CN103422170A - Disc-shaped MgF2 crystal filming material and production method thereof - Google Patents
Disc-shaped MgF2 crystal filming material and production method thereof Download PDFInfo
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- CN103422170A CN103422170A CN2013103238784A CN201310323878A CN103422170A CN 103422170 A CN103422170 A CN 103422170A CN 2013103238784 A CN2013103238784 A CN 2013103238784A CN 201310323878 A CN201310323878 A CN 201310323878A CN 103422170 A CN103422170 A CN 103422170A
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Abstract
The invention relates to the field of optical filming materials, particularly to a disc-shaped MgF2 crystal filming material and a production method thereof. The disc-shaped MgF2 crystal filming material is characterized in that the material is a colorless and transparent polycrystal optical crystal; at the position that the wave length is 500 mm, the refractive index Ne is equal to 1.38, and the material density is about 3.17 g/cm<3>, the material is designed and processed to be disc-shaped, conical or cylindrical, and the diameter and depth of the material are applicable to crucibles or crucible linings of electronic guns with various specifications, wherein the diameter ranges 20mm to 56 mm, and the thickness ranges between 5mm to 30 mm. Compared with the prior art, the disc-shaped MgF2 crystal filming material has the following benefits: the size requirement for MgF2-plated crucible of the electronic gun is fully met; material feeding and taking are very convenient; excellent evaporation characteristics of no splashing, no point collapsing, no gas discharging, and a flat evaporation surface are provided; the surface smoothness of a to-be-plated optical element is effectively improved; the disc-shaped MgF2 crystal filming material is particularly suitable for surface coating of super-smooth optical elements needing higher filming requirements.
Description
Technical field
The present invention relates to the optical filming material field, relate in particular to a kind of disc magnesium fluoride MgF
2Crystal coating material and production method thereof.
Background technology
MgF
2Splashing and collapsing a phenomenon in vacuum plating can have a strong impact on the smooth finish surperficial by light-plated, and this is to be difficult to the global problem thoroughly solved always.The eighties latter stage, Britain and Germany, successively by advanced synthetic method of purification, prepare white powder MgF
2, its chemical purity is 99.99%, has basically solved MgF
2The excessive spatter of plated film, collapse a problem, but this Powdered MgF
2Be only applicable to the resistance-type evaporation in vacuum plating, can not be for the electron beam gun plated film.
1997, Chinese Changchun vacuum sintering method that ray machine passes through, developed " particle MgF
2The crystal coating material ", its quality is the leading level in the world, but unstable because of its processing condition, still could not thoroughly solve and splashes and collapse a problem, the large particle of diameter 6-70 μ m also happens occasionally.And granular MgF
2The crystal coating material fills in electron beam gun plated film crucible to be got very inconveniently, also can cause artifact pollution, and this is also to cause in plated film splash and collapse another kind of factor a little.
Along with the development of electron beam gun plated film, through colding pressing, after hot pressing and pressure, sintering method forms corresponding the appearing on the market of the various Coating Materials of disc, as ZrO
2, MgO, TiO
2, Al
2O
3+ ZrO
2, Al
2O
3The kinds such as+MgO are numerous, and its purpose is drawn materials exactly just as electron beam gun crucible size, and dress is got conveniently, be difficult for polluting, and in evaporation, discharge quantity are few, therefore obtain widespread use.
In production due to the electron beam gun plated film to MgF
2Coating Materials has the strict quality requirement of " do not splash, do not collapse a little ", usually by high-purity MgF
2Material is through Leng Ya ﹑ hot compacting, then through the method for sintering prepared disc MgF
2Material can not be used at all.Within 2007, Japan once developed a kind of opaque " white disc MgF
2Coating Materials ", after colding pressing, sintering processes forms exactly, enter at that time Chinese market once fast-selling for the moment, can be just not good enough because of inner quality equally soon, splash and collapse a little seriously and discharge quantity is large etc. that problem exits market very soon.
" disc MgF
2The crystal coating material " be the Coating Materials that vast plated film worker suddenly expects use always.Take into account angle, " disc MgF from making method and cost two aspects
2Crystal " must come from the MgF of various diameters
2The rod crystal, then shape through optical-mechanical.
Current " the particle MgF of widespread use
2The crystal coating material " the vacuum sintering making method, owing to being type of heating in large crucible adopts, crucible is heated seriously unbalanced, can't make qualified MgF
2The rod crystal.
General descending manner single crystal growing furnace is manufactured the method for crystal, can go out MgF with excellent hole crucible sintering
2The rod crystal, and be monocrystalline, but, because body of heater Shou Heng warm area and pull down mechanism limit, its crucible is all little, at diameter, is generally Ф 300mm, high 350mm left and right, the MgF that sintering goes out
2Rod amount of crystals and limited length, its weight is no more than 20 kilograms at most, and length consuming time, and power consumption is large, involves great expense, if shape as disc MgF
2Crystal per kilogram price will be over 5000 yuan, so it can only at all can't be for vacuum plating for optical element.That these reasons cause " disc MgF
2The crystal coating material " can not appear on the market and apply so far.
Summary of the invention
The purpose of this invention is to provide a kind of disc magnesium fluoride MgF
2Crystal coating material and production method thereof, for the electron beam gun plated film, have Coating Materials do not splash, do not collapse point, without discharge quantity and the good evaporation characteristic such as generating surface is smooth, and coating process dress feeding is convenient, can avoid causing artifact pollution because of the dress feeding.
For achieving the above object, the technical solution used in the present invention is:
A kind of disc magnesium fluoride MgF
2Crystal coating material and production method thereof, this material is a kind of water white polycrystalline optical crystal Coating Materials, at wavelength 500mm place, its specific refractory power Ne=1.38, density of material is about 3.17 grams/cm
3The shape of this material is to adapt to the diameter of plurality of specifications electron beam gun crucible or crucible lining and disc or the circular cone cylindricality that depth design processes, and its diameter dimension scope is 20mm ~ 56mm, and the gauge scope is: 5mm ~ 30mm;
The making method of this material comprises vacuum sintering magnesium fluoride rhabdolith and two operations of optical-mechanical shaping processing, and wherein: 1) process of vacuum sintering magnesium fluoride rhabdolith is:
1. heat up: the magnesium fluoride powder is added in vaccum sintering device and vacuumizes, be equipped with graphite heater inside and outside being provided with how excellent hole plumbago crucible and crucible in this vaccum sintering device, after in device, vacuum tightness reaches 2Pa, heating simultaneously inside and outside crucible is implemented, and, with 100 ℃ ~ 120 ℃/h speed intensification, 10 ~ 12h, make temperature in device reach 1050 ℃ ~ 1200 ℃;
2. constant temperature: in device, keep vacuum tightness at 0.2 ~ 0.06Pa, 1250 ℃ ~ 1260 ℃ of temperature, keep constant temperature 14 ~ 16h;
3. cooling: keep vacuum tightness at 0.06 ~ 0.004Pa in device, with speed cooling 30 ~ 32h of 20 ℃ ~ 25 ℃/h; When the device temperature reaches 640 ℃ ~ 600 ℃, stop heating, the device body naturally cools to room temperature;
2) optical-mechanical shaping manufacturing procedure step is:
Take out the magnesium fluoride rhabdolith sintered from vaccum sintering device, according to the diameter of needed electron beam gun crucible or crucible lining and the MgF that the degree of depth is got corresponding size
2Rhabdolith, by the wafer type MgF of design
2The specification of crystal coating material is carried out the optical-mechanical forming process:
1. at first through inside diameter slicer the MgF of respective diameters size
2Rhabdolith is cut into the wafer type MgF of certain thickness and certain thickness tolerance by size
2
2. by the MgF of this thickness
2Disk reaches the disk of intended diameter size through optics edge polisher tarry matter, its smooth finish should reach ▽ more than 6;
3. last by the MgF of moulding
2Disk cleans through Ultrasonic Cleaners, and baking box is dried and vacuum packaging, is final disc magnesium fluoride crystal Coating Materials product.
Described Coating Materials product is applicable to all electron beam gun plating MgF
2Film, be particularly useful for surface smoothness and be better than 5/20 ultra-smooth optical element surface plating MgF
2Film, plated film particle diameter can be less than 5 μ m.
Compared with prior art, the invention has the beneficial effects as follows:
1) wafer type MgF of the present invention
2The specification of crystalline material is to process according to all kinds of electron beam gun crucibles or crucible lining size design, meets electron beam gun plating MgF fully
2The dimensional requirement of film crucible, the dress feeding is very convenient and can avoid artifact pollution.
2) MgF gone out through secondary-cleaned vacuum sintering
2The rod crystal, its inner quality excellence, " particle MgF
2The crystal coating material " purity is higher, and chemical purity is greater than 99.99%, MgF
2MgO in crystal and Mg(OH)
2Be eliminated ground more at the bottom of Toru, can exempt in plated film that 6-70 μ m is large diameter to be collapsed a little, and effectively reduce below diameter 5 μ m and collapse point (collapsing a little below disregarding 5 μ m during at present quality inspection), have really do not splash, do not collapse point, without discharge quantity and the excellent evaporation characteristic such as generating surface is smooth, can effectively improve by light-plated element surface smooth finish.The present invention especially is suitable for the ultra-smooth optical element surface plating MgF of high quality plated film requirement
2Film.
3) product cost of the present invention is far below traditional descending manner single crystal growing furnace MgF
2Rod crystal product (be only this cost 1/5th), make " disc MgF
2The crystal coating material " can be accepted by vast electron beam gun plated film field application, and become high-grade magnesium fluoride crystal plated film novel material and appear on the market.
The accompanying drawing explanation
Fig. 1 is a kind of electron beam gun crucible sectional view in current electron beam gun coating equipment;
Fig. 2 is the disc MgF of the present invention for this electron beam gun crucible
2The crystal sectional view;
Fig. 3 is the circular cone cylindricality MgF of the present invention for this electron beam gun crucible
2The crystal sectional view.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
A kind of disc magnesium fluoride crystal of the present invention Coating Materials is a kind of water white polycrystalline optical crystal, at wavelength 500mm place, and its specific refractory power Ne=1.38, density of material is about 3.17 grams/cm
3The shape of this material is to adapt to the diameter of all size electron beam gun crucible or crucible lining and disc or the circular cone cylindricality of depth design processing, and its diameter dimension scope is 20mm ~ 56mm, and its gauge scope is: 5mm ~ 30mm;
The making method of this material comprises vacuum sintering magnesium fluoride rhabdolith and two operations of optical-mechanical shaping processing, and wherein: 1) process of vacuum sintering magnesium fluoride rhabdolith is:
1. heat up: the magnesium fluoride powder is added in vaccum sintering device and vacuumizes, be equipped with graphite heater inside and outside being provided with how excellent hole plumbago crucible and crucible in this vaccum sintering device, after in device, vacuum tightness reaches 2Pa, heating simultaneously inside and outside crucible is implemented, and, with 100 ℃ ~ 120 ℃/h speed intensification, 10 ~ 12h, make temperature in device reach 1050 ℃ ~ 1200 ℃;
2. constant temperature: in device, keep vacuum tightness at 0.2 ~ 0.06Pa, 1250 ℃ ~ 1260 ℃ of temperature, keep constant temperature 14 ~ 16h;
3. cooling: in device, keep vacuum tightness at 0.06 ~ 0.004Pa, the speed cooling 30 ~ 32h with 20 ℃ ~ 25 ℃/h, when unit temp drops to 640 ℃ ~ 600 ℃, stop heating, and device naturally cools to room temperature;
2) optical-mechanical shaping manufacturing procedure step is:
Take out the magnesium fluoride rhabdolith sintered from vaccum sintering device, according to the diameter of needed electron beam gun crucible or crucible lining and the MgF that the degree of depth is got corresponding size
2Rhabdolith, by the wafer type MgF of design
2The specification of crystal coating material is carried out the optical-mechanical forming process:
1. at first through inside diameter slicer the MgF of respective diameters size
2Rhabdolith is cut into the disc MgF of certain thickness and certain thickness tolerance by size
2
2. by the MgF of this thickness
2Disk reaches the disk of intended diameter size through optics edge polisher tarry matter, this disc magnesium fluoride crystal surface smoothness should reach ▽ 6;
3. finally by the MgF be shaped
2Disk cleans through Ultrasonic Cleaners, and baking box is dried and vacuum packaging, is final disc magnesium fluoride crystal Coating Materials product.
Seeing Fig. 1, is a kind of electron beam gun crucible sectional view in current electron beam gun coating equipment.
Seeing Fig. 2, is the disc MgF of the present invention for Fig. 1 electron beam gun crucible
2The crystal sectional view.
This its diameter dimension of disc magnesium fluoride crystal Coating Materials has Ф 20mm ~ 56mm different size, and its gauge can be that 1/2,1/3,1/4 of the crucible degree of depth does not wait, and needs specification for 5mm ~ 30mm is various.
Seeing Fig. 3, is the circular cone cylindricality MgF of the present invention for Fig. 1 electron beam gun crucible
2The crystal sectional view.
" disc MgF due to various diameters and thickness
2The crystal coating material " with electron beam gun crucible used or crucible lining specification, be complementary; make coating process dress feeding and visual evaporating state all very convenient; the product price is moderate; have again do not splash, Beng Dian ﹑ is not without discharge quantity and the good evaporation characteristic such as generating surface is smooth; therefore can effectively improve coated product quality and finished product rate, and appear on the market and widespread use as high-grade magnesium fluoride crystal plated film novel material.
MgF of the present invention
2Crystal coating novel material material product is specially adapted to surface smoothness and is better than 5/20 optical element surface plating MgF
2Film, guarantee that plated film particle diameter is less than 5 μ m.
Claims (2)
1. a disc magnesium fluoride MgF
2Crystal coating material and production method thereof, is characterized in that, this material is a kind of water white polycrystalline optical crystal Coating Materials, at wavelength 500mm place, and its specific refractory power Ne=1.38, density of material is about 3.17 grams/cm
3The shape of this material is to adapt to the diameter of plurality of specifications electron beam gun crucible or crucible lining and disc or the circular cone cylindricality that depth design processes, and its diameter dimension scope is 20mm ~ 56mm, and the gauge scope is: 5mm ~ 30mm;
The making method of this material comprises vacuum sintering magnesium fluoride rhabdolith and two operations of optical-mechanical shaping processing, and wherein: 1) process of vacuum sintering magnesium fluoride rhabdolith is:
1. heat up: the magnesium fluoride powder is added in vaccum sintering device and vacuumizes, be equipped with graphite heater inside and outside being provided with how excellent hole plumbago crucible and crucible in this vaccum sintering device, after in device, vacuum tightness reaches 2Pa, heating simultaneously inside and outside crucible is implemented, and, with 100 ℃ ~ 120 ℃/h speed intensification, 10 ~ 12h, make temperature in device reach 1050 ℃ ~ 1200 ℃;
2. constant temperature: in device, keep vacuum tightness at 0.2 ~ 0.06Pa, 1250 ℃ ~ 1260 ℃ of temperature, keep constant temperature 14 ~ 16h;
3. cooling: keep vacuum tightness at 0.06 ~ 0.004Pa in device, with speed cooling 30 ~ 32h of 20 ℃ ~ 25 ℃/h; When the device temperature reaches 640 ℃ ~ 600 ℃, stop heating, the device body naturally cools to room temperature;
2) optical-mechanical shaping manufacturing procedure step is:
Take out the magnesium fluoride rhabdolith sintered from vaccum sintering device, according to the diameter of needed electron beam gun crucible or crucible lining and the MgF that the degree of depth is got corresponding size
2Rhabdolith, by the wafer type MgF of design
2The specification of crystal coating material is carried out the optical-mechanical forming process:
1. at first through inside diameter slicer the MgF of respective diameters size
2Rhabdolith is cut into the wafer type MgF of certain thickness and certain thickness tolerance by size
2
2. by the MgF of this thickness
2Disk reaches the disk of intended diameter size through optics edge polisher tarry matter, its smooth finish should reach ▽ more than 6;
3. last by the MgF of moulding
2Disk cleans through Ultrasonic Cleaners, and baking box is dried and vacuum packaging, is final disc magnesium fluoride crystal Coating Materials product.
2. require described a kind of disc magnesium fluoride MgF according to right 1
2Crystal coating material and production method thereof, is characterized in that, described Coating Materials product is applicable to all electron beam gun plating MgF
2Film, be particularly useful for surface smoothness and be better than 5/20 ultra-smooth optical element surface plating MgF
2Film, plated film particle diameter can be less than 5 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310323878.4A CN103422170B (en) | 2013-07-29 | 2013-07-29 | A kind of disc magnesium fluoride MgF 2crystal coating material and production method thereof |
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|---|---|---|---|
| CN201310323878.4A CN103422170B (en) | 2013-07-29 | 2013-07-29 | A kind of disc magnesium fluoride MgF 2crystal coating material and production method thereof |
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|---|---|
| CN103422170A true CN103422170A (en) | 2013-12-04 |
| CN103422170B CN103422170B (en) | 2016-03-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104790025A (en) * | 2015-04-14 | 2015-07-22 | 营口市荣兴达科技实业有限公司 | Preparation device and preparation technology for magnesium fluoride single crystal coating material |
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| JP2000211999A (en) * | 1999-01-22 | 2000-08-02 | Canon Inc | Production of fluoride |
| JP2006036619A (en) * | 2004-07-27 | 2006-02-09 | Soratesu Lab:Kk | Method and apparatus for manufacturing material |
| CN201289302Y (en) * | 2008-11-03 | 2009-08-12 | 长春晶科光电有限公司 | Device for heating stove stock in crucible |
| CN101850995A (en) * | 2010-06-18 | 2010-10-06 | 承德创为光电材料有限公司 | Process for preparing 5-20mm high-purity polycrystalline magnesium fluoride by liquid crystallization method |
| CN102674410A (en) * | 2011-03-09 | 2012-09-19 | 多氟多化工股份有限公司 | Production method for high-purity magnesium fluoride crystal |
| CN103147119A (en) * | 2013-03-21 | 2013-06-12 | 北京雷生强式科技有限责任公司 | Preparation method and growth equipment of magnesium fluoride crystal |
-
2013
- 2013-07-29 CN CN201310323878.4A patent/CN103422170B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000211999A (en) * | 1999-01-22 | 2000-08-02 | Canon Inc | Production of fluoride |
| JP2006036619A (en) * | 2004-07-27 | 2006-02-09 | Soratesu Lab:Kk | Method and apparatus for manufacturing material |
| CN201289302Y (en) * | 2008-11-03 | 2009-08-12 | 长春晶科光电有限公司 | Device for heating stove stock in crucible |
| CN101850995A (en) * | 2010-06-18 | 2010-10-06 | 承德创为光电材料有限公司 | Process for preparing 5-20mm high-purity polycrystalline magnesium fluoride by liquid crystallization method |
| CN102674410A (en) * | 2011-03-09 | 2012-09-19 | 多氟多化工股份有限公司 | Production method for high-purity magnesium fluoride crystal |
| CN103147119A (en) * | 2013-03-21 | 2013-06-12 | 北京雷生强式科技有限责任公司 | Preparation method and growth equipment of magnesium fluoride crystal |
Non-Patent Citations (2)
| Title |
|---|
| 沈永宏: "多孔体坩埚生长氟化钙晶体", 《光学精密工程》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104790025A (en) * | 2015-04-14 | 2015-07-22 | 营口市荣兴达科技实业有限公司 | Preparation device and preparation technology for magnesium fluoride single crystal coating material |
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| CN103422170B (en) | 2016-03-30 |
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