CN110183972B - Acidic polishing solution and application thereof in obtaining YAG series materials with ultra-smooth surfaces - Google Patents
Acidic polishing solution and application thereof in obtaining YAG series materials with ultra-smooth surfaces Download PDFInfo
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- CN110183972B CN110183972B CN201910588392.0A CN201910588392A CN110183972B CN 110183972 B CN110183972 B CN 110183972B CN 201910588392 A CN201910588392 A CN 201910588392A CN 110183972 B CN110183972 B CN 110183972B
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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
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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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
Abstract
The invention discloses an acidic polishing solution and application thereof in obtaining YAG series materials with ultra-smooth surfaces, wherein the preparation of the acidic polishing solution comprises the following steps: concentrated sulfuric acid, glacial acetic acid, ammonium dichromate, phosphoric acid and water are mixed according to a mass ratio of 1: 1: 1: 0.8-1.2: 50, adding water to dilute the mixture until the pH value is 3-5 when the mixture is used, and polishing the surface of the YAG series material by using the acid polishing solution to obtain the YAG series material with an ultra-smooth surface.
Description
Technical Field
The invention relates to the technical field of crystal polishing, in particular to an acidic polishing solution and application thereof in obtaining a YAG series material with an ultra-smooth surface.
Background
The large-size YAG laser crystal is used as the most important optical element in a high-power laser system, and has the requirements of high-power-density operation and high beam quality, so that obtaining an ultra-smooth surface on the surface of the large-size YAG laser crystal is a necessary condition for realizing the high-power laser system.
In order to obtain an ultra-smooth surface, researchers at home and abroad have conducted a great deal of research on the surface of fused quartz by aiming at different polishing methods in recent decades, but the research on obtaining the ultra-smooth surface on the surface of YAG crystal is basically blank. In addition, various novel polishing methods generally have the problems of complex process, high processing cost, low polishing efficiency and the like, which cannot be adopted in large quantity.
The traditional processing mode has the following two problems:
(1) in the traditional processing method, because the surface of an element is directly contacted with a traditional polishing disk (a polyurethane polishing die and an asphalt polishing die), the surface of the processed element has the problems of large roughness and deep subsurface damage layer due to large friction in the polishing process;
(2) the upper disc mode of the traditional processing method is to directly bond the upper disc, and the problem of serious plane deformation of a large plane element is caused by large bonding tension.
Disclosure of Invention
The invention aims to provide an acidic polishing solution and application thereof in obtaining YAG series materials with an ultra-smooth surface, and solves the problems of complex process, low polishing efficiency and high polishing cost of the existing non-contact polishing technologies such as auxiliary chemical etching, ion beam polishing and the like.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides an acidic polishing solution, which is used for polishing the surface of YAG series materials and is prepared by the following method: concentrated sulfuric acid, glacial acetic acid, ammonium dichromate, phosphoric acid and water are mixed according to a mass ratio of 1: 1: 1: 0.8-1.2: 50 and mixing.
The invention provides a method for obtaining a YAG series material with an ultra-smooth surface, which comprises the following steps: the YAG series material is polished by the acid polishing solution,
preferably, the YAG family of materials is selected from YAG crystals or YAG crystal laths,
more preferably, the polishing is performed so that the surface roughness of the YAG crystal is controlled within 0.3nm,
more preferably, the polishing is performed so that the roughness on the large surface of the YAG crystal lath is controlled to be within 0.3nm and the flatness is controlled to be within 0.5 μm.
The invention has the beneficial effects that: the invention provides an acidic polishing solution and application thereof in obtaining a YAG series material with an ultra-smooth surface, wherein the acidic polishing solution is prepared according to the properties of the YAG series material, and on the basis of overcoming the defect that the stability of the polishing solution is reduced without adding a corrosion inhibitor, the acidic polishing solution prepared by adopting the components has the functions of corroding a crystal surface damage layer and improving the polishing efficiency, and has better lubricating and heat dissipation functions, so that the surface smoothness of the crystal can be further improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a graph showing a roughness test in comparative example 1 of the present invention;
FIG. 2 is a graph showing a roughness test in example 2 of the present invention;
FIG. 3 is a graph of roughness test in example 3 of the present invention;
FIG. 4 is a graph of roughness test in example 3 of the present invention;
FIG. 5 is a graph of roughness test in example 4 of the present invention;
FIG. 6 is a graph of roughness test in example 4 of the present invention;
FIG. 7 is a graph showing flatness test in example 4 of the present invention;
fig. 8 is a graph of flatness test in example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a specific description of an acidic polishing solution and its application in obtaining a YAG series material with an ultra-smooth surface provided by an embodiment of the present invention.
The embodiment of the invention provides an acidic polishing solution, which is prepared by the following steps: the acid polishing solution is used for polishing the surface of YAG series materials, and is prepared by the following steps: concentrated sulfuric acid, glacial acetic acid, ammonium dichromate, phosphoric acid and water are mixed according to a mass ratio of 1: 1: 1: 0.8-1.2: 50 and mixing.
The embodiment of the invention provides an acidic polishing solution, which is used for polishing the surface of YAG series materials, and the selection of various components in the preparation process of the acidic polishing solution is as follows: according to YAG series materials, the materials can be slightly dissolved in phosphoric acid at high temperature (more than 250 ℃), the reaction can be carried out at normal temperature under the condition of adding a catalyst ammonium dichromate, namely, the phosphoric acid and the ammonium dichromate can quickly react a ground surface loose layer and a sub-surface damaged layer, and the sub-surface damaged layer is removed while the polishing efficiency is improved; in addition, according to the hydrolysis characteristic of YAG series materials, the hydrolysis can be promoted in an acid environment to further improve the polishing efficiency, so that sulfuric acid with good chemical stability is selected to improve the acidity of the polishing solution; because ammonium dichromate is mixed with strong acid and has explosion risk, glacial acetic acid is used as a solvent to dissolve ammonium dichromate, and then phosphoric acid and sulfuric acid are added, and finally, water, preferably distilled water, is added.
According to the above explanation, phosphoric acid in the acidic polishing solution is critical, the polishing efficiency is low when the concentration of phosphoric acid is too low, the sub-damaged layer is not completely removed, and the surface quality is affected by excessive corrosion caused by too high concentration of phosphoric acid, so the phosphoric acid ratio is important and must be in the range of 0.8-1.2. Therefore, the acidic polishing solution overcomes the defects that the acidic slurry of the existing acidic polishing solution has high corrosivity and high requirement on polishing equipment, and the stability of the polishing solution is reduced by adding a corrosion inhibitor.
In some embodiments, the acidic polishing solution is diluted with water to a pH of 3 to 5, preferably, the water is selected from distilled water.
The embodiment of the invention provides a method for obtaining a YAG series material with an ultra-smooth surface, which comprises the following steps: the YAG series material is polished by the acid polishing solution,
preferably, the YAG family of materials is selected from YAG crystals or YAG crystal laths,
more preferably, the polishing is performed so that the surface roughness of the YAG crystal is controlled within 0.3nm,
more preferably, the polishing is performed so that the roughness on the large surface of the YAG crystal lath is controlled to be within 0.3nm and the flatness is controlled to be within 0.5 μm.
In some embodiments, the preparation of YAG crystal comprises the steps of:
respectively heating the dispensing disc and the YAG crystal, feeding the YAG crystal on the disc in a dispensing manner,
at least one surface of the YAG crystal is ground and polished,
and (4) heating the polished YAG crystal and the dispensing disc again, and taking down the YAG crystal from the dispensing disc.
In some embodiments, the preparation of the YAG crystal slab comprises the steps of:
respectively heating the dispensing disc and the YAG crystal lath, hanging the YAG crystal lath on the disc in a dispensing manner, grinding and polishing the first surface of the YAG crystal lath, controlling the flatness within 0.5 lambda @632.8nm, heating the polished YAG crystal lath again, taking the YAG crystal lath off the dispensing disc,
cleaning a YAG crystal lath, then hanging the plate in a light adhesive mode, coating waterproof paint, grinding a second surface of the YAG crystal lath by using a 280# boron carbide abrasive to control the final thickness to be 6 +/-0.1 mm, measuring the thickness deviation of 4 points to be controlled within 0.003mm, grinding and polishing the second surface of the YAG crystal lath by using the same method as the first surface of the YAG crystal lath, controlling the flatness to be within 0.5 lambda 632 @.8 nm, heating the polished YAG crystal lath again, taking the YAG crystal lath off the point adhesive plate,
carrying out flatness test on the YAG crystal strip, identifying a high point area of a large surface of the strip by using an identification pen, and carrying out pressure polishing on the identified high point by using a non-deformation separation disc clamp to control the flatness of the YAG crystal strip within 0.5 lambda @632.8 nm.
In some embodiments, the grinding comprises: removing scratches on the surface of the crystal by using 280# boron carbide, grinding by using W40 boron carbide for at least 0.04mm, grinding by using W20 boron carbide for at least 0.03mm, and grinding by using W10 boron carbide for at least 0.02 mm.
The grinding process of the YAG series material with the ultra-smooth surface provided by the embodiment of the invention comprises the following steps: the grinding is respectively carried out by adopting 280# boron carbide, W40 boron carbide, W20 boron carbide and W10 boron carbide, and after the grinding materials with the specifications are subjected to step-by-step rough grinding, the roughness of the surface of the material can be gradually reduced, and the subsequent further polishing treatment is facilitated.
In some embodiments, the polishing comprises the steps of: the mixed solution containing W1 white corundum micropowder and acidic polishing solution is used for polishing on a polyurethane polishing pad for 8-12 hours, the mixed solution containing W0.5 white corundum micropowder and acidic polishing solution is used for polishing on an asphalt polishing die for 4-8 hours, the mixed solution containing W0.1 white corundum micropowder and acidic polishing solution is used for polishing on the asphalt polishing die for 4-8 hours, and the acidic polishing solution is used for polishing on a polytetrafluoroethylene polishing die for 3-6 hours.
The polishing process of the YAG series material with the ultra-smooth surface provided by the embodiment of the invention comprises the following steps: the mixed liquid of the abrasive materials with different particle sizes and the acidic polishing liquid is used for polishing at least once, the chemical polishing liquid has a good chemical corrosion effect on the surface and the sub-surface damaged layer of the YAG series material after being ground, the removal of the damaged layer can be accelerated, the polishing efficiency is improved, and compared with the efficiency of polishing only by using polishing powder, the polishing efficiency can be improved by 30%.
In some embodiments, the heating temperature is 100-110 ℃.
In some embodiments, the preparation process of the YAG crystal lath further comprises the steps of preparing a glue dispensing disc: a dispensing disc is made of YAG crystal columns according to the size of a YAG crystal lath, and the flatness of the dispensing disc is trimmed to be less than 1 lambda @632.8nm before the dispensing disc is heated.
In some embodiments, the YAG family of materials is selected from YAG, Nd: YAG, Nd, Ce: YAG and Cr4+: YAG and Yb: any of YAGThe method is as follows.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The preparation process of the acidic polishing solution is as follows: concentrated sulfuric acid, glacial acetic acid, ammonium dichromate, phosphoric acid and water are mixed according to a mass ratio of 1: 1: 1: 0.8-1.2: 50, and adding distilled water to dilute until the pH is 3-5 when in use.
Comparative examples 1 to 4 and the corresponding experimental results after the compounding ratio was changed are as follows:
comparative example 1
An acidic polishing solution was prepared, which was different from example 1 only in that: mixing concentrated sulfuric acid, glacial acetic acid, ammonium dichromate and phosphoric acid according to the weight ratio of 1: 1: 1: 0.6: 50, and adding distilled water to dilute until the pH is 3-5 when in use.
The acidic polishing solution is used for polishing one side of Cr with the size of phi 10 multiplied by 4mm4+: the application in the YAG wafer processing process is as follows:
1) heating the upper disc: mixing Cr of phi 10X 4mm4+: YAG and aluminum plate are heated to 100-110 ℃, bonding wax is evenly coated on the aluminum plate, and then pure Cr is coated on the aluminum plate4+: YAG is bonded on the aluminum plate;
2) grinding: and sequentially grinding and removing the cutting tool mark on the crystal surface by using a 280# boron carbide grinding material → grinding by using a W40 boron carbide grinding material for 0.06mm to remove the coarse sand hole left by the 280# boron carbide grinding material → grinding by using a W20 boron carbide grinding material for 0.05mm to remove the coarse sand hole left by the W40 boron carbide grinding material → grinding by using a W10 boron carbide grinding material for 0.03mm to remove the coarse sand hole left by the W20 boron carbide grinding material.
3) Polishing: polishing the mixed W1 white corundum micro powder and the acidic polishing solution on a polyurethane polishing pad for about 12 hours → polishing the mixed W0.5 white corundum micro powder and the acidic polishing solution on a self-made asphalt polishing die for about 6 hours → polishing the mixed W0.1 white corundum micro powder and the acidic polishing solution on the self-made asphalt polishing die for about 6 hours → polishing the acidic polishing solution on a polytetrafluoroethylene polishing die for 5 hours.
4) Heating a lower disc: cr to be polished4+: YAG is heated to 100-110 ℃ until the bonding wax is softenedMixing Cr4+: and (5) taking down the YAG.
Cr in comparative example 14+: the results of the YAG wafer roughness test are shown in fig. 1. As can be seen, Cr was present after polishing with the acidic polishing solution of comparative example 14+: the YAG wafer has a large roughness value and does not meet the use requirement.
Comparative example 2
An acidic polishing solution was prepared, which was different from example 1 only in that: mixing concentrated sulfuric acid, glacial acetic acid, ammonium dichromate and phosphoric acid according to the weight ratio of 1: 1: 1: 1.5: 50, and adding distilled water to dilute until the pH is 3-5 when in use.
Cr Using the same procedure as in comparative example 14+: YAG wafers were polished except that the polishing solution used was the acidic polishing solution of comparative example 2, and Cr was detected after polishing with the acidic polishing solution of comparative example 24+: the YAG surface has corrosion points which can not meet the requirement of smoothness.
Comparative example 3
The preparation method of the acid polishing solution is different from that of the embodiment 1 only in that the dosage of concentrated sulfuric acid is different, and the YAG crystal hydrolysis is alkalescent, so that the YAG crystal material can promote the hydrolysis of the YAG surface under the action of the acid polishing solution, and the dosage of the concentrated sulfuric acid can influence the progress of the hydrolysis reaction and the polishing efficiency, so that the dosage of the concentrated sulfuric acid is reduced, the hydrolysis reaction is weakened, the efficiency is reduced, the roughness of the crystal surface cannot be further reduced, and the crystal is seriously corroded to generate pits on the surface of the crystal beyond the dosage, and the crystal surface is damaged.
Comparative example 4
The preparation of an acidic polishing solution is different from that of example 1 only in that glacial acetic acid and ammonium dichromate are used in different amounts, and according to YAG series materials, the YAG series materials can be slightly dissolved in phosphoric acid at high temperature (more than 250 ℃), the reaction can be carried out at normal temperature under the condition of adding a catalyst ammonium dichromate, namely phosphoric acid and ammonium dichromate can quickly react a ground surface loose layer and a sub-surface damaged layer, the polishing efficiency is improved, and the sub-surface damaged layer is removed at the same time, so that the reaction rate can be changed by using the catalyst, and the catalytic reaction rate can be changed by reducing or increasing the catalyst amount, and the polishing process cannot be effectively controlled; because the ammonium dichromate and the strong acid are mixed to cause explosion risk, the glacial acetic acid is adopted as a solvent to firstly dissolve the ammonium dichromate, and then the phosphoric acid and the sulfuric acid are added, and the glacial acetic acid plays a role in moderating reaction, so that the acidic polishing solution can be used under a mild condition, and the corrosion effect of the polishing solution is reduced.
Example 2
Yb polished on a single side with a size of 40X 5 mm: the method for obtaining the ultra-smooth surface on the YAG square sheet comprises the following steps:
1) heating the upper disc: yb of 40X 5 mm: YAG square pieces and an aluminum plate are heated to 100-: YAG square pieces are bonded on the aluminum plate;
2) grinding: and sequentially grinding and removing the cutting tool mark on the crystal surface by using a 280# boron carbide grinding material → grinding by using a W40 boron carbide grinding material for 0.06mm to remove the coarse sand hole left by the 280# boron carbide grinding material → grinding by using a W20 boron carbide grinding material for 0.05mm to remove the coarse sand hole left by the W40 boron carbide grinding material → grinding by using a W10 boron carbide grinding material for 0.03mm to remove the coarse sand hole left by the W20 boron carbide grinding material.
3) Polishing: the mixed solution containing W1 white corundum micropowder and acidic polishing solution is sequentially adopted to polish on a polyurethane polishing pad for about 12 hours → the mixed solution containing W0.5 white corundum micropowder and acidic polishing solution is polished on a self-made asphalt polishing mould for about 6 hours → the mixed solution containing W0.1 white corundum micropowder and acidic polishing solution is polished on the self-made asphalt polishing mould for about 6 hours → the acidic polishing solution is polished on a polytetrafluoroethylene polishing mould for 5 hours.
4) Heating a lower disc: and (3) polishing the surface of the polished Yb: YAG square piece is heated to 100-: and taking down the YAG square piece.
Yb: the results of the YAG square piece roughness measurement are shown in fig. 2.
Example 3
A method for obtaining an ultra-smooth surface on a double-side polished pure YAG wafer of size phi 10 x 4mm, comprising the steps of:
1) heating the upper disc: heating a pure YAG wafer with the diameter of 10 multiplied by 4mm and an aluminum disc to the temperature of 100-;
2) grinding the first surface: and grinding by using a 280# boron carbide abrasive to remove the cutting tool mark on the crystal surface → grinding by using a W40 boron carbide abrasive for 0.04mm to remove the coarse sand hole left by the 280# boron carbide abrasive → grinding by using a W20 boron carbide abrasive for 0.03mm to remove the coarse sand hole left by the W40 boron carbide abrasive → grinding by using a W10 boron carbide abrasive for 0.02mm to remove the coarse sand hole left by the W20 boron carbide abrasive.
3) Polishing the first surface: the mixed solution containing W1 white corundum micropowder and acidic polishing solution is sequentially adopted to polish on a polyurethane polishing pad for about 8 hours → the mixed solution containing W0.5 white corundum micropowder and acidic polishing solution is polished on a self-made asphalt polishing mould for about 4 hours → the mixed solution containing W0.1 white corundum micropowder and acidic polishing solution is polished on the self-made asphalt polishing mould for about 4 hours → the acidic polishing solution is polished on a polytetrafluoroethylene polishing mould for 3 hours.
4) Heating a lower disc: heating the polished pure YAG wafer with the diameter of 10 multiplied by 4mm to 110 ℃ of 100-.
5) And (3) optical cement feeding: cleaning a pure YAG wafer with the diameter of 10 multiplied by 4mm, uniformly coating the YAG wafer on a light adhesive backing plate, and then coating waterproof paint.
6) Grinding the second surface: grinding by using a 280# boron carbide grinding material, controlling the final thickness to be 4 +/-0.1 mm, measuring the thickness of 4 points on a photoresist disc, controlling the thickness deviation to be within 0.003mm after grinding, and grinding the rest grinding processes with the first surface.
7) Polishing the second surface: the polishing process is the same as the first side polishing.
The results of the roughness test of the pure YAG wafer prepared in this example are shown in fig. 3 and 4.
Example 4
In a Nd size of 6X 35X 140 mm: a method for obtaining an ultra-smooth surface with good flatness on a large surface (35 x 140mm) of YAG lath comprises the following steps:
1) dispensing and hanging the disc: heating the dispensing disc and the lath to be processed to 100-110 ℃, uniformly coating adhesive wax on the dispensing disc, and then adding Nd: YAG laths are bonded on the dispensing disc;
the glue dispensing disc is made by uniformly bonding phi 5X 4mm YAG small crystal columns on a phi 180X 20mm aluminum disc by 502 glue, the distance between each crystal column and the adjacent crystal column is 10mm, compared with the traditional upper disc, the glue dispensing upper disc reduces the bonding tension by reducing the bonding surface, further reduces the deformation of the upper plate and the lower plate of the small strip disc, and further obtains better flatness (generally, 5 microns of the conventional upper disc can be lifted to about 1 micron),
2) grinding the first surface: and sequentially grinding and removing the cutting tool mark on the crystal surface by using a 280# boron carbide grinding material → grinding by using a W40 boron carbide grinding material for 0.06mm to remove the coarse sand hole left by the 280# boron carbide grinding material → grinding by using a W20 boron carbide grinding material for 0.05mm to remove the coarse sand hole left by the W40 boron carbide grinding material → grinding by using a W10 boron carbide grinding material for 0.03mm to remove the coarse sand hole left by the W20 boron carbide grinding material.
3) Polishing the first surface: the mixed solution containing W1 white corundum micropowder and acidic polishing solution is sequentially adopted to polish on a polyurethane polishing pad for about 12 hours → the mixed solution containing W0.5 white corundum micropowder and acidic polishing solution is polished on a self-made asphalt polishing mould for about 8 hours → the mixed solution containing W0.1 white corundum micropowder and acidic polishing solution is polished on the self-made asphalt polishing mould for about 8 hours → the acidic polishing solution is polished on a polytetrafluoroethylene polishing mould for 6 hours, and before polishing, the flatness of a batten disc is required to be ensured to be superior to 0.5 lambda @632.8 nm.
4) Heating a lower disc: and heating the polished lath to 110 ℃ at 100 ℃, and taking down the lath after the bonding wax is softened.
5) And (3) optical cement feeding: mixing Nd: after the YAG lath is cleaned, the uniform optical cement is coated on the optical cement backing plate, and then waterproof paint is coated.
6) Grinding the second surface: the final thickness is controlled to be 6 +/-0.1 mm by using a 280# boron carbide abrasive, the thickness deviation of 4 measured points is controlled to be within 0.003mm, and the rest grinding processes are carried out in the same way as the grinding of the first surface.
7) Polishing the second surface: the polishing process is the same as the first side polishing.
8) The flatness is improved by a deformation-free separation disc loading method: and after polishing the second surface, measuring the flatness of the two large surfaces by adopting a Zygo interferometer, marking the high points of the planes by using a marker pen, putting the lath into a separator, pressurizing and polishing the marked high points, correcting the flatness of the lath, and finally controlling the flatness within 0.5 lambda @632.8 nm.
Nd prepared in this example: the results of the YAG crystal plate roughness test are shown in the attached figures 5 and 6, and the results of the flatness test are shown in the attached figures 7 and 8.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
1) polishing YAG series crystals by using an acidic polishing solution to improve polishing efficiency, and simultaneously reducing surface roughness through chemical action;
the acid polishing solution is prepared according to the characteristics of YAG series crystal materials by the following steps: concentrated sulfuric acid, glacial acetic acid, ammonium dichromate, phosphoric acid and water are mixed according to a mass ratio of 1: 1: 1: 0.8-1.2: 50, adding distilled water to dilute the mixture to pH 3-5 when in use, wherein the acid polishing solution has good chemical corrosion effect on the surface and sub-surface damaged layers of the ground YAG series, can accelerate the removal of the damaged layers and improve the polishing efficiency, and can improve the polishing efficiency by 30 percent compared with the polishing efficiency only by adopting polishing powder.
2) Adopting a dispensing and deformation-free separation technology to control the surface roughness of the YAG crystal below 0.3nm and improve the surface flatness of the large-size YAG crystal lath from 5 microns in a traditional feeding mode to within 0.5 microns;
3) and a polishing procedure without polishing powder is added to further improve the surface roughness: after the conventional polishing is finished, polishing for 3 hours by using self-made acidic polishing solution on a polytetrafluoroethylene polishing die, further reducing the surface roughness, and improving the surface roughness to the atomic level: the polytetrafluoroethylene polishing mold has the characteristics of good surface roughness and difficult deformation, and is the most suitable polishing mold material for improving the surface roughness of YAG crystals. The final surface roughness of a polishing material is determined to a great extent by the particle size of polishing powder, polishing without the polishing powder is the most effective method for improving the surface roughness of crystals, but in the actual production process, the problem of subsurface damage caused by friction increase and untimely heat dissipation in the pure water polishing process is solved, and the acidic polishing solution has better lubricating and heat dissipation effects besides the effect of corroding a crystal surface damage layer to improve the polishing efficiency, so that the crystal surface roughness can be further improved.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of protection of the present invention.
Claims (13)
1. An acidic polishing solution, which is used for polishing the surface of YAG series materials and is prepared by the following method: concentrated sulfuric acid, glacial acetic acid, ammonium dichromate, phosphoric acid and water are mixed according to a mass ratio of 1: 1: 1: 0.8-1.2: 50, mixing;
when the acidic polishing solution is used, water is added to dilute the acidic polishing solution until the pH value is 3-5.
2. The acidic polishing solution according to claim 1, wherein the water is selected from distilled water.
3. A method for obtaining a YAG-based material with an ultra-smooth surface, comprising: polishing the YAG series material with the acidic polishing liquid according to claim 2.
4. The method according to claim 3, wherein the YAG series material is selected from any one of a YAG crystal wafer, a YAG crystal square and a YAG crystal lath.
5. The method of claim 4, wherein polishing controls the surface roughness of the YAG crystal wafer or square wafer to within 0.3 nm.
6. The method of claim 4, wherein polishing controls the roughness to within 0.3nm and the flatness to within 0.5 μm on the large face of the YAG crystal lath.
7. The method of claim 4, wherein the preparation of the YAG crystal wafer or square YAG crystal wafer comprises the steps of:
respectively heating a dispensing disc and the YAG crystal wafer or the YAG crystal square plate, feeding the YAG crystal wafer or the YAG crystal square plate in a dispensing mode,
grinding and polishing at least one surface of the YAG crystal wafer or the YAG crystal square plate,
and after the polished YAG crystal wafer or YAG crystal square piece and the dispensing disc are heated again, taking down the YAG crystal wafer or YAG crystal square piece from the dispensing disc.
8. The method of claim 4, wherein the preparation of the YAG crystal slab comprises the steps of:
respectively heating a dispensing disc and the YAG crystal lath, feeding the YAG crystal lath in a dispensing manner, grinding and polishing the first surface of the YAG crystal lath, controlling the flatness within 0.5 lambda @632.8nm, heating the polished YAG crystal lath again, taking the YAG crystal lath off the dispensing disc,
cleaning the YAG crystal lath, then hanging the plate in a manner of optical cement, coating waterproof paint, grinding the second surface of the YAG crystal lath by using a 280# boron carbide abrasive to control the final thickness to be 6 +/-0.1 mm, measuring 4 points to control the thickness deviation to be within 0.003mm, grinding and polishing the second surface of the YAG crystal lath by adopting the same method as the first surface of the YAG crystal lath, controlling the flatness to be within 0.5 @ lambda 632.8nm, heating the polished YAG crystal lath again, taking the YAG crystal lath down from the adhesive tape,
and carrying out flatness test on the YAG crystal strip, identifying a high point area of a large surface of the strip by using an identification pen, and pressurizing and polishing the identified high point by using a non-deformation separation disc clamp to control the flatness of the YAG crystal strip within 0.5 lambda @632.8 nm.
9. The method according to claim 7 or 8, wherein the grinding comprises the steps of: removing scratches on the surface of the crystal by using 280# boron carbide, grinding by using W40 boron carbide for at least 0.04mm, grinding by using W20 boron carbide for at least 0.03mm, and grinding by using W10 boron carbide for at least 0.02 mm.
10. The method according to claim 7 or 8, wherein the polishing comprises the steps of: the mixed solution containing W1 white corundum micropowder and acidic polishing solution is used for polishing on a polyurethane polishing pad for 8-12 hours, the mixed solution containing W0.5 white corundum micropowder and acidic polishing solution is used for polishing on an asphalt polishing die for 4-8 hours, the mixed solution containing W0.1 white corundum micropowder and acidic polishing solution is used for polishing on the asphalt polishing die for 4-8 hours, and the acidic polishing solution is used for polishing on a polytetrafluoroethylene polishing die for 3-6 hours.
11. The method as claimed in claim 7 or 8, wherein the heating temperature is 100-110 ℃.
12. The method of claim 8, further comprising the step of forming a dispensing tray: and manufacturing a dispensing disc by using a YAG crystal column according to the size of the YAG crystal lath, and trimming the flatness of the dispensing disc to be less than 1 lambda @632.8nm before heating the dispensing disc.
13. The method according to claim 7 or 8, characterized in that said YAG family material is selected from the group consisting of YAG, Nd: YAG, Nd, Ce: YAG and Cr4+: YAG and Yb: any one of YAG.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654585A (en) * | 2005-01-17 | 2005-08-17 | 上海大学 | Core/shell nano particle grinding agent polishing solution composition and method for preparing same |
| JP2005225683A (en) * | 2004-02-10 | 2005-08-25 | Sumitomo Metal Mining Co Ltd | Production method for non-magnetic garnet substrate, and substrate produced thereby |
| JP2006315880A (en) * | 2005-05-10 | 2006-11-24 | Nikon Corp | Method for manufacturing optical element, optical element, and projection aligner equipped with the same |
| CN102909650A (en) * | 2012-11-01 | 2013-02-06 | 成都精密光学工程研究中心 | Surface processing method of strip laser medium |
| CN103231320A (en) * | 2013-04-16 | 2013-08-07 | 北京理工大学 | Multi-point supporting surface type adjustable self-locking polishing disk for surface machining |
| CN205852447U (en) * | 2016-08-31 | 2017-01-04 | 东莞市兰光光学科技有限公司 | Frock for optical element grinding and polishing |
| CN107011806A (en) * | 2017-04-27 | 2017-08-04 | 安徽智诚光学科技有限公司 | A kind of mobile phone liquid crystal touch control screen polishing agent and preparation method thereof |
| CN107597504A (en) * | 2017-10-27 | 2018-01-19 | 中国科学院上海光学精密机械研究所 | Optical element original position automatic dispensing device and dispensing method |
| CN109193334A (en) * | 2018-10-08 | 2019-01-11 | 安徽环巢光电科技有限公司 | The preparation method of disc waveguide laser crystal |
| CN109590820A (en) * | 2019-01-02 | 2019-04-09 | 中国科学院上海光学精密机械研究所 | The processing method of superhard laser crystal surface roughness |
| CN109807694A (en) * | 2019-01-16 | 2019-05-28 | 西安应用光学研究所 | It is a kind of to control disk tooling and polishing method on the mass center that the special-shaped high parallel error of optical window part is processed |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7344988B2 (en) * | 2003-10-27 | 2008-03-18 | Dupont Air Products Nanomaterials Llc | Alumina abrasive for chemical mechanical polishing |
-
2019
- 2019-07-02 CN CN201910588392.0A patent/CN110183972B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005225683A (en) * | 2004-02-10 | 2005-08-25 | Sumitomo Metal Mining Co Ltd | Production method for non-magnetic garnet substrate, and substrate produced thereby |
| CN1654585A (en) * | 2005-01-17 | 2005-08-17 | 上海大学 | Core/shell nano particle grinding agent polishing solution composition and method for preparing same |
| JP2006315880A (en) * | 2005-05-10 | 2006-11-24 | Nikon Corp | Method for manufacturing optical element, optical element, and projection aligner equipped with the same |
| CN102909650A (en) * | 2012-11-01 | 2013-02-06 | 成都精密光学工程研究中心 | Surface processing method of strip laser medium |
| CN103231320A (en) * | 2013-04-16 | 2013-08-07 | 北京理工大学 | Multi-point supporting surface type adjustable self-locking polishing disk for surface machining |
| CN205852447U (en) * | 2016-08-31 | 2017-01-04 | 东莞市兰光光学科技有限公司 | Frock for optical element grinding and polishing |
| CN107011806A (en) * | 2017-04-27 | 2017-08-04 | 安徽智诚光学科技有限公司 | A kind of mobile phone liquid crystal touch control screen polishing agent and preparation method thereof |
| CN107597504A (en) * | 2017-10-27 | 2018-01-19 | 中国科学院上海光学精密机械研究所 | Optical element original position automatic dispensing device and dispensing method |
| CN109193334A (en) * | 2018-10-08 | 2019-01-11 | 安徽环巢光电科技有限公司 | The preparation method of disc waveguide laser crystal |
| CN109590820A (en) * | 2019-01-02 | 2019-04-09 | 中国科学院上海光学精密机械研究所 | The processing method of superhard laser crystal surface roughness |
| CN109807694A (en) * | 2019-01-16 | 2019-05-28 | 西安应用光学研究所 | It is a kind of to control disk tooling and polishing method on the mass center that the special-shaped high parallel error of optical window part is processed |
Non-Patent Citations (3)
| Title |
|---|
| "Acid resistance of erbium-doped yttrium aluminum garnet laser-treated and phosphoric acid-etched enamels";Kim, Jung-Ho 等;《ANGLE ORTHODONTIST》;20061130;第76卷(第6期);1052-1056 * |
| "无蜡上盘加工 Nd :YAG 激光晶体板条";徐斌 等;《新技术新工艺》;20101231(第7期);52-53 * |
| "硬脆材料超精密加工关键技术研究";李军;《中国博士学位论文全文数据库（工程科技I辑）》;20070415(第4期);I135-4 * |
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