CN105922083B - The surface polishing method of potassium dihydrogen phosphate crystalloid - Google Patents
The surface polishing method of potassium dihydrogen phosphate crystalloid Download PDFInfo
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- CN105922083B CN105922083B CN201610271922.5A CN201610271922A CN105922083B CN 105922083 B CN105922083 B CN 105922083B CN 201610271922 A CN201610271922 A CN 201610271922A CN 105922083 B CN105922083 B CN 105922083B
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- dihydrogen phosphate
- potassium dihydrogen
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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
Abstract
The present invention relates to the surface polishing method of potassium dihydrogen phosphate crystalloid.Surface roughness existing for the surface polishing technique of existing potassium dihydrogen phosphate crystalloid is high, brings damage or impurity insertion, potassium dihydrogen phosphate crystalloid surface the problems such as periodicity tool marks ripple to be present to potassium dihydrogen phosphate crystalloid surface.The present invention is in one layer of planarization layer of potassium dihydrogen phosphate crystalloid surface spin coating, its surface roughness is set to be less than 1.5nm, then Low Temperature Heat Treatment certain time is carried out, it is put into vacuum chamber, utilize ion beam polishing, until removing surface planarisation layer completely, the smooth surface of planarization layer is delivered to potassium dihydrogen phosphate crystalloid surface, obtain the super-smooth surface of potassium dihydrogen phosphate crystalloid.Without mechanical machining stress in the technology process, material removal amount can control atom magnitude in polishing process, can reach very high polishing effect.
Description
Technical field
The present invention relates to Ultraprecision Machining field, and in particular to a kind of surface polishing side of potassium dihydrogen phosphate crystalloid
Method.
Background technology
Potassium dihydrogen phosphate（KDP）Crystalloid is a kind of high-quality non-linear optical crystal material, while is had preferably non-
Linear coefficient and higher laser damage threshold, thus do frequency doubling device and optoelectronic switch with it extensively in laser aid.
Especially played in the high-tech key equipments such as inertial confinement fusion solid state laser facility, light laser weapon extremely important
Effect.In the optical element used in these key equipments, large scale, high-precision high-quality KDP are widely used in high power
In the light path system of solid state laser etc..
Due to potassium dihydrogen phosphate（KDP）Crystalloid has the characteristics that soft, crisp, easy deliquescence, to temperature change sensitivity, to high-quality
The processing request of amount brings great difficulty, is acknowledged as one of most unmanageable optical element at present.To potassium dihydrogen phosphate
（KDP）Crystalloid optical crystal part, if surface roughness does not reach requirement, the thang-kng performance of part is not only influenced whether,
High power laser light is caused to scatter, so that laser output energy and energy density are low during laser target shooting, and will not meeting
Plated film will be such that the anti-light laser damage capability of film layer weakens significantly on the roughness surface asked, so as to reduce the broken of film layer and material
Bad threshold value, cause the heavy caliber potassium dihydrogen phosphate of a large amount of costlinesses（KDP）Crystalloid element material and film layer are destroyed.
Domestic and international application is in potassium dihydrogen phosphate at present（KDP）The precision machined technology of crystalloid mainly has single-point diamond car
Cut, superfine grinding, MRF（MRF）And potassium dihydrogen phosphate（KDP）Crystalloid deliquescence polishes.Due to potassium dihydrogen phosphate
（KDP）The characteristics such as soft, crisp, the easy deliquescence of crystalloid, make above-mentioned process technology and method all inevitably to potassium dihydrogen phosphate
（KDP）Crystalloid surface bring damage or impurity insertion, and be extremely difficult to inertial confinement fusion solid state laser facility,
The roughness required in the high-tech key equipment such as light laser weapon in use is less than 1.5nm requirement.List the most frequently used at present
Point diamond turning, its plane of crystal roughness after processing typically is above 2nm, but also periodic tool marks be present
Ripple, these will all have a strong impact on potassium dihydrogen phosphate（KDP）Other optical characteristics such as the laser damage threshold of crystalloid.
PC3-1500 planarization glue is nonphotosensitive smoothing material, is mainly used in provisional adhesion, base between substrate
Mechanical protection is handled when piece surface large area planarization process and substrate are cut.It is thinned after being separated with chip and is easy at back
Removed in remover RD3 or RD6.Its main advantage is superior planarization process ability.Primary solvent is butyl acetate,
The thickness of planarization layer can be adjusted by the solvent in an experiment.
The content of the invention
It is an object of the invention to provide a kind of surface polishing method of potassium dihydrogen phosphate crystalloid, prior art is overcome to exist
Surface roughness it is high, to potassium dihydrogen phosphate（KDP）Bring damage or impurity insertion, potassium dihydrogen phosphate in crystalloid surface（KDP）
The problems such as periodicity tool marks ripple be present in crystalloid surface.
The technical solution adopted in the present invention is：
The surface polishing method of potassium dihydrogen phosphate crystalloid, it is characterised in that：
Realized by following steps：
Step 1: in potassium dihydrogen phosphate crystalloid sample surfaces one layer of planarization layer of spin coating, handled by planarization
Afterwards, the surface roughness of sample is less than 1.5nm；
Step 2: the potassium dihydrogen phosphate crystalloid sample after planarization process is placed in vacuum heat treatment furnace, vacuum
Pressure is less than 1Pa, heat treatment time 1-5 hours, and heat treatment temperature is less than 80 DEG C, and heat treatment is naturally cold in a vacuum chamber after terminating
But to room temperature, potassium dihydrogen phosphate crystalloid sample is taken out；
Step 3: potassium dihydrogen phosphate crystalloid sample is fixed on the fixture of ion beam etching system, adjustment fixture with
Angle between ion beam incidence, scope are 30 ° to 60 °；
Step 4: pressure in vacuum tank is extracted into less than 5 × 10 using vacuum system-4Pa vacuum, quarter is passed through in proportion
Erosion, the working gas of reaction, including argon gas and oxygen, its O2 to Ar ratio scope are 0:13.2 to 6:7.2, gas flow total amount
13.2sccm, vacuum control valve is adjusted, pressure in vacuum tank is maintained at 2 × 10-2Pa to 8 × 10-2Pa；
Step 5: the rotational velocity of alignment jig, is controlled in the range of 5r/min to 30r/min, make potassium dihydrogen phosphate class
Crystal prototype and fixture together rotation, to eliminate the inhomogeneities of ion beam；
Step 6: regulation ion source discharge technological parameter, makes ion beam to planarization layer and potassium dihydrogen phosphate crystalloid material
Material has identical etch rate；
Step 7: opening potassium dihydrogen phosphate crystalloid sample baffle plate, ion beam is set to perform etching polishing to it, until completely
Planarization layer is removed, the super-smooth surface of planarization layer is transferred on potassium dihydrogen phosphate crystalloid；
Step 8：Wait 2 hours, when sample temperature is down to room temperature, take out sample.
Step 1 is using PC3-1500 glue as planarization layer.
In step 6, ion source discharge technological parameter is：Ion energy 200eV to 800eV, ion beam line 10mA are arrived
50mA。
The present invention has advantages below：
1. it is to be based on atom sputtering effect that material, which removes Physical Mechanism, material removal amount can control original in polishing process
Sub- magnitude, reach very high polishing precision, the potassium dihydrogen phosphate after polishing（KDP）Crystalloid can reach super-smooth surface.
2. contact stress and strain are not present in polishing process, therefore workpiece face shape is good after processing, surface texture is good.
3. impurity will not be introduced after present invention polishing.
4. the present invention is applicable not only to potassium dihydrogen phosphate（KDP）The polishing of crystalloid material, if the suitable planarization of selection
Layer and ion beam technology parameter, apply also for the polishing of other materials.
Brief description of the drawings
Fig. 1 is each stage schematic diagram in polishing process of the invention.
Wherein, a is KDP plane of crystal primary morphologies, and b is the surface topography that spin coating planarizes thickness, during c is broken closes
Pattern, d be completely remove planarize thickness KDP plane of crystal patterns.
Fig. 2 is the schematic diagram of polissoir.
Fig. 3 is the potassium dihydrogen phosphate after polishing（KDP）Crystalloid surface roughness test result figure.
Embodiment
With reference to embodiment, the present invention will be described in detail.
The surface polishing method of potassium dihydrogen phosphate crystalloid of the present invention, it is potassium dihydrogen phosphate（KDP）Crystalloid
Flattening method and planarization layer and potassium dihydrogen phosphate（KDP）The constant speed lithographic technique of crystalloid material, can realize di(2-ethylhexyl)phosphate
Hydrogen potassium（KDP）The high quality polished effect on crystalloid surface, roughness can be less than 1.5nm.It is specifically real by following steps
It is existing：
Step 1: in potassium dihydrogen phosphate crystalloid sample surfaces one layer of planarization layer of spin coating, handled by planarization
Afterwards, the surface roughness of sample is less than 1.5nm；
Step 2: the potassium dihydrogen phosphate crystalloid sample after planarization process is placed in vacuum heat treatment furnace, vacuum
Pressure is less than 1Pa, heat treatment time 1-5 hours, and heat treatment temperature is less than 80 DEG C, and heat treatment is naturally cold in a vacuum chamber after terminating
But to room temperature, potassium dihydrogen phosphate crystalloid sample is taken out；
Step 3: potassium dihydrogen phosphate crystalloid sample is fixed on the fixture of ion beam etching system, adjustment fixture with
Angle between ion beam incidence, scope are 30 ° to 60 °；
Step 4: pressure in vacuum tank is extracted into less than 5 × 10 using vacuum system-4Pa vacuum, quarter is passed through in proportion
Erosion, the working gas of reaction, including argon gas and oxygen, its O2 to Ar ratio scope are 0:13.2 to 6:7.2, gas flow total amount
13.2sccm, vacuum control valve is adjusted, pressure in vacuum tank is maintained at 2 × 10-2Pa to 8 × 10-2Pa；
Step 5: the rotational velocity of alignment jig, is controlled in the range of 5r/min to 30r/min, make potassium dihydrogen phosphate class
Crystal prototype and fixture together rotation, to eliminate the inhomogeneities of ion beam；
Step 6: regulation ion source discharge technological parameter, makes ion beam to planarization layer and potassium dihydrogen phosphate crystalloid material
Material has identical etch rate；
Step 7: opening potassium dihydrogen phosphate crystalloid sample baffle plate, ion beam is set to perform etching polishing to it, until completely
Planarization layer is removed, the super-smooth surface of planarization layer is transferred on potassium dihydrogen phosphate crystalloid；
Step 8：Wait 2 hours, when sample temperature is down to room temperature, take out sample.
Step 1 is using PC3-1500 glue as planarization layer.
In step 6, ion source discharge technological parameter is：Ion energy 200eV to 800eV, ion beam line 10mA are arrived
50mA。
Embodiment：
In one layer of PC3-1500 planarization layer of KDP planes of crystal spin coating, have sacrifice layer after planarization is handled
There is super-smooth surface；KDP crystal prototypes after planarization process are placed in vacuum heat treatment furnace, vacuum pressure 0.1Pa, heat
4 hours processing times, 75 DEG C of heat treatment temperature, heat treatment naturally cool to room temperature in a vacuum chamber after terminating, take out KDP samples
Product；KDP samples are fixed on the fixture of ion beam etching system, it is 45 ° to adjust the angle between fixture and ion beam incidence；
Pressure in vacuum tank is extracted into less than 5 × 10 using vacuum system-4Pa vacuum, is passed through working gas：Argon gas 12.2sccm, oxygen
Gas 1sccm, vacuum control valve is adjusted, pressure in vacuum tank is maintained at 5 × 10-2Pa；It is 15r/min to control fixture rotational velocity；
It is ion beam energy 400eV, ion beam line 35mA to adjust ion gun running parameter；Baffle plate is opened, ion beam is carried out it
Etching polishing, until removing planarization layer completely, the super-smooth surface of planarization layer is transferred on KDP；Wait 2 hours, treat
When sample temperature is down to room temperature, sample is taken out；Test sample surface roughness Sq is 1.3574nm.
Present disclosure is not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And any equivalent conversion taken technical solution of the present invention, it is that claim of the invention is covered.
Claims (3)
1. the surface polishing method of potassium dihydrogen phosphate crystalloid, it is characterised in that：
Realized by following steps：
Step 1: in potassium dihydrogen phosphate crystalloid sample surfaces one layer of planarization layer of spin coating, after planarization is handled, sample
The surface roughness of product is less than 1.5nm；
Step 2: the potassium dihydrogen phosphate crystalloid sample after planarization process is placed in vacuum heat treatment furnace, vacuum pressure
Less than 1Pa, heat treatment time 1-5 hours, heat treatment temperature is less than 80 DEG C, and heat treatment naturally cools in a vacuum chamber after terminating
Room temperature, take out potassium dihydrogen phosphate crystalloid sample；
Step 3: potassium dihydrogen phosphate crystalloid sample is fixed on the fixture of ion beam etching system, fixture and ion are adjusted
Angle between beam incidence, scope are 30 ° to 60 °；
Step 4: pressure in vacuum tank is extracted into less than 5 × 10 using vacuum system-4Pa vacuum, etching, anti-is passed through in proportion
The working gas answered, including argon gas and oxygen, its O2 to Ar ratio scope are 0:13.2 to 6:7.2, gas flow total amount 13.2sccm,
Vacuum control valve is adjusted, pressure in vacuum tank is maintained at 2 × 10-2Pa to 8 × 10-2Pa；
Step 5: the rotational velocity of alignment jig, is controlled in the range of 5r/min to 30r/min, make potassium dihydrogen phosphate crystalloid
Sample and fixture together rotation, to eliminate the inhomogeneities of ion beam；
Step 6: regulation ion source discharge technological parameter, makes ion beam have planarization layer and potassium dihydrogen phosphate crystalloid material
There is identical etch rate；
Step 7: opening potassium dihydrogen phosphate crystalloid sample baffle plate, ion beam is set to perform etching polishing to it, until removing completely
Planarization layer, the super-smooth surface of planarization layer is transferred on potassium dihydrogen phosphate crystalloid；
Step 8：Wait 2 hours, when sample temperature is down to room temperature, take out sample.
2. the surface polishing method of potassium dihydrogen phosphate crystalloid according to claim 1, it is characterised in that：
Step 1 is using PC3-1500 glue as planarization layer.
3. the surface polishing method of potassium dihydrogen phosphate crystalloid according to claim 1, it is characterised in that：
In step 6, ion source discharge technological parameter is：Ion energy 200eV to 800eV, ion beam line 10mA to 50mA.
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| CN106683998A (en) * | 2016-11-28 | 2017-05-17 | 中国电子科技集团公司第四十八研究所 | Flexible substrate pretreatment process |
| CN106835035B (en) * | 2017-04-21 | 2019-01-18 | 西安工业大学 | A kind of method of potassium dihydrogen phosphate crystalloid optical surface planarization |
| CN107052929A (en) * | 2017-05-18 | 2017-08-18 | 深圳市瑞德森智能设备有限责任公司 | Composite ceramics turning blank and preparation method thereof |
| CN107053486B (en) * | 2017-05-18 | 2019-11-12 | 深圳市瑞德森智能设备有限责任公司 | Composite ceramics turning blank and preparation method thereof |
| CN107052913B (en) * | 2017-05-31 | 2018-10-30 | 西安工业大学 | RB-SiC optical element polishing process processing methods |
| WO2020225225A1 (en) * | 2019-05-06 | 2020-11-12 | Leibniz Institut Für Oberflächenmodifizierung E.V. | Method for smoothing surfaces |
| CN111257077B (en) * | 2020-02-28 | 2023-06-02 | 西安工业大学 | Method and device for preparing lithium niobate nano dot domain structure by ion beam irradiation |
| CN111257078B (en) * | 2020-02-28 | 2023-06-02 | 西安工业大学 | Method and device for preparing lithium niobate nano domain structure by ion beam irradiation |
| CN112171205B (en) * | 2020-09-28 | 2022-01-11 | 湖南天创精工科技有限公司 | Ion beam assisted aluminum alloy reflector processing method |
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