CN104445970B - Rapid demoulding method for fluoride film on surface of fused quartz optical substrate - Google Patents
Rapid demoulding method for fluoride film on surface of fused quartz optical substrate Download PDFInfo
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- CN104445970B CN104445970B CN201410621218.9A CN201410621218A CN104445970B CN 104445970 B CN104445970 B CN 104445970B CN 201410621218 A CN201410621218 A CN 201410621218A CN 104445970 B CN104445970 B CN 104445970B
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- fused quartz
- demoulding
- fluoride film
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- optical component
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- 230000003287 optical effect Effects 0.000 title claims abstract description 55
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000005350 fused silica glass Substances 0.000 title claims abstract description 40
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000758 substrate Substances 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000001117 sulphuric acid Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 239000012528 membrane Substances 0.000 abstract description 9
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 230000003746 surface roughness Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 25
- 239000000243 solution Substances 0.000 description 13
- 239000002253 acid Substances 0.000 description 12
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 6
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 229910001634 calcium fluoride Inorganic materials 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229910017053 inorganic salt Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000411 transmission spectrum Methods 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000001459 lithography Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 2
- 241001132374 Asta Species 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 229910003947 H3AlF6 Inorganic materials 0.000 description 1
- 229910004048 HBF4+3H2O Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 fluoride Compound Chemical class 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 229960002050 hydrofluoric acid Drugs 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- WOSISLOTWLGNKT-UHFFFAOYSA-L iron(2+);dichloride;hexahydrate Chemical group O.O.O.O.O.O.Cl[Fe]Cl WOSISLOTWLGNKT-UHFFFAOYSA-L 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- CAYKLJBSARHIDI-UHFFFAOYSA-K trichloroalumane;hydrate Chemical compound O.Cl[Al](Cl)Cl CAYKLJBSARHIDI-UHFFFAOYSA-K 0.000 description 1
- 239000002888 zwitterionic surfactant Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for quickly stripping a fluoride film on the surface of a fused quartz optical substrate, which belongs to the technical field of optical element preparation methods, and the method utilizes double decomposition reaction or complex reaction under room temperature or heating condition to ensure that the fluoride on the surface of the fused quartz optical substrate is completely removed by chemical reaction, the membrane removal reaction in a hot water bath is carried out only for 20-30 minutes at the fastest speed, the membrane removal in the warm water bath needs 1.5-2.5 hours, and the membrane removal at room temperature needs 3-7 hours. Compared with the uncoated optical substrate, the surface roughness of the optical substrate after demoulding has no obvious change and no detectable physical or chemical damage.
Description
Technical field
The present invention relates to optical element preparation method technical field, be specifically related to a kind of fused quartz optical substrate surface fluoride film
Quickly method for demoulding.
Background technology
In 193nm excimer lithography optical system, employ in a large number substrate be fused quartz material, thin film be fluoride material
The optical element of material.These optical elements due to different reasons need to remove the existing fluoride film plated film the most again in surface time, often
Realize thin film by optical polish method to remove.Optical polish method is the most time-consuming, cost is high, and can change to a certain extent
Becoming optical element surface face type, the imaging characteristic affecting optical element even makes optical element lose recycle value completely.And such as
Fruit can use loseless method to be rapidly removed by fused quartz optical substrate surface fluoride film, then can make the fused quartz optics after demoulding
Substrate, again with, effectively save cost, produces considerable economic benefit.Chemistry striping beyond doubt a kind of economical, effectively take off
Film method.For the fluoride film of fused quartz optical substrate surface, the selection of chemical method must be according to concrete fluoride film
Material determines.For the optical element of 193nm excimer lithography optical system, its fluoride film Main Ingredients and Appearance includes fluorine
Change magnesium, aluminium fluoride and lanthanum fluoride.Their character is as follows: Afluon (Asta) is a kind of colourless tetragonal crystal or powder, tasteless,
It is insoluble in water and alcohol, is slightly soluble in diluted acid, be dissolved in nitric acid.Aluminium fluoride: colourless or white crystals, water insoluble, insoluble in acid and
Alkali, character is the most stable, heats altogether with liquefied ammonia or concentrated sulphuric acid, or the most reactionless with potassium hydroxide congruent melting.Lanthanum fluoride: white powder
End, water insoluble, it is insoluble in hydrochloric acid, nitric acid and sulphuric acid, but perchloric acid can be dissolved in.From the character of three kinds of fluorides, adopt
Also having more limitation, such as aluminium fluoride during with chemical reaction demoulding, character is the most stable, and strong acid, highly basic do not react, moreover alkali
Can etch quartz sheet.In addition, outside dehydrogenation fluoric acid, hot phosphoric acid, quartz glass has preferable acid resistance to general acid.
Summary of the invention
A kind of method that it is an object of the invention to propose fused quartz quick demoulding of optical substrate surface fluoride film, the method makes
With conventional mineral acid and inorganic salt as reactant, greatly reduce cost, simplified laboratory operating procedures, when shortening reaction
Between, there is the features such as easy quick, safe and efficient, with low cost, environmental protection.
To achieve these goals, a kind of fused quartz quick method for demoulding of optical substrate surface fluoride film of the present invention, step
As follows:
Pipetting the mineral acid of certain volume, be poured in the deionized water of certain volume, making mineral acid ultimate density is 1.0-5.0
mol/L.By inorganic acid solution and surfactant solution (0.0 20mmol/L) or metal salt solution (0.1-5.0mol/L)
Mixing, forms liquid parting.The optical element of fused quartz substrate fluoride film is inserted in liquid parting, room temperature, tepidarium or
Take out after reacting 10 500 minutes under the conditions of hot bath and use deionized water to clean, obtaining the fused quartz optics unit of thorough demoulding
Part.
Wherein said mineral acid is concentrated sulphuric acid or concentrated nitric acid or strong phosphoric acid or concentrated hydrochloric acid or boric acid;
The preparation method of surfactant solution therein is: pipettes or weighs a certain amount of surfactant, be dissolved in certain volume
Deionized water in, making surfactant ultimate density is 0.0 20mmol/L.
Described surfactant is anionic surfactant sodium dodecylbenzene sulfonate or cationic surfactant cetyl
Trimethylammonium bromide or zwitterionic surfactant or non-ionic surfactant Tween 40;
The preparation method of metal salt solution therein is: weighs a certain amount of trivalent metal salt hydrate, is dissolved in going of certain volume
In ionized water, making inorganic salt ultimate density is 0.1-5.0mol/L.
Described inorganic salt is iron chloride hexahydrate or trichloride hydrate aluminum.
Further, the ratio of the amount of reactant species is mineral acid: surfactant=1:0.0-0.05;Mineral acid: inorganic
Salt=1:0.1 1.0.
Further, bath temperature 40-100 DEG C.
Further, heating device therefor is thermostat water bath or hydrothermal reaction kettle.
The principle of the present invention is:
Industrial employing fluorite (calcium fluoride CaF2) and concentrated sulphuric acid be heated to when 700 DEG C prepare Fluohydric acid. (Zhang Qinglian, " nothing
Chemical machine book series " volume six: Science Press, 1995:30-31)
Chemical equation is as follows:
CaF2+H2SO4(heat is dense) → 2HF+CaSO4 (1)
This realizes based on metathesis reaction, and heating is conducive to reaction to carry out;Equally, remove fluoride based on complex reaction to need equally
Heat.Such as H3BO3-HCl and calcium fluoride Hybrid Heating are dissolved, and calcium fluoride proceeds in solution, now boron and fluorine be combined into network from
Son.
2CaF2+4HCl+H3BO3=2CaCl2+HBF4+3H2O (2)
When continuing evaporation solution, fluorine is with BF3Form escapes.
Visible, said method all be unable to do without heating, and heating is conducive to reaction to carry out, and can make again fluoride evaporation effusion, make simultaneously
Product dissolubility increases, and is unlikely to be deposited in optical substrate.
Utilize F-In the solution with Al3+、Fe3+Etc. forming AlF6 3-, make the reaction of plating filmed metals fluoride form soluble fluoride
Compound, reaction equation is as follows:
MgF2+3HC l+AlC l3=3MgC l2+H3AlF6 (3)
Research finds, this reaction has higher reaction rate at ambient temperature, is suitable for room temperature membrane removal, properly increases reaction
Temperature, can accelerate response speed, prevents product from depositing.
Compared with prior art, the method have the advantages that:
Method for demoulding of the present invention is simple to operate, and raw material is cheap and easily-available, uses hot bath method to accelerate response speed, can be in very short time
Interior demoulding, is suitable for the emergent membrane removal of compact optical element, is i.e. suitable for the molten of larger area except i.e. use, tepidarium and room temperature method
The thin film of quartz-optical substrate surface is removed.
Accompanying drawing explanation
Fig. 1 is the ultraviolet-visible optical transmission spectra figure of quick membrane removal in hot bath, wherein floride-free with fused quartz optical substrate surface
Transmitance during thin film is as 100% baseline.
Fig. 2 is the ultraviolet-visible optical transmission spectra figure of very fast membrane removal in tepidarium, wherein floride-free with fused quartz optical substrate surface
Transmitance during thin film is as 100% baseline.
Fig. 3 is the ultraviolet-visible optical transmission spectra figure removing plated film under room temperature condition, wherein with fused quartz optical substrate surface without
Transmitance during fluoride film is as 100% baseline.
Detailed description of the invention
Below in conjunction with specific embodiment, the inventive method is described in further detail.Following example are the one of the present invention
A little preferred implementations, it is therefore intended that preferably illustrate present disclosure rather than protection scope of the present invention is produced any
Limit.
Embodiment 1
A kind of fused quartz quick method for demoulding of optical substrate surface fluoride film, it specifically comprises the following steps that
Pipette 11.1mL concentrated sulphuric acid, be poured slowly into equipped with in the beaker in appropriate amount of deionized water along walls of beaker, suitably turn after cooling
Moving on to, in 100mL volumetric flask, be settled to 100mL, solution concentration is 2M.Pipette this solution 12mL, pipette 2mM's
Surfactant cetyl trimethylammonium bromide solution 8mL, in beaker, will be coated with the fused quartz optics unit of fluoride film
Part is put in beaker, this beaker is put into heating different time in 95 DEG C of water-baths, takes out fused quartz optical component and clean, measure
The transmitance of fused quartz optical component.Finding that 20 minutes plated films of reaction are the most thoroughly removed, ultraviolet-visible optical transmission spectra curve returns
Near baseline.
In embodiment 1, bath temperature is 95 DEG C, sulfuric acid concentration 1.2M and above time, 20-30 minute can thoroughly membrane removal
(result is shown in Fig. 1).
Embodiment 2
A kind of fused quartz quick method for demoulding of optical substrate surface fluoride film, it specifically comprises the following steps that
Pipetting 27mL concentrated hydrochloric acid in 100mL volumetric flask, be settled to 100mL, solution concentration is 3.24M.Weigh water
Closing aluminum chloride 12.07 grams to be dissolved in this hydrochloric acid solution, aluminum trichloride concentration is 1M.Pipette this mixed liquor 10mL, be heated to
55 DEG C, the fused quartz optical component being coated with fluoride film is put into reaction different time in beaker, takes out fused quartz optical component
And clean, measure the transmitance of fused quartz optical component.Finding reaction 2.0 hours, plated film is the most thoroughly removed, and ultraviolet-visible is saturating
The rate curve of spectrum of mistake returns near baseline.
In example 2, when the mol ratio of hydrochloric acid Yu aluminum chloride be 3:1 and above time, under room temperature condition 3-7 hour can be thorough
End membrane removal (result is shown in Fig. 3).If wanting to make the response time shorten, reaction temperature can be properly increased, reacting in tepidarium and removing
Film, when bath temperature is 55 DEG C, can thoroughly remove plated film (result is shown in Fig. 2) within 1.5-2.5 hour.
Embodiment 3
A kind of fused quartz quick method for demoulding of optical substrate surface fluoride film, it specifically comprises the following steps that
Pipetting 27mL concentrated hydrochloric acid in 100mL volumetric flask, be settled to 100mL, solution concentration is 3.24M.Weigh water
Closing aluminum chloride 12.07 grams to be dissolved in this hydrochloric acid solution, aluminum trichloride concentration is 1M.Pipette this mixed liquor 10mL, will be coated with
The fused quartz optical component of fluoride film is put in beaker, reacts different time, take out fused quartz optical component under room temperature condition
And clean, measure the transmitance of fused quartz optical component.Finding reaction 7.0 hours, plated film is the most thoroughly removed, and ultraviolet-visible is saturating
The rate curve of spectrum of mistake returns near baseline (result is shown in Fig. 3).
Claims (3)
1. the fused quartz quick method for demoulding of optical substrate surface fluoride film, it is characterised in that step is as follows:
Pipette 11.1mL concentrated sulphuric acid, be poured slowly into equipped with in the beaker in appropriate amount of deionized water along walls of beaker, suitably turn after cooling
Moving on to, in 100mL volumetric flask, be settled to 100mL, solution concentration is 2M, pipettes this solution 12mL, pipettes 2mM's
Surfactant cetyl trimethylammonium bromide solution 8mL, in beaker, will be coated with the fused quartz optics unit of fluoride film
Part is put in beaker, is put into by this beaker in 95 DEG C of water-baths and heats 20 minutes, takes out fused quartz optical component and cleans, obtaining
The fused quartz optical component of demoulding.
2. the fused quartz quick method for demoulding of optical substrate surface fluoride film, it is characterised in that step is as follows:
Pipetting 27mL concentrated hydrochloric acid in 100mL volumetric flask, be settled to 100mL, solution concentration is 3.24M, weighs water
Closing aluminum chloride 12.07 grams to be dissolved in this hydrochloric acid solution, aluminum trichloride concentration is 1M, pipettes this mixed liquor 10mL, is heated to
55 DEG C, the fused quartz optical component being coated with fluoride film is put in beaker and react 2 hours, take out fused quartz optical component
And clean, obtain the fused quartz optical component of demoulding.
3. the fused quartz quick method for demoulding of optical substrate surface fluoride film, it is characterised in that step is as follows:
Pipetting 27mL concentrated hydrochloric acid in 100mL volumetric flask, be settled to 100mL, solution concentration is 3.24M, weighs water
Closing aluminum chloride 12.07 grams to be dissolved in this hydrochloric acid solution, aluminum trichloride concentration is 1M, pipettes this mixed liquor 10mL, will be coated with
The fused quartz optical component of fluoride film is put in beaker, reacts 7 hours under room temperature condition, takes out fused quartz optical component also
Clean, obtain the fused quartz optical component of demoulding.
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