CN103231302B - Method for obtaining super-smooth surface low-sub-surface-damage crystal - Google Patents
Method for obtaining super-smooth surface low-sub-surface-damage crystal Download PDFInfo
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- CN103231302B CN103231302B CN201310127749.8A CN201310127749A CN103231302B CN 103231302 B CN103231302 B CN 103231302B CN 201310127749 A CN201310127749 A CN 201310127749A CN 103231302 B CN103231302 B CN 103231302B
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Abstract
The invention relates to a method for obtaining super-smooth surface low-sub-surface-damage crystal. The method includes the following steps: (1) grinding crystal on a cast iron disc by using boron carbide with the specification as W1 as a grinding material; (2) polishing the crystal on an asphalt disc by using cerium oxide polishing liquid with the particle size as 1 mum; (3) soaking the crystal surface in an organic solvent and processing for 30-60 seconds in an ultrasonic mode; (4) polishing the crystal for 10-15 minutes on a polyurethane polishing gasket by using silicon dioxide polishing liquid with the particle size as 100 nm; (5) placing the crystal in the organic solvent, washing for 30-60 seconds in an ultrasonic mode, and observing the surface topography of the crystal by using a high-power microscope; and (6) if the crystal surface still has scratches, repeating the step (2) to step (5), replacing the cerium oxide polishing liquid with the particle size as 1 mum in the step (2) with cerium oxide polishing liquid with the particle size as 100-300 nm. Compared with the prior art, the method is simple to operate, high in processing efficiency and convenient to popularize.
Description
Technical field
The present invention relates to crystal ultra-smooth precision machining method, especially relate to a kind of method obtaining the low sub-surface damage crystal of super-smooth surface.
Background technology
The technology such as high energy ultra-short pulse laser, except requiring that the crystal such as such as YCOB, KDP, LBO have good surface roughness so that except plated film, can not cause the absorption to laser, scattering because plane of crystal has the defect such as cut or trachoma when light laser is incident.Therefore ensureing that plane of crystal reaches outside dust magnitude roughness, needing the quantity as far as possible controlling the sub-surface scratch of crystal.The general own quality of this crystalloid softer (Mohs' hardness about 6.5), traditional finishing method is easy to leave tiny cut at plane of crystal or only have smooth surface, but the subsurface stratum under top layer remains numerous scratch damage.Domestic not scientific research institution provides the detailed glossing of the similar crystal such as YCOB and removes the method for sub-surface damage cut at present.The present invention is directed to the Ultra-precision Turning technique that domestic current present situation proposes a kind of crystal photoelement, this abrasive polishing process can obtain the precision crystal optical element that face type is good, have super-smooth surface and extremely low sub-surface damage, also has the advantages such as working (machining) efficiency is high, process stabilizing simultaneously.Reach ring after this patent can being made to implement on traditional twin shaft lapping and buffing machine by custom-designed fixture and throw level, and then reduce process costs.
Summary of the invention
Object of the present invention be exactly provide to overcome defect that above-mentioned prior art exists a kind of simple to operate, with strong points, reliability is high, working (machining) efficiency is high, be convenient to the method for the low sub-surface damage crystal of acquisition super-smooth surface promoted.
The present invention, under the condition of existing twin shaft lapping and buffing machine or glass polishing machine, designs a kind of method obtaining the low sub-surface damage crystal of super-smooth surface.The method can by suitably adjusting the grinding and polishing being applied to multiple crystal.
Object of the present invention can be achieved through the following technical solutions:
Obtain a method for the low sub-surface damage crystal of super-smooth surface, the method comprises the following steps:
(1) grind: use the boron carbide that specification is W1 to grind crystal on cast iron plate as abrasive material;
(2) rough polishing: prepare pitch dish and after revising pitch card type, roughness, uses particle diameter to be that the cerium oxide polishing slurry of 1 μm carries out machine glazed finish to crystal until plane of crystal roughness reaches 1nm or basic no marking on pitch dish;
(3) etch: plane of crystal is immersed in organic solvent, utilize ultrasonic washing instrument ultrasonic process 30-60 second, to remove plane of crystal hydrolysis layer, polishing powder or crystal powder ultrasonic erosion in crystal scratch defects will be inserted and fall;
(4) chemically mechanical polishing: the silicon dioxide polishing solution that uses particle diameter to be 100nm is to polishing crystal 10 ~ 15 minutes on polyurethane polishing pad, and remove remaining minute scratch marks within a short period of time does not affect crystal face type simultaneously;
(5) detect: crystal is placed in organic solvent for ultrasonic cleaning 30-60 second, with ultramicroscopic observation plane of crystal pattern;
(6) if plane of crystal no marking, then the crystal with the low sub-surface damage of super-smooth surface is obtained; If plane of crystal still has cut, repeat step (2) ~ (5), and the cerium oxide polishing slurry being 1 μm by particle diameter in step (2) changes the cerium oxide polishing slurry that particle diameter is 100-300nm into.
The concrete steps of the grinding described in step (1) comprise: paste screening glass by around crystal; crystal paraffin is fixed on grinding tool; then crystal is clamped with clamping device; twin shaft fine grinding polish machine use boron carbide that specification is W1 as abrasive material; and coordinate cast iron plate to grind crystal; fast by the damage layer that the upper operation of removal is brought, make plane of crystal have good face type, flatness is up to standard.
The temperature of the rough polishing described in step (2) is 19.5 ~ 20.5 DEG C, and the time of rough polishing is 2 ~ 3 hours.
In the process of the middle polishing crystal of step (2), be that the mass fraction of cerium oxide in the cerium oxide polishing slurry of 1 μm drops to 3% gradually by 6% by particle diameter.
Step (3) or the organic solvent described in step (5) are that (be called for short Me6Si2, molecular formula is (CH to hexamethyldisilane
3)
3siSi (CH
3)
3).
The temperature of the organic solvent described in step (3) is 40 ~ 50 DEG C.
Chemically mechanical polishing described in step (4) adopts twin shaft polishing machine, and the speed of mainshaft of this twin shaft polishing machine is 30 revs/min, and the balance staff rotating speed of twin shaft polishing machine is 12 revs/min.
Compared with prior art, the present invention has the following advantages and beneficial effect:
1, the crystal photoelement with super-smooth surface can be processed within a short period of time, there is extremely low sub-surface damage and good face type simultaneously.This processing method is applicable to obtain the precision crystal optical element of extremely low sub-surface damage, and similar crystal polishing technique has certain guidance meaning.
2, compared with prior art, the present invention is easy and simple to handle, with strong points, and reliability is high, is applicable to multiple types like crystal grinding and polishing, also has the advantages such as working (machining) efficiency is high, process stabilizing simultaneously, is convenient to promote.
3, reach ring after this patent can being made to implement on traditional twin shaft lapping and buffing machine by custom-designed fixture and throw level, and then reduce process costs.
Accompanying drawing explanation
Fig. 1 is YCOB crystal plane of crystal pattern under light microscope after the grinding of W1 boron carbide cast iron plate in embodiment 1;
Fig. 2 is YCOB crystal plane of crystal pattern under light microscope after 1 μm of cerium oxide polishing in embodiment 1;
Fig. 3 be in embodiment 1 YCOB crystal through organic solvent ultrasonic washing instrument ultrasonic erosion 45 seconds rear surface patterns;
Fig. 4 be in embodiment 1 YCOB crystal through the polishing of 100nm silicon dioxide polishing solution and cleaning treatment rear surface microstructure.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Grinding and polishing process is carried out to YCOB crystal:
1, grind---YCOB crystal paraffin is fixed on carrying disk, around crystal, pastes screening glass.Ground on cast iron plate by crystal, collocation abrasive material is the boron carbide of W1, and milled processed on Nanjing profit raw twin shaft fine grinding polish machine JM 030.2, the surface topography of crystal as shown in Figure 1.Reduce damage layer depth while can ensureing grinding rate like this, shorten follow-up polishing time.And the crystal turned-down edge introduced unbalanced by moment when the cooperation of holding tool avoids axle to move on twin shaft lapping and buffing machine, and then ensure that crystal face type is good.
2, lacquer disk(-sc) is made---select Switzerland's GUGOLZ company No.55 pitch to be placed on carrying disk, fix a circle adhesive tape around, increase heating-up temperature gradually, avoid stirring as far as possible and introduce bubble.Paraffin can be added in right amount and avoid that pitch dish is really up to the mark introduces cut in polishing process.Pitch panel surface is smooth and a little after cooling, mark indentation in panel surface, and flattens through row asphalt surface with the optical glass that face type, roughness are good immediately.Finally to pitch dish repair dish work to ensure pitch panel surface face type, flatness all reaches standard.
3, rough polishing---YCOB crystal ground is before thrown in advance.Regulate indoor temperature to make it be stabilized in 19.5 ~ 20.5 DEG C, utilize for the clamping device involved by twin shaft polishing machine, by polishing with repair dish and operate and carry out simultaneously, guarantee the smooth of pitch card.Carry out machine glazed finish with the cerium rouge that particle diameter is 1 μm, under the effect of mechanical grinding, realize global planarizartion, the surface topography of crystal as shown in Figure 2.After determining that substantially previous step grinding operation being produced damage layer removes, reduce polishing fluid concentration gradually and carry out successively polishing.
4, etching---in polishing process, YCOB plane of crystal can produce cut under the effect of polishing powder and lacquer disk(-sc), polishing powder or the chip of crystal own can be packed in cut, plane of crystal also can constantly produce the hydrolysis layer with mobility, cause the defects such as the cut in crystal sub-surface damage layer cover by the hydrolysis layer of flowing, be difficult to effective abatement.Crystal is immersed in organic solvent and carry out ultrasonic etching processing with the brilliant VGT-1860QTD/40KHz ultrasonic washing instrument of Hefei section, control time is within 30 seconds to 1 minute, hydrolysis layer and filler are dissolved, cut in sub-surface damage layer reveals, this body structure of crystal can not be destroyed by organic solvent by the accurate control of etch period, simultaneously for next step process lays the first stone, the surface topography of crystal as shown in Figure 3.
5, CMP essence is thrown---and the silica colloidal polishing liquid using particle diameter to be about 100nm coordinates polyurethane polishing pad, chemically mechanical polishing is carried out to the crystal after etching processing, the speed of mainshaft be 30 revs/min, under the condition of balance staff rotating speed 12 revs/min, it is 15 minutes that polishing time controls, shorter polishing time can while removal cut, the as far as possible little face type affecting crystal.
6, detect---crystal is placed in organic solvent and cleans 30-60 second at ultrasonic washing instrument, with ultramicroscopic observation plane of crystal pattern.
If 7, secondary fine is thrown---plane of crystal still has fine scratches, continue to utilize more small particle diameter (100-300nm) cerium oxide polishing slurry polishing 2-3 hour, ultrasonic erosion 30 seconds, and coordinating 100nm silicon dioxide gel polishing fluid to carry out polishing in short-term in 10 minutes to obtain required super-smooth surface with polyurethane polishing pad, the surface topography of crystal is as shown in Figure 4.
Embodiment 2
Obtain a method for the low sub-surface damage crystal of super-smooth surface, the method comprises the following steps:
(1) grind: paste screening glass by around crystal, crystal paraffin is fixed on grinding tool, then crystal is clamped with clamping device, twin shaft fine grinding polish machine use boron carbide that specification is W1 as abrasive material, and coordinate cast iron plate to grind crystal, fast by the damage layer that the upper operation of removal is brought, make plane of crystal have good face type, flatness is up to standard;
(2) rough polishing: prepare pitch dish and after revising pitch card type, roughness, use particle diameter is that the cerium oxide polishing slurry of 1 μm carries out machine glazed finish to crystal until plane of crystal roughness reaches 1nm or basic no marking on pitch dish, wherein, the temperature of rough polishing remains on 19.5 ~ 20.5 DEG C, the time of rough polishing is 2 hours, in the process of polishing crystal, be that the mass fraction of cerium oxide in the cerium oxide polishing slurry of 1 μm drops to 3% gradually by 6% by particle diameter, in the process of polishing crystal, pitch dish is trimmed simultaneously and makes the card of pitch dish smooth;
(3) etch: plane of crystal is immersed in organic solvent hexamethyldisilane, the temperature of organic solvent is 40 DEG C, utilize the ultrasonic process of ultrasonic washing instrument 60 seconds, to remove plane of crystal hydrolysis layer, polishing powder or crystal powder ultrasonic erosion in crystal scratch defects will be inserted and fall;
(4) chemically mechanical polishing: the silicon dioxide polishing solution that uses particle diameter to be 100nm on polyurethane polishing pad to polishing crystal 10 minutes, chemically mechanical polishing adopts twin shaft polishing machine, the speed of mainshaft of this twin shaft polishing machine is 30 revs/min, the balance staff rotating speed of twin shaft polishing machine is 12 revs/min, and remove remaining minute scratch marks within a short period of time does not affect crystal face type simultaneously;
(5) detect: crystal is placed in organic solvent hexamethyldisilane ultrasonic cleaning 30 seconds, with ultramicroscopic observation plane of crystal pattern;
(6) if plane of crystal no marking, then the crystal with the low sub-surface damage of super-smooth surface is obtained; If plane of crystal still has cut, repeat step (2) ~ (5), and the cerium oxide polishing slurry being 1 μm by particle diameter in step (2) changes the cerium oxide polishing slurry that average grain diameter is 100nm into.
Embodiment 3
Obtain a method for the low sub-surface damage crystal of super-smooth surface, the method comprises the following steps:
(1) grind: paste screening glass by around crystal, crystal paraffin is fixed on grinding tool, then crystal is clamped with clamping device, twin shaft fine grinding polish machine use boron carbide that specification is W1 as abrasive material, and coordinate cast iron plate to grind crystal, fast by the damage layer that the upper operation of removal is brought, make plane of crystal have good face type, flatness is up to standard;
(2) rough polishing: prepare pitch dish and after revising pitch card type, roughness, use particle diameter is that the cerium oxide polishing slurry of 1 μm carries out machine glazed finish to crystal until plane of crystal roughness reaches 1nm or basic no marking on pitch dish, wherein, the temperature of rough polishing remains on 19.5 ~ 20.5 DEG C, the time of rough polishing is 3 hours, in the process of polishing crystal, be that the mass fraction of cerium oxide in the cerium oxide polishing slurry of 1 μm drops to 3% gradually by 6% by particle diameter, in the process of polishing crystal, pitch dish is trimmed simultaneously and makes the card of pitch dish smooth;
(3) etch: plane of crystal is immersed in organic solvent hexamethyldisilane, the temperature of organic solvent is 50 DEG C, utilize the ultrasonic process of ultrasonic washing instrument 30 seconds, to remove plane of crystal hydrolysis layer, polishing powder or crystal powder ultrasonic erosion in crystal scratch defects will be inserted and fall;
(4) chemically mechanical polishing: the silicon dioxide polishing solution that uses particle diameter to be 100nm on polyurethane polishing pad to polishing crystal 15 minutes, chemically mechanical polishing adopts twin shaft polishing machine, the speed of mainshaft of this twin shaft polishing machine is 30 revs/min, the balance staff rotating speed of twin shaft polishing machine is 12 revs/min, and remove remaining minute scratch marks within a short period of time does not affect crystal face type simultaneously;
(5) detect: crystal is placed in organic solvent hexamethyldisilane ultrasonic cleaning 60 seconds, with ultramicroscopic observation plane of crystal pattern;
(6) if plane of crystal no marking, then the crystal with the low sub-surface damage of super-smooth surface is obtained; If plane of crystal still has cut, repeat step (2) ~ (5), and the cerium oxide polishing slurry being 1 μm by particle diameter in step (2) changes the cerium oxide polishing slurry that average grain diameter is 300nm into.
Embodiment 4
Obtain a method for the low sub-surface damage crystal of super-smooth surface, the method comprises the following steps:
(1) grind: paste screening glass by around crystal, crystal paraffin is fixed on grinding tool, then crystal is clamped with clamping device, twin shaft fine grinding polish machine use boron carbide that specification is W1 as abrasive material, and coordinate cast iron plate to grind crystal, fast by the damage layer that the upper operation of removal is brought, make plane of crystal have good face type, flatness is up to standard;
(2) rough polishing: prepare pitch dish and after revising pitch card type, roughness, use particle diameter is that the cerium oxide polishing slurry of 1 μm carries out machine glazed finish to crystal until plane of crystal roughness reaches 1nm or basic no marking on pitch dish, wherein, the temperature of rough polishing remains on 19.5 ~ 20.5 DEG C, the time of rough polishing is 2.5 hours, be that the mass fraction of cerium oxide in the cerium oxide polishing slurry of 1 μm drops to 3% gradually by 6% by particle diameter in the process of polishing crystal, in the process of polishing crystal, pitch dish is trimmed simultaneously and makes the card of pitch dish smooth;
(3) etch: plane of crystal is immersed in organic solvent hexamethyldisilane, the temperature of organic solvent is 45 DEG C, utilize the ultrasonic process of ultrasonic washing instrument 45 seconds, to remove plane of crystal hydrolysis layer, polishing powder or crystal powder ultrasonic erosion in crystal scratch defects will be inserted and fall;
(4) chemically mechanical polishing: the silicon dioxide polishing solution that uses particle diameter to be 100nm on polyurethane polishing pad to polishing crystal 13 minutes, chemically mechanical polishing adopts twin shaft polishing machine, the speed of mainshaft of this twin shaft polishing machine is 30 revs/min, the balance staff rotating speed of twin shaft polishing machine is 12 revs/min, and remove remaining minute scratch marks within a short period of time does not affect crystal face type simultaneously;
(5) detect: crystal is placed in organic solvent hexamethyldisilane ultrasonic cleaning 45 seconds, with ultramicroscopic observation plane of crystal pattern;
(6) if plane of crystal no marking, then the crystal with the low sub-surface damage of super-smooth surface is obtained; If plane of crystal still has cut, repeat step (2) ~ (5), and the cerium oxide polishing slurry being 1 μm by particle diameter in step (2) changes the cerium oxide polishing slurry that particle diameter is 200nm into.
Claims (7)
1. obtain a method for the low sub-surface damage crystal of super-smooth surface, it is characterized in that, the method comprises the following steps:
(1) grind: use the boron carbide that specification is W1 to grind crystal on cast iron plate as abrasive material;
(2) rough polishing: use particle diameter is that the cerium oxide polishing slurry of 1 μm carries out polishing to crystal on pitch dish;
(3) etch: plane of crystal is immersed in organic solvent, ultrasonic process 30-60 second;
(4) chemically mechanical polishing: the silicon dioxide polishing solution that uses particle diameter to be 100nm on polyurethane polishing pad to polishing crystal 10 ~ 15 minutes;
(5) detect: crystal is placed in organic solvent for ultrasonic cleaning 30-60 second, with ultramicroscopic observation plane of crystal pattern;
(6) if plane of crystal no marking, then the crystal with the low sub-surface damage of super-smooth surface is obtained; If plane of crystal still has cut, repeat step (2) ~ (5), and the cerium oxide polishing slurry being 1 μm by particle diameter in step (2) changes the cerium oxide polishing slurry that particle diameter is 100-300nm into.
2. a kind of method obtaining the low sub-surface damage crystal of super-smooth surface according to claim 1; it is characterized in that; the concrete steps of the grinding described in step (1) comprise: paste screening glass by around crystal; then crystal is clamped with clamping device; twin shaft fine grinding polish machine uses boron carbide that specification is W1 as abrasive material, and coordinate cast iron plate to grind crystal.
3. a kind of method obtaining the low sub-surface damage crystal of super-smooth surface according to claim 1, is characterized in that, the temperature of the rough polishing described in step (2) is 19.5 ~ 20.5 DEG C, and the time of rough polishing is 2 ~ 3 hours.
4. a kind of method obtaining the low sub-surface damage crystal of super-smooth surface according to claim 1, it is characterized in that, in the process of the middle polishing crystal of step (2), be that the mass fraction of cerium oxide in the cerium oxide polishing slurry of 1 μm drops to 3% gradually by 6% by particle diameter.
5. a kind of method obtaining the low sub-surface damage crystal of super-smooth surface according to claim 1, is characterized in that, step (3) or the organic solvent described in step (5) are hexamethyldisilane.
6. a kind of method obtaining the low sub-surface damage crystal of super-smooth surface according to claim 1, is characterized in that, the temperature of the organic solvent described in step (3) is 40 ~ 50 DEG C.
7. a kind of method obtaining the low sub-surface damage crystal of super-smooth surface according to claim 1, it is characterized in that, chemically mechanical polishing described in step (4) adopts twin shaft polishing machine, the speed of mainshaft of this twin shaft polishing machine is 30 revs/min, and the balance staff rotating speed of twin shaft polishing machine is 12 revs/min.
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| CN109623581A (en) * | 2019-01-04 | 2019-04-16 | 芜湖启迪半导体有限公司 | A kind of surface polishing method of hard material |
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| CN103882378B (en) * | 2014-02-13 | 2015-12-09 | 同济大学 | A kind of preparation method of three boracic acid oxygen calcium yttrium crystal (YCOB) high laser damage threshold anti-reflection films |
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| CN109590820B (en) * | 2019-01-02 | 2021-07-06 | 中国科学院上海光学精密机械研究所 | Method for processing surface roughness of superhard laser crystal |
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| CN115181498A (en) * | 2022-06-29 | 2022-10-14 | 大连理工大学 | Polishing solution for KDP crystal and efficient grinding and polishing process |
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