen, and standing the substrate in a drying cabinet for 12 hours.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention takes the chemical reaction kinetics control on a polishing interface as a basic starting point to coat a novel KDP chemical active component (an organic acid ionic liquid solution), and the organic acid ionic liquid solution continuously carries out mass transfer diffusion among different micelle particles due to continuous Brownian motion and mutual collision among the micelle particles in the microemulsion. The special dispersion mode and mass transfer state of the organic acid solution in the microemulsion are utilized, and the advantage of a chemical polishing stress-free method is combined, so that the controllable chemical reaction of the KDP crystal surface high point is realized.
2. The invention comprehensively considers the reaction characteristic of KDP crystal and the characteristic of chemical polishing technology, designs a novel chemical polishing method of microemulsion based on organic acid-ionic liquid solution in oil, has high point selectivity on the basis of stress-free processing, and is a more advanced polishing technology.
3. The chemical polishing solution for the KDP crystal is a completely anhydrous and particle-free microemulsion, and the surface of the KDP crystal can be cleaned by rinsing the residual organic solution on the surface of the polished KDP crystal by adopting a matched organic solvent, so that secondary damage to the surface of the KDP crystal can be avoided.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that: it is not necessary to employ these specific details to practice the present invention. In other instances, well-known structures, circuits, materials, or methods have not been described in detail so as not to obscure the present invention.
Throughout the specification, reference to "one embodiment," "an embodiment," "one example," or "an example" means: the particular features, structures, or characteristics described in connection with the embodiment or example are included in at least one embodiment of the invention. Thus, the appearances of the phrases "one embodiment," "an embodiment," "one example" or "an example" in various places throughout this specification are not necessarily all referring to the same embodiment or example. Furthermore, the particular features, structures, or characteristics may be combined in any suitable combination and/or sub-combination in one or more embodiments or examples. Further, those of ordinary skill in the art will appreciate that the illustrations provided herein are for illustrative purposes and are not necessarily drawn to scale. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The present invention will be described in detail with reference to examples.
In a first aspect, the invention provides a chemical polishing solution for KDP crystals, which is a functionalized microemulsion taking organic acid and ionic liquid as internal phases and consists of vegetable oil, organic acid, ionic liquid, surfactant and cosurfactant, wherein the components in percentage by mass are as follows:
vegetable oil: 20 to 65 percent;
surfactant (b): 36 to 56 percent;
cosurfactant: 9% -14%;
organic acid: 0.5 to 5 percent;
ionic liquid: 10% -25%;
the mass ratio of the surfactant to the cosurfactant is 4: 1;
the mass ratio range of the organic acid to the ionic liquid is as follows: 0.05 to 0.20.
Further, the vegetable oil is one of castor oil or epoxidized soybean oil.
Further, the surfactant is a nonionic surfactant polyethylene glycol octyl phenyl ether (TX-100).
Further, the cosurfactant is one of n-butyl alcohol or n-hexyl alcohol.
Further, the organic acid is bis (trifluoromethanesulfonimide) (TF)2NH)。
Further, the ionic liquid is 1-butyl-3-methylimidazole bistrifluoromethanesulfonylimide salt ([ Bmim)][TF2N]) 1-hexyl-3-methylimidazolium bistrifluoromethylsulfonyl imide salt ([ Hmim ]][TF2N]) Or 1-octyl-3-methylimidazolium bistrifluoromethylsulfonyl imide salt ([ Omim][TF2N]) One kind of (1).
Furthermore, the polishing solution is a novel anhydrous microemulsion and is suitable for chemical polishing of the KDP crystal surface after single-point diamond fly-cutting.
The invention designs a novel microemulsion of oil-packed organic acid-ionic liquid solution by comprehensively considering the reaction characteristic of KDP crystal and the characteristic of chemical polishing technology. The chemical polishing solution is a completely anhydrous chemical polishing solution, KDP crystal chemical polishing based on the polishing solution has surface high-point selectivity on the basis of stress-free processing, and is a more advanced polishing technology. Specifically, the polishing solution is a functional microemulsion taking organic acid and ionic liquid as internal phases, and mainly comprises 20-60% of vegetable oil, 1-5% of organic acid, 10-30% of ionic liquid, 16-48% of surfactant and 4-12% of cosurfactant. The invention takes the chemical reaction kinetics control on a polishing interface as a basic starting point to coat the ionic liquid solution of the organic acid as an active ingredient, and because the micelle particles in the microemulsion are subjected to continuous Brownian motion and mutual collision, the ionic liquid solution of the organic acid is subjected to continuous mass transfer diffusion among different micelle particles. The special dispersion mode and mass transfer state of the organic acid solution in the microemulsion are utilized, and the advantage of a chemical polishing stress-free method is combined, so that the controllable chemical reaction of the KDP crystal surface high point is realized. The chemical polishing solution for the KDP crystal is a microemulsion which is completely anhydrous and particle-free, the microemulsion can uniformly remove the surface of the KDP crystal in a controllable manner in the polishing process, and the organic solution remained on the surface of the KDP crystal after polishing can be cleaned by rinsing with a matched organic solvent, so that the surface of the KDP crystal cannot be damaged secondarily.
In a second aspect, the invention further provides a preparation method of the polishing solution, which comprises the following steps:
(1) adding organic acid with certain mass into the ionic liquid in a glove box, after the organic acid is fully dissolved, recording the obtained organic acid solution as a solution a, and taking out the solution a from the glove box for later use;
(2) fully mixing the surfactant and the cosurfactant according to the mass ratio of 4:1, and uniformly stirring to obtain a compound surfactant which is recorded as a solution b for later use;
(3) mixing the solution b and the vegetable oil according to a certain mass ratio, and fully and uniformly stirring at 200rpm to obtain a mixed solution, and recording the mixed solution as a solution c;
(4) dropwise adding a certain mass of the solution a into a ground triangular-conical flask filled with the solution c in the step (3), stirring at 200rpm for 2h (2 h), placing the triangular-conical flask in 37kHz ultrasonic waves for 30min, taking out, and standing for 12h (12 h) to obtain the anhydrous microemulsion type chemical polishing solution.
In a third aspect, the present invention also provides a polishing method of the polishing solution, including the steps of:
1) adding the chemical polishing solution for KDP crystal into a polytetrafluoroethylene polishing container;
2) after the KDP crystal is installed by a clamp, immersing the surface to be polished below the liquid level of the polishing solution, and carrying out chemical polishing;
3) the polishing environment temperature is 25 ℃, the relative humidity is 40%, the polishing liquid temperature is 25 ℃, and the polishing time is 10-90 minutes;
4) and sequentially rinsing the polished substrate by adopting absolute ethyl alcohol, isopropanol, acetone and normal hexane, blow-drying the surface by using high-purity nitrogen, and standing the substrate in a drying cabinet for 12 hours.
The preparation of the polishing solution is characterized in that a quasi-ternary phase diagram of vegetable oil, organic acid, ionic liquid, surfactant and cosurfactant is taken as a technical means, and a single-phase microemulsion area of the vegetable oil-in-organic acid and the ionic liquid is obtained by drawing a phase diagram. And (4) screening polishing solutions with different proportions in a micro-emulsion area, and performing surface processing by using a self-made chemical polishing device.
Example 1
This example was carried out as follows:
(1) obtaining of initial surface: KDP crystal of 60mm multiplied by 8mm obtained by single point diamond fly cutting is used as crystal to be polished, and surface roughness Ra measured by a white light interferometer is 5.2.
(2) Preparing the microemulsion of the vegetable oil-in-organic acid and the ionic liquid: the vegetable oil is castor oil; the surfactant is polyethylene glycol octyl phenyl ether (TX-100), and the cosurfactant is n-hexanol; the organic acid is bis (trifluoromethanesulfonimide) (TF)2NH), the ionic liquid is [ Bmim ]]TF2N。
(3) Taking 56.0g of TX-100 and 14.0g of n-hexanol, stirring uniformly at a low speed of 200rpm, and fully mixing and stirring uniformly the mixture with 120.0g of castor oil to obtain a mixed solution for later use.
(4) In a glove box, 0.1g TF2NH was added to 9.9g [ Bmim ]]TF2And N, after uniform mixing, taking out the mixture from a glove box, dropwise adding the mixture into the mixed solution obtained in the step (3), stirring the mixture at 200rpm for 2 hours (2 hours), then placing the mixture in ultrasonic waves of 37kHz for 30 minutes, taking out the mixture, and standing the mixture for 12 hours (12 hours) to obtain castor oil: (TX-100+ n-hexanol): (TF)2NH+[Bmim]TF2N) ratio of 60 (28:7) to (0.05: 4.95) of the microemulsion of (1).
(5) Chemical polishing experiment: putting the polishing solution into a self-made polishing device, putting a magnetic stirrer, and keeping the rotating speed of 150 rpm; after the KDP crystal is mounted by a clamp, the surface to be polished is immersed into polishing solution, a cover is covered, and polishing treatment is carried out for 30min at the temperature of 20 ℃ and in the environment with the relative humidity not more than 40%.
(6) Cleaning after polishing: absolute ethyl alcohol, isopropanol and normal hexane are sequentially adopted as cleaning liquids, megasonic is used for assisting in cleaning after polishing, then clean, dry and high-purity nitrogen is used for blow-drying, and finally the polished glass is placed in a drying cabinet to stand for 12 hours (12 hours).
Under the polishing condition, after polishing and cleaning, the surface roughness of the sample is characterized by adopting a white light interferometer, and the surface roughness Ra is 3.6 nm.
Example 2
This example was carried out as follows:
(1) obtaining of initial surface: KDP crystal of 60mm multiplied by 8mm obtained by single-point diamond fly cutting is used as crystal to be polished, and surface roughness Ra measured by a white light interferometer is 7.2 nm.
(2) Preparing the microemulsion of the vegetable oil-in-organic acid and the ionic liquid: the vegetable oil is epoxidized soybean oil; the surfactant is polyethylene glycol octyl phenyl ether (TX-100), and the cosurfactant is n-butanol; the organic acid is bis (trifluoromethanesulfonimide) (TF)2NH), the ionic liquid is [ Bmim ]]TF2N。
(3) Taking 56.0g of TX-100 and 14.0g of n-butanol, stirring uniformly at a low speed of 200rpm, and fully mixing and stirring uniformly the mixture with 120.0g of epoxidized soybean oil to obtain a mixed solution for later use.
(4) In a glove box, 0.1g TF2NH was added to 9.9g [ Bmim ]]TF2And N, after uniformly mixing, taking out the mixture from a glove box, dropwise adding the mixture into the mixed solution obtained in the step (3), stirring the mixture at 200rpm for 2 hours, then placing the mixture in ultrasonic waves of 37kHz for 30 minutes, taking out the mixture and standing the mixture for 12 hours to obtain epoxidized soybean oil: (TX-100+ n-butanol): (TF)2NH+[Bmim]TF2N) ratio of 60 (28:7) to (0.05: 4.95) of the microemulsion of (1).
(5) Chemical polishing experiment: a self-made chemical polishing device is adopted, polishing solution is filled into the polishing device, a magnetic stirrer is placed, and the rotating speed of 150rpm is kept; after the KDP crystal is mounted by a clamp, the surface to be polished is immersed into polishing solution, a cover is covered, and polishing treatment is carried out for 30min at the temperature of 25 ℃ and in the environment with the relative humidity not more than 40%.
(6) Cleaning after polishing: absolute ethyl alcohol, isopropanol and normal hexane are sequentially adopted as cleaning liquids, megasonic is used for assisting in cleaning after polishing, and then clean and dry air is used for drying.
Under the polishing condition, after polishing and cleaning, the surface roughness of the sample is characterized by adopting a white light interferometer, and the surface roughness Ra is 4.7 nm.
This example is essentially the same as the embodiment of example 1, with the main difference being the formulation of the microemulsion; in the polishing process, the device, the polishing method and the environment temperature and humidity adopted by polishing are kept unchanged.
Other experimental results are summarized in tables 1 to 4.
TABLE 1 polishing solution composition and results of polishing experiments examples 3-8 (Castor oil System)
Figure BDA0002594381340000071
TABLE 2 polishing compositions and results of polishing experiments examples 9-16 (epoxidized soybean oil system)
Figure BDA0002594381340000081
TABLE 3 composition of different Ionic liquid polishing solutions and results of polishing experiments examples 17-19 (Castor oil System)
Figure BDA0002594381340000082
TABLE 4 composition of different ionic liquid polishing solutions and results of polishing experiments examples 20-22 (epoxidized soybean oil system)
Figure BDA0002594381340000083
Therefore, the polishing solution is a novel completely anhydrous microemulsion, and under the combined action of the surfactant and the cosurfactant, the ionic liquid solution of the organic acid with KDP chemical reaction activity is coated in the vegetable oil as a disperse phase. When the microemulsion is used for chemically polishing the surface of the KDP crystal, the stress-free controllable chemical reaction removal of the surface of the KDP crystal can be realized. The chemical polishing solution for KDP crystal has simple preparation method and use method and stable property, comprehensively considers the reaction characteristic of the KDP crystal and the technical advantage of chemical polishing, not only has the characteristic of microemulsion high-point selective chemical reaction, but also is compatible with the technical advantage of stress-free processing of chemical polishing, and can improve the surface quality of the KDP crystal without introducing new stress damage.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (6)

1. The chemical polishing solution for KDP crystals is a functionalized microemulsion taking organic acid and ionic liquid as internal phases, and is composed of vegetable oil, organic acid, ionic liquid, surfactant and cosurfactant, and the mass percentages of the components are as follows:
vegetable oil: 20 to 65 percent;
surfactant (b): 36 to 56 percent;
cosurfactant: 9% -14%;
organic acid: 0.5 to 5 percent;
ionic liquid: 10% -25%;
the mass ratio of the surfactant to the cosurfactant is 4: 1;
the mass ratio range of the organic acid to the ionic liquid is as follows: 0.05 to 0.20;
the vegetable oil is one of castor oil or epoxidized soybean oil;
the organic acid is bis (trifluoromethanesulfonimide);
the ionic liquid is one of 1-butyl-3-methylimidazole bistrifluoromethylsulfonyl imide salt, 1-hexyl-3-methylimidazole bistrifluoromethylsulfonyl imide salt or 1-octyl-3-methylimidazole bistrifluoromethylsulfonyl imide salt.
2. The chemical polishing solution for KDP crystals according to claim 1, characterized in that the surfactant is a nonionic surfactant polyethylene glycol octyl phenyl ether.
3. The chemical polishing solution for KDP crystals according to claim 1, wherein the co-surfactant is one of n-butanol or n-hexanol.
4. The chemical polishing solution for KDP crystal as claimed in claim 1, wherein the polishing solution is a novel anhydrous microemulsion suitable for chemical polishing of KDP crystal surface after single point diamond fly-cutting.
5. A method for preparing the polishing liquid according to any one of claims 1 to 4, comprising the steps of:
(1) adding organic acid with certain mass into the ionic liquid in a glove box, after the organic acid is fully dissolved, recording the obtained organic acid solution as a solution a, and taking out the solution a from the glove box for later use;
(2) fully mixing the surfactant and the cosurfactant according to the mass ratio of 4:1, and uniformly stirring to obtain a compound surfactant which is recorded as a solution b for later use;
(3) mixing the solution b and the vegetable oil according to a certain mass ratio, and fully and uniformly stirring at 200rpm to obtain a mixed solution, and recording the mixed solution as a solution c;
(4) dropwise adding a certain mass of the solution a into a ground triangular-conical flask filled with the solution c in the step (3), stirring at 200rpm for 2h, placing the triangular-conical flask in 37kHz ultrasonic waves for 30min, taking out, and standing for 12h to obtain the anhydrous microemulsion type chemical polishing solution.
6. A polishing method using the polishing liquid according to any one of claims 1 to 4, comprising the steps of:
1) adding the chemical polishing solution for KDP crystal into a polytetrafluoroethylene polishing container;
2) after the KDP crystal is installed by a clamp, immersing the surface to be polished below the liquid level of the polishing solution, and carrying out chemical polishing;
3) the polishing environment temperature is 25 ℃, the relative humidity is 40%, the polishing liquid temperature is 25 ℃, and the polishing time is 10-90 minutes;
4) and sequentially rinsing the polished substrate by adopting absolute ethyl alcohol, isopropanol, acetone and normal hexane, blow-drying the surface by using high-purity nitrogen, and standing the substrate in a drying cabinet for 12 hours.
CN202010704951.2A 2020-07-21 2020-07-21 Chemical polishing solution for KDP crystal, preparation method and polishing method Active CN111763478B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010704951.2A CN111763478B (en) 2020-07-21 2020-07-21 Chemical polishing solution for KDP crystal, preparation method and polishing method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010704951.2A CN111763478B (en) 2020-07-21 2020-07-21 Chemical polishing solution for KDP crystal, preparation method and polishing method

Publications (2)

Publication Number Publication Date
CN111763478A CN111763478A (en) 2020-10-13
CN111763478B true CN111763478B (en) 2021-11-02

Family

ID=72726821

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010704951.2A Active CN111763478B (en) 2020-07-21 2020-07-21 Chemical polishing solution for KDP crystal, preparation method and polishing method

Country Status (1)

Country Link
CN (1) CN111763478B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114561643B (en) * 2022-03-16 2023-03-17 四川大学 Chemical polishing solution for aluminum material and polishing method thereof
CN115157110B (en) * 2022-09-02 2022-12-13 江苏先进无机材料研究院 Method for improving surface quality of cesium iodide flexible crystal

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103242934A (en) * 2013-04-02 2013-08-14 华南理工大学 Ionic liquid/vegetable oil microemulsion type biological lubricant base oil and preparation method thereof
CN103937587A (en) * 2014-04-28 2014-07-23 华南理工大学 Vegetable oil based ionic liquid microemulsion type nano lubricating oil and preparation method thereof
CN106519989A (en) * 2017-01-09 2017-03-22 中国工程物理研究院机械制造工艺研究所 Polishing solution used for KDP crystal
CN106811135A (en) * 2017-01-11 2017-06-09 中国工程物理研究院机械制造工艺研究所 A kind of oily bag acidic ion liquid polishing fluid for KDP crystal
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103242934A (en) * 2013-04-02 2013-08-14 华南理工大学 Ionic liquid/vegetable oil microemulsion type biological lubricant base oil and preparation method thereof
CN103937587A (en) * 2014-04-28 2014-07-23 华南理工大学 Vegetable oil based ionic liquid microemulsion type nano lubricating oil and preparation method thereof
CN106519989A (en) * 2017-01-09 2017-03-22 中国工程物理研究院机械制造工艺研究所 Polishing solution used for KDP crystal
CN106811135A (en) * 2017-01-11 2017-06-09 中国工程物理研究院机械制造工艺研究所 A kind of oily bag acidic ion liquid polishing fluid for KDP crystal
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
高伟.KDP晶体的无磨料射流去除机理及受质层减缓研究.《工程科技I辑》.2020, *

Also Published As

Publication number Publication date
CN111763478A (en) 2020-10-13

Similar Documents

Publication Publication Date Title
CN111763478B (en) Chemical polishing solution for KDP crystal, preparation method and polishing method
Ohnishi et al. A-site layer terminated perovskite substrate: NdGaO 3
US6343976B1 (en) Abrasive, method of polishing wafer, and method of producing semiconductor device
CN102179390B (en) Method for cleaning ultra-smooth surface
CN103333748B (en) Silicon wafer cleaning fluid, preparation method and use thereof and silicon wafer cleaning method
EP3193356B1 (en) Cleaning method and laminate of aluminum nitride single-crystal substrate
US20060288929A1 (en) Polar surface preparation of nitride substrates
Zhou et al. Flux pinning properties of Gd–Ba–Cu–O trapped field magnets grown by a modified top-seeded melt growth
JPH01197396A (en) Epitaxial structure of superconductor
Zhai et al. The processing and properties of single grain Y–Ba–Cu–O fabricated from graded precursor powders
CN110295011B (en) Polishing solution for KDP crystal and preparation method and application thereof
CN110114518A (en) GaAs substrate and its manufacturing method
TW201938623A (en) Composition for semiconductor process and semiconductor process
Bhakay-Tamhane et al. Kinetics and symmetry changes in low-temperature phase transitions in LiKSO4
JPH0442893A (en) Silicon wafer
Auvray et al. X-ray diffraction and freeze-fracture electron microscopy study of the cubic phase in the cetylpyridinium chloride/formamide and cetyltrimethylammonium chloride/formamide systems
Leontiou et al. Suppression of intermixing in strain-relaxed epitaxial layers
Le Bellac et al. Mechanism of the incommensurate phase in lead oxide α-PbO
Levinstein et al. Calcium tungstate. II. Observation of dislocations
US4396459A (en) Method and solution for etching indium antimonide
Tomashyk et al. Optimization of conditions for treatment of ZnSe crystal surfaces by chemical etching
Xian et al. Optimization and Mechanism of SiO2-Based Slurry Components for Atomically Smooth Gallium Nitride Surface Obtained Using Chemical Mechanical Polishing Technique
CN115537915B (en) Method for reusing garnet substrate in single crystal epitaxial growth
Jee et al. Dissolution and resolidification of SmBa/sub 2/Cu/sub 3/O/sub 7-y/seed during top seeded melt texturing of YBa/sub 2/Cu/sub 3/O/sub 7-y
JP4348539B2 (en) Nonmagnetic garnet substrate manufacturing method, nonmagnetic garnet substrate, and bismuth-substituted magnetic garnet film obtained using the substrate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant