CN106826409A - A kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound - Google Patents
A kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound Download PDFInfo
- Publication number
- CN106826409A CN106826409A CN201710070811.2A CN201710070811A CN106826409A CN 106826409 A CN106826409 A CN 106826409A CN 201710070811 A CN201710070811 A CN 201710070811A CN 106826409 A CN106826409 A CN 106826409A
- Authority
- CN
- China
- Prior art keywords
- calcium fluoride
- polishing
- mono crystal
- fluoride mono
- crystal
- 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.)
- Granted
Links
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- 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
- B24B13/00—Machines or devices designed for grinding or polishing optical surfaces on lenses or surfaces of similar shape on other work; Accessories therefor
-
- 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
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- 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
- C09G1/06—Other polishing compositions
- C09G1/14—Other polishing compositions based on non-waxy substances
- C09G1/18—Other polishing compositions based on non-waxy substances on other substances
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound, comprise the following steps：Treatment is ground to calcium fluoride mono crystal；The calcium fluoride mono crystal after grinding is polished using the first polishing fluid, and ultrasonic wave cleaning is carried out to calcium fluoride mono crystal to set interval time in polishing process；First polishing fluid is the alkalescence polishing liquid being made up of the nanometer grade silica polishing powder mixed with nanoscale aluminium salt, nanoscale chromium and nanometer ferro oxide；It is polished on optics pitch mould using the second polishing fluid.The present invention adds the cmp method of the compounds such as aluminium salt to be polished calcium fluoride mono crystal using in polishing fluid, a small amount of aluminium salt and chromium oxide etc. can produce complex compound with calcium fluoride mono crystal in the basic conditions, thus accelerate the polishing process to calcium fluoride mono crystal, so as to further remove calcium fluoride mono crystal surface damage and sub-surface damage, obtain more smooth plane of crystal so that high in machining efficiency, the good product quality of calcium fluoride mono crystal.
Description
Technical field
The present invention relates to calcium fluoride crystal processing technique field, more particularly, to a kind of calcirm-fluoride based on aluminium salt complex compound
Monocrystalline polishing method.
Background technology
In recent years, monocrystal material already occupied consequence with its excellent combination property, and particularly some are high-precision
Spend, high-quality artificial single crystal receives the favor of various aspects researcher, wherein calcirm-fluoride (Calcium
Fluoride, CaF2) monocrystalline (as shown in Figure 1) is even more outstanding person therein, its transmission range is (125nm~10 μm) wide, has
Excellent achromatism and apochromatism ability, excellent mechanical performance and metastable physical and chemical performance, are widely used in system
Make the optical elements such as lens, prism and window.Particularly in ultraviolet optics system, the excellent UV-permeable of calcium fluoride mono crystal
Property, shortwave tolerance high, phenomenon free of birefringence, high transmissivity, refractive index homogeneity and low birefringence, as photoetching
The first-selected lens material of system and high energy laser system.High energy laser system requirements optical element has damage from laser high
Threshold value and transmission performance, this requires that calcium fluoride mono crystal has nano level roughness, the flatness of submicron order, high integrality
Surface.
However, calcium fluoride mono crystal has the characteristics such as low, broken hardness, anisotropy, thermal coefficient of expansion higher, therefore
Process technology requirement to calcirm-fluoride is more increased, and difficulty of processing is larger, to realize the Precision Machining of calcium fluoride mono crystal, traditional crystalline substance
Body processing method can cause that calcium fluoride mono crystal surface produces surface and the sub-surface damages such as cut, therefore reduce calcium fluoride mono crystal table
The damage in face is accomplished by improving constantly the level of processing of calcium fluoride mono crystal.
The content of the invention
The purpose of the present invention is exactly to provide a kind of based on aluminium salt complexing for the defect for overcoming above-mentioned prior art to exist
The cmp method of thing, reduces the surface damage and sub-surface damage produced when calcium fluoride mono crystal is processed, and obtains quality
Good, practicality calcium fluoride mono crystal high.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound, comprises the following steps：
1) treatment is ground to calcium fluoride mono crystal；
2) calcium fluoride mono crystal after grinding is polished using the first polishing fluid, and setting interval in polishing process
Time carries out ultrasonic wave cleaning to calcium fluoride mono crystal；
First polishing fluid is by the nanoscale two mixed with nanoscale aluminium salt, nanoscale chromium and nanometer ferro oxide
The alkalescence polishing liquid that silica polishing powder is made；
3) calcium fluoride mono crystal is polished on optics pitch mould using the second polishing fluid, second polishing fluid is nothing
Water-ethanol and ether mixed liquor.
Further, the step 1) it is specially：
A, respectively use 302# and 303# sand paper are roughly ground to calcium fluoride mono crystal；
B, calcium fluoride mono crystal is refined with the diamond abrasive cream of 1500# and 2500#；
C, abrasive material is made of the bortz powder of W1 and W0.5 essence is carried out again to calcium fluoride mono crystal on polyamino resin polishing pad
Mill, while using ionized water as lapping liquid.
Further, in first polishing fluid, the mass percent of nanoscale aluminium chloride is less than 2.5%, nanoscale oxygen
The mass percent for changing chromium is 0.1%, and the mass percent of nanometer ferro oxide is 0.2%.
Further, the ultrasonic wave cleaning is specially：Use frequency for 30KHZ, 40KHZ, 50KHZ and 80KHZ not
Ultrasonic wave cleaning is carried out to calcium fluoride mono crystal with ultrasonic wave is combined.
Further, the step 3) in, optics pitch mould is to add to have mass percent less than the 55# of 0.5% rosin
Pitch mould.
Further, the temperature of polishing process is 20-21 DEG C, and humidity is less than 40%, and the pH value of the first polishing fluid is 9-11.
Compared with prior art, the present invention has advantages below：
1st, the present invention is using by the nanoscale titanium dioxide mixed with nanoscale aluminium salt, nanoscale chromium and nanometer ferro oxide
The alkalescence polishing liquid that silicon polishing powder is made can produce complex compound to polishing crystal in polishing process, so as to accelerate calcirm-fluoride list
Brilliant polishing process, improves polishing precision, polishing efficiency, product quality in polishing process.
2nd, with the bortz powder of W1 and W0.5 on polyamino resin polishing pad to crystal grind can effectively remove line and
Modification aperture.
3rd, ultrasonic wave cleaning is carried out to calcium fluoride mono crystal can dissolve surface hydrolysis layer so as to remove more polishing fluids
Impurity.
4th, it is blended in using absolute ethyl alcohol and ether and is dripped less than the 55# after 0.5% Abietyl modified treatment through mass percent
Blue or green mould polishing, can further correct the face shape error of calcium fluoride mono crystal, and it is to adjust the hardness of pitch lacquer disk(-sc) to add rosin
The polishing for making it be applied to calcirm-fluoride.
5th, polishing method of the present invention can remove surface that tradition machinery polishing method produces on calcium fluoride mono crystal surface and
Some produced on calcium fluoride mono crystal surface when sub-surface damage, surface and sub-surface damage refer to tradition machinery grinding and polishing are drawn
Micro- broken, the surface impurity insertion defect of trace, fragility.
Brief description of the drawings
Fig. 1 is calcium fluoride crystal and its crystal structure figure；
Fig. 2 is schematic flow sheet of the invention；
Fig. 3 is chemically mechanical polishing principle schematic；
Fig. 4 is calcium fluoride mono crystal surface (a) and sub-surface (b) after mechanical rough polishing under light microscope；
Subsurface microscopy pattern after Fig. 5 chemically mechanical polishings；
Plane of crystal quality after Fig. 6 chemically mechanical polishings.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, give detailed implementation method and specific operating process, but protection scope of the present invention is not limited to
Following embodiments.
The present embodiment with diameter 110mm (effective aperture 90mm), thickness 12mm calcirm-fluoride flat work pieces as processing object
Calcium fluoride mono crystal polishing method of the present invention based on aluminium salt complex compound is illustrated, as shown in Fig. 2 detailed process is：
In step S101, calcium fluoride mono crystal is roughly ground with 302#, 303# sand paper respectively first, secondly with 1500# and
The diamond abrasive cream of 2500# is refined to calcium fluoride mono crystal, can greatly reduce the time of follow-up polishing, improves processing efficiency, is connect
And do abrasive material with W1 and W0.5 bortz powders calcium fluoride mono crystal is ground on polyamino resin polishing pad, used in process of lapping
Deionized water cooks lapping liquid, and grinding now obtains the calcium fluoride mono crystal with certain surface figure accuracy after a period of time, but can be
Calcium fluoride mono crystal surface forms hydrolysis layer, and has impurity particle insertion calcium fluoride mono crystal surface, and Fig. 4 is fluorine after mechanical rough polishing
Change the image that calcium single-crystal surface and sub-surface are observed under an optical microscope.
In step s 102, adding nanoscale aluminium chloride in alkalescence polishing liquid that nanometer grade silica is main abrasive material
(mass percent is less than 2.5%), nanoscale chromium (mass percent is 0.1%) and nanometer ferro oxide (quality percentage
Than for 0.2%), being configured to alkalescence polishing liquid with this and calcium fluoride crystal being polished, because adding a small amount of aluminium salt (chlorine in polishing fluid
Change aluminium), chromium oxide, the abrasive material such as iron oxide, and polishing fluid is alkaline solution, and complex compound is formed so as to have in aluminium salt in polishing process
Help accelerate polishing crystal process, its chemically mechanical polishing operation principle is as shown in Figure 3.
In step s 103, at regular intervals with absolute ethyl alcohol and ether mixed liquor to calcium fluoride mono crystal in polishing process
Ultrasonic wave cleaning is carried out, wherein combined to calcirm-fluoride using the ultrasonic wave of 30KHZ, 40KHZ, 50KHZ and 80KHZ different frequency
Carry out ultrasonic wave cleaning, in order to remove surface hydrolysis layer, and be embedded in the polishing fluid impurity under hydrolysis layer.
In step S104, the polished die of the present embodiment is 55# pitch moulds, and it adds mass percent less than 0.5% pine
The fragrant hardness to change abrasive disk, in order to further eliminate sub-surface damage layer, in addition it is also necessary on pitch mould with absolute ethyl alcohol and
Ether mixed liquor carries out last time polishing to calcirm-fluoride.
Through the initial CaF after mechanical polishing process2Workpiece surface is formed with substantial amounts of surface and sub-surface damage (Fig. 4),
As chemically mechanical polishing is constantly carried out, the cut for occurring before is gradually become shallower as and attenuates, and surface roughness is reduced, when removing completely
When calcium fluoride mono crystal surface damage layer and sub-surface damage layer, preferable atomic layer is just exposed, and understands to throw from Fig. 5 and Fig. 6
The calcium fluoride crystal with certain surface figure accuracy has been obtained after light.
To sum up, processed by the present embodiment, finally obtained the calcium fluoride crystal surface of ultra-smooth, illustrate that the above method can be with
Realize the Precision Machining of calcium fluoride mono crystal.
Part that the present invention does not relate to is same as the prior art or can be realized using prior art.
Preferred embodiment of the invention described in detail above.It should be appreciated that one of ordinary skill in the art without
Need creative work just can make many modifications and variations with design of the invention.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical scheme, all should be in the protection domain being defined in the patent claims.
Claims (6)
1. a kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound, it is characterised in that comprise the following steps：
1) treatment is ground to calcium fluoride mono crystal；
2) calcium fluoride mono crystal after grinding is polished using the first polishing fluid, and setting interval time in polishing process
Ultrasonic wave cleaning is carried out to calcium fluoride mono crystal；
First polishing fluid is by the nanoscale titanium dioxide mixed with nanoscale aluminium salt, nanoscale chromium and nanometer ferro oxide
The alkalescence polishing liquid that silicon polishing powder is made；
3) calcium fluoride mono crystal is polished on optics pitch mould using the second polishing fluid, second polishing fluid is anhydrous second
Alcohol and ether mixed liquor.
2. the calcium fluoride mono crystal polishing method based on aluminium salt complex compound according to claim 1, it is characterised in that the step
It is rapid 1) to be specially：
A, respectively use 302# and 303# sand paper are roughly ground to calcium fluoride mono crystal；
B, calcium fluoride mono crystal is refined with the diamond abrasive cream of 1500# and 2500#；
C, abrasive material is made of the bortz powder of W1 and W0.5 calcium fluoride mono crystal is ground again on polyamino resin polishing pad, together
Shi Caiyong ionized waters are used as lapping liquid.
3. the calcium fluoride mono crystal polishing method based on aluminium salt complex compound according to claim 1, it is characterised in that described
In one polishing fluid, the mass percent of nanoscale aluminium chloride is less than 2.5%, and the mass percent of nanoscale chromium is 0.1%,
The mass percent of nanometer ferro oxide is 0.2%.
4. the calcium fluoride mono crystal polishing method based on aluminium salt complex compound according to claim 1, it is characterised in that described super
Sound wave cleaning is specially：Use frequency combined to calcirm-fluoride list for the different ultrasonic waves of 30KHZ, 40KHZ, 50KHZ and 80KHZ
Crystalline substance carries out ultrasonic wave cleaning.
5. the calcium fluoride mono crystal polishing method based on aluminium salt complex compound according to claim 1, it is characterised in that the step
It is rapid 3) in, optics pitch mould be add have mass percent less than 0.5% rosin 55# pitch moulds.
6. the calcium fluoride mono crystal polishing method based on aluminium salt complex compound according to claim 1, it is characterised in that polished
The temperature of journey is 20-21 DEG C, and humidity is less than 40%, and the pH value of the first polishing fluid is 9-11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710070811.2A CN106826409B (en) | 2017-02-09 | 2017-02-09 | A kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710070811.2A CN106826409B (en) | 2017-02-09 | 2017-02-09 | A kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106826409A true CN106826409A (en) | 2017-06-13 |
| CN106826409B CN106826409B (en) | 2018-05-08 |
Family
ID=59121649
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710070811.2A Expired - Fee Related CN106826409B (en) | 2017-02-09 | 2017-02-09 | A kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106826409B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110576342A (en) * | 2018-07-17 | 2019-12-17 | 蓝思科技（长沙）有限公司 | Polishing method for improving surface shape precision yield of glass mirror, camera and electronic equipment |
| CN111638305A (en) * | 2020-06-08 | 2020-09-08 | 郑州磨料磨具磨削研究所有限公司 | Method for determining optimal processing direction of single crystal material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001000907A1 (en) * | 1999-06-25 | 2001-01-04 | Corning Incorporated | Polishing of fluoride crystal optical lenses and preforms using cerium oxide for microlithography |
| EP1372010A2 (en) * | 2002-06-13 | 2003-12-17 | Canon Kabushiki Kaisha | Method for manufacturing optical element |
| CN102896558A (en) * | 2012-10-17 | 2013-01-30 | 中国人民解放军国防科学技术大学 | Calcium fluoride single crystal ultra-precision machining method based on chemico-mechanical polishing and ion beam polishing combined process |
| CN105269412A (en) * | 2015-09-17 | 2016-01-27 | 中国科学院光电技术研究所 | Combined technology method suitable for efficient processing of calcium fluoride convex cone mirror |
-
2017
- 2017-02-09 CN CN201710070811.2A patent/CN106826409B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001000907A1 (en) * | 1999-06-25 | 2001-01-04 | Corning Incorporated | Polishing of fluoride crystal optical lenses and preforms using cerium oxide for microlithography |
| EP1372010A2 (en) * | 2002-06-13 | 2003-12-17 | Canon Kabushiki Kaisha | Method for manufacturing optical element |
| CN102896558A (en) * | 2012-10-17 | 2013-01-30 | 中国人民解放军国防科学技术大学 | Calcium fluoride single crystal ultra-precision machining method based on chemico-mechanical polishing and ion beam polishing combined process |
| CN105269412A (en) * | 2015-09-17 | 2016-01-27 | 中国科学院光电技术研究所 | Combined technology method suitable for efficient processing of calcium fluoride convex cone mirror |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110576342A (en) * | 2018-07-17 | 2019-12-17 | 蓝思科技（长沙）有限公司 | Polishing method for improving surface shape precision yield of glass mirror, camera and electronic equipment |
| CN111638305A (en) * | 2020-06-08 | 2020-09-08 | 郑州磨料磨具磨削研究所有限公司 | Method for determining optimal processing direction of single crystal material |
| CN111638305B (en) * | 2020-06-08 | 2023-09-22 | 郑州磨料磨具磨削研究所有限公司 | Method for determining optimal processing direction of monocrystalline material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106826409B (en) | 2018-05-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5664471B2 (en) | Method for producing synthetic quartz glass substrate for semiconductor | |
| CN107378654B (en) | A kind of polishing method of lithium tantalate wafer | |
| CN109545680B (en) | Rapid preparation method of high-flatness and low-damage monocrystalline silicon carbide substrate | |
| CN103252708B (en) | Based on the ultraprecise processing method of the Sapphire Substrate of concretion abrasive polishing pad | |
| KR102471865B1 (en) | High-flatness, low-damage and large-diameter monocrystalline silicon carbide substrate, and manufacturing method therefor | |
| CN1833816A (en) | Nano-glass supersmooth processing technique of sapphire crystal sheet | |
| CN102896558A (en) | Calcium fluoride single crystal ultra-precision machining method based on chemico-mechanical polishing and ion beam polishing combined process | |
| CN106826409B (en) | A kind of calcium fluoride mono crystal polishing method based on aluminium salt complex compound | |
| CN102172879A (en) | Method for processing soft and crisp LBO crystals based on consolidated abrasive polishing pad | |
| CN104044015A (en) | Lens processing process | |
| CN100443260C (en) | Scatheless grinding method for rigid, fragile crystal wafer | |
| CN110744364A (en) | Double-side polishing method for large-size ultrathin lithium niobate substrate | |
| CN102172859B (en) | Processing method for ultrathin plain glass based on consolidated abrasive | |
| Li et al. | Influence of acid slurries on surface quality of LBO crystal in fixed abrasive CMP | |
| JP2007284341A (en) | Methods for production of glass substrate for mask blank, mask blank, transfer mask, semiconductor device, glass substrate for mask blank, and mask blank and transfer mask | |
| JP2005298312A (en) | Microprocessing method for glass and microprocessed glass | |
| Hallock et al. | Recent advances in deterministic low-cost finishing of sapphire windows | |
| CN106433478B (en) | One kind being suitable for CaF2The magnetic fluid polishing fluid and preparation method of material Ultra-smooth machining | |
| JP2009087439A (en) | Manufacturing method of glass substrate for magnetic disk | |
| CN116460667B (en) | Processing method of calcium fluoride optical part | |
| JP3329594B2 (en) | Method of manufacturing sapphire substrate for photomask | |
| Zhang et al. | The wear behavior and lapping performance of fixed abrasive pad for acidity and alkalinity of lapping fluid in lapping quartz glass | |
| JP2006196144A (en) | Glass substrate for magnetic disk and its production method | |
| Li et al. | Effect of FAP characteristics on fixed abrasive polishing of CaF2 crystal | |
| JP6208565B2 (en) | Polishing carrier manufacturing method, magnetic disk substrate manufacturing method, and magnetic disk glass substrate manufacturing method |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180508 Termination date: 20210209 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |