CN101328016A - Preparation of rare earth doping transparent halogenide phase separation glass - Google Patents
Preparation of rare earth doping transparent halogenide phase separation glass Download PDFInfo
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- CN101328016A CN101328016A CNA200810058766XA CN200810058766A CN101328016A CN 101328016 A CN101328016 A CN 101328016A CN A200810058766X A CNA200810058766X A CN A200810058766XA CN 200810058766 A CN200810058766 A CN 200810058766A CN 101328016 A CN101328016 A CN 101328016A
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- rare earth
- phase separation
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- halogenide
- glove box
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- 239000011521 glass Substances 0.000 title claims abstract description 61
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 34
- 238000005191 phase separation Methods 0.000 title claims abstract description 29
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000000460 chlorine Substances 0.000 claims abstract description 23
- -1 rare earth ions Chemical class 0.000 claims abstract description 18
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000004455 differential thermal analysis Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 239000005283 halide glass Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 2
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 abstract 2
- 150000004820 halides Chemical class 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 abstract 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 241000209456 Plumbago Species 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 230000006698 induction Effects 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910052794 bromium Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910001507 metal halide Inorganic materials 0.000 description 3
- 150000005309 metal halides Chemical class 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000931526 Acer campestre Species 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 229910016655 EuF 3 Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000005383 fluoride glass Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000006058 strengthened glass Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Abstract
The invention provides a method for preparing a rare earth-doped transparent halide phase separation glass characterized in that the mol percentage composition of the glass is as follows: AlF3 25-40%, MgF2 5-63%, MX2 1-15%, YF3 10-20%, ReF3 0.1-1%, wherein M is one or more selected from the divalent alkaline earth ions Mg<2+>, Ba<2+> and Sr<2+>, X is one or two selected from Br<-> and Cl<->, Re is one or two selected from the trivalent rare earth ions Sm<3+>, Tb<3+>, Eu<3+> or Ce<3+>. The rare earth-doped transparent halide phase separation glass is obtained by melting for 10-45 minutes in a high-frequency furnace under the chlorine or inert atmosphere protection at 800-1000 DEG C and heat-treating for 0.5-5 hours around the phase separation temperature after cooling. The threshold of the rare earth ionic valence energy change is reduced under the action of femto-second laser in the glass medium, which is more useful for information writing by femto-second laser and has better luminescence intensity.
Description
Technical field
The present invention relates to a kind of preparation method of rare earth doping transparent halogenide phase separation glass, be specifically related to the preparation of femtosecond laser three-dimensional optical storage material of write-read in transparent medium.
Technical background
Femtosecond laser is because pulsewidth is very narrow, can be at the material absorbing laser energy, and finally pass in the characteristic time of lattice with the form of heat energy, will have in the energy injecting material zone selected of height space, the influence that realizes heat nanosecond and the picosecond laser hyperfine processing of material that is difficult to realize seldom.Simultaneously, even material does not originally exist intrinsic to absorb in the optical maser wavelength place, owing to have superelevation strength of electric field (～10 near the focus of focusing femtosecond laser
10V/cm), also can be because of nonlinearity responses such as induced with laser multiphoton absorption, multi-photon ionizations.Therefore, by femtosecond laser can the implementation space high selectivity the microstructure modification, and give the light function of material uniqueness.Last century the nineties, the respectable and morally lofty or upright grade in three Pus of Japan realizes the three-dimensional light storage by the micro-nano structure that femtosecond laser changes transparent medium, and the achievement in research of particularly utilizing ultra-short pulse laser to change the variation of glass middle-weight rare earths ionic valence condition allows people see the dawn of three-dimensional light memory deviceization.(A.Toriumi, S.Kawata, Reflection confocal microscope readout system for three-dimensional photochromic optical datastorage.Opt Lett, 23 (1998) 1924.) the relevant result of study of utilizing femtosecond laser to realize containing the erasable three-dimensional light storage of realization of gold ion glass delivered of professor Qiu Jianrong of Zhejiang University.(J.Qiu，X.Jiang，C.Zhu，et?al.，Manipulation?ofgold?nanoparticles?inside?transparent?materials，Angew，Chem.Int.Ed.43(2004)2234.)
Because in theory, the higher cause of technical feasible degree, utilize femtosecond laser to change transparent medium and realize that the research of three-dimensional light storage mainly concentrates in the research that changes the rare earth ion valence state.In researchs such as Qiu, find, rare earth ion is not can both realize variation of valence in all glass, the composition of it and glass has very big relation, be that the polarizability of glass ingredient has overriding influence (J.Qiu to the rare earth ion variation of valence around the optical basicity of glass and the rare earth ion, M.shirai, T.Nakaya, et al., Space-selective precipation of silver nanoparticles inside glasses, Appl.Phys.Lett.81 (2002) 3040.).Make and utilize femtosecond laser to change glass middle-weight rare earths ionic valence condition realization three-dimensional light storage practicability, just must reduce the energy threshold of ionic valence condition variation, and this depends on glass material itself.In the glass system of selecting rare earth ion is had a reductibility its chemical stability often, physical strength etc. all relatively a little less than, therefore, the glass system that the reductibility of single phase is strong can not become the base mateiral of device.And for the glass system that generally rare earth ion is not had reductibility, the stability and the physical strength of glass are better, but glass matrix middle-weight rare earths ionic valence condition energy variation threshold value is higher usually, is unfavorable for that also femtosecond laser changes glass middle-weight rare earths ionic valence condition and realizes three-dimensional light storage practicability.
Halide glass has mechanical property preferably, be expected to be used for the three-dimensional information inscription of femtosecond laser, but the main component of this class glass is high-purity metal halide, metal halide has very strong water absorbability in air in preparation process, absorb airborne moisture easily and cause deliquescence, rotten, and introduce hydroxyl, influence the transparency and the mechanical property of the character of glass on the one hand, and the luminous intensity of rare earth ion; On the one hand, airborne oxygen also can react with metal halide, introduces hydroxyl in glass basis, thereby influences the character of glass in addition.
Summary of the invention
For overcoming existing rare earth doping transparent halogenide phase separation glass, when under the femtosecond laser effect, realizing information writing, be subject to the shortcoming of ambient conditions influence, the invention provides a kind of preparation method who is used for the rare earth doping transparent halogenide phase separation glass of the three dimensional optical information storage that femtosecond laser inscribes.
Design of the present invention is: when femtosecond laser affacts in the glass, compare with O, the F ion of rare-earth ion coordination, the easier electronics that provides of Cl, Br, and and produce electronics between rare earth and give and accept, make the rare earth ion reduction, thereby reduce the optical storage threshold value that changes based on ionic valence condition.The present invention aims to provide a kind of novel rare-earth doping transparent halogenide phase separation glass material, this material is good in chemical stability, introduce halogenide (Cl in the high glass of physical strength, Br) phase, behind the femtosecond laser focus irradiation, regional area is undergone phase transition, and make rare earth ion optionally enter into precipitated phase (second of introducing is principal constituent mutually), thereby reduce the energy threshold of rare earth ion variation of valence, both had advantages of excellent stability energy and physical strength, the substrate material that the rare earth ion valence state is changed easily, achievement of the present invention has extremely important meaning for the practical application of three-dimensional light storage.
Purpose of the present invention is finished by following technical proposal: a kind of preparation method of rare earth doping transparent halogenide phase separation glass is characterized in that through following process steps:
A, in glove box by following molar percentage batching, and carry out the mixing of component:
AlF
3 25～40mol％
MF
2 5～63mol％
MX
2 1～15mol％
YF
3 10～20mol％
ReF
3 0.1～1mol％
Wherein, M is the divalent alkaline-earth metal ION Mg
2+, Sr
2+, Ba
2+In one or more, Re is trivalent rare earth ions Sm
3+, Tb
3+, Eu
3+Or Ce
3+In one or more, X is univalent halide-ions Cl
-And Br
-In one or both;
B, above-mentioned compound is warming up to 800～1000 ℃, is incubated 10～45 minutes, make raw materials melt become liquid, be cooled to room temperature then, obtain rear-earth-doped halide glass;
C, step B gained glass is carried out differential thermal analysis obtain its halid phase separation temperature, in the positive and negative 20 ℃ of scopes of this phase separation temperature, rare earth doping transparent halogenide phase separation glass is carried out phase-splitting to be handled 0.5～5 hour, then it is carried out cutting and polishing, promptly get rare earth doping transparent halogenide phase separation glass.
The glove box condition of using in the described steps A is as follows: glove box is vacuumized, and the glove box body vacuum tightness that obtains is not higher than 1 * 10
-1Torr, limit case vacuum tightness is not higher than 5 * 10
-2Torr, oxygen content below the moisture value 1.47ppb, charge into nitrogen or the argon gas identical with ambient atmosphere air pressure then in glove box below 100ppb.
The purity of described each component 〉=99.95%.
Heat temperature raising among the described step B can be done carry out under the condition of protection gas feeding chlorine, and the chlorine flowrate that feeds is 2ml～20ml/ minute, with the Cl that prevents to add in the component
-, become Cl
2After the volatilization, influence quality product.
The present invention compares with existing common rear-earth-doped glass material that is used for the femtosecond laser inscription and preparation method thereof, has following outstanding advantage:
By halogens chlorine and bromide anion are introduced in the rear-earth-doped transparent halogenide phase separation glass, reduced in this glass medium the threshold value of rare earth ion variation of valence energy under the femtosecond laser effect, be beneficial to femtosecond laser more and carry out information writing; Because Cl and Br compare O, F lower phonon energy is arranged, relatively with simple fluoride glass, after the femtosecond laser effect, the rare earth ion in the halogenide phase-splitting is because the change in ligand field has better luminous intensity.
Carry out the preparation process of halide glass in glove box, by vacuum tightness, the control of moisture and oxygen content reduces or has stopped airborne moisture, and oxygen has reduced the OH in the glass matrix to the influence of the glass of halogenide and formation thereof
-Content has reduced the absorption of glass material infrared band optical signal, and the middle-weight rare earths ionic luminous intensity that has strengthened glass.
Adopt high-frequency furnace (high frequency induction heating device) that halide glass is melted system, the characteristics that have being rapidly heated and lower the temperature have reduced the volatilization of halogenic ingredient, and surrounding environment such as air are to the influence of glass quality.
Specific embodiment
Further illustrate content of the present invention below in conjunction with example, but these examples do not limit protection scope of the present invention.
Embodiment 1
(1), at first glove box (the MDB-2BL type of being produced by Japanese ponding Mechanology Inc.) is vacuumized processing, control glove box body vacuum tightness is not higher than 1 * 10
-1Torr, limit case vacuum tightness are not higher than 5 * 10
-2Torr, control simultaneously oxygen content below the 100ppb, moisture value below 1.47ppb, and in glove box, charge into the argon gas that is equal to pressure with around atmospheric pressure; In glove box be then: 39 moles AlF by forming molar percentage
3, 49.9 moles MgF
2, 1 mole BaCl
2, 10 moles YF
3, 0.1 mole SmF
3, taking by weighing raw material 20g altogether, the purity of above-mentioned raw materials is not less than 99.95%, with the above-mentioned raw materials thorough mixing, inserts in the plumbago crucible;
(2), (Japan is beautiful and make institute, is rapidly heated in MU-1700C), feeds Cl simultaneously in the heating chamber of high frequency induction heating device the plumbago crucible of above-mentioned charging to be put into the small-sized high frequency induction heating device that places glove box
2Gas carries out atmosphere protection, and wherein the chlorine flowrate of Tong Ruing is 2ml/ minute, when being heated to 800 ℃, is incubated 45 minutes, makes raw materials melt become liquid, is cooled to room temperature then, obtains glass sample;
(3), above-mentioned gained glass sample being carried out obtaining its muriatic phase separation temperature after the differential thermal analysis is 430 ℃, under 450 ℃ of temperature, sample is heated i.e. phase-splitting processing 0.5 hour, with the prior art means it is carried out cutting and polishing then, obtain halogenide phase separation glass.
Embodiment 2
(1), the vacuum-treat of glove box is with embodiment 1, in glove box, form, i.e. an AlF of 35 moles by mole per-cent
3, 49.5 moles MgF
2, 8 moles BaCl
2, 2 moles MgBr
2, 5 moles YF
3, 0.5 mole TbF
3, taking by weighing raw material 20g altogether, the purity of above-mentioned raw materials is not less than 99.95%, and with the said components thorough mixing, inserts in the plumbago crucible;
(2), the plumbago crucible of above-mentioned charging is put into the small-sized high frequency induction heating device identical with embodiment 1, be rapidly heated, in the heating chamber of high frequency induction heating device, feed Cl simultaneously
2Gas carries out atmosphere protection, and the airshed that wherein feeds chlorine is 6ml/ minute, is heated to 900 ℃ of insulations 35 minutes, makes raw materials melt become liquid, is cooled to room temperature then, obtains glass sample;
(3), above-mentioned glass sample being carried out the phase separation temperature that differential thermal analysis obtains its muriate and bromide is 425 ℃, under 435 ℃ of temperature, sample is heated i.e. phase-splitting processing 2 hours, with conventional means it is carried out cutting and polishing then, obtain the halogenide phase separation glass of chlorine and bromine.
Embodiment 3
(1), the vacuum-treat of glove box is with embodiment 1, in glove box, form, i.e. an AlF of 40 moles by mole per-cent
3-, 24 moles MgF
2, 15 moles SrBr
2, 20 moles YF
3, 1 mole EuF
3, taking by weighing raw material 20g altogether, the purity of above-mentioned raw materials is not less than 99.95%, and with the said components thorough mixing, inserts in the plumbago crucible;
(2), the plumbago crucible of above-mentioned charging is put into the small-sized high frequency induction heating device identical with embodiment 1, be rapidly heated, be incubated 20 minutes, make raw materials melt become liquid, be cooled to room temperature then, obtain glass sample to 950 ℃;
(3), glass sample is carried out the phase separation temperature that differential thermal analysis obtains its bromide is 420 ℃, under 400 ℃ of temperature, sample is heated, i.e. phase-splitting processing 4 hours is carried out cutting and polishing to it then, obtains bromide phase-splitting glass.
Embodiment 4
(1), the vacuum-treat of glove box is with embodiment 1, in glove box, form, i.e. an AlF of 40 moles by mole per-cent
3-, 24 moles MgF
2, 15 moles BaCl
2, 20 moles YF
3, 1 mole CeF
3, taking by weighing raw material 20g altogether, the purity of above-mentioned raw materials is not less than 99.95%, and with the said components thorough mixing, inserts in the plumbago crucible;
(2), the plumbago crucible of above-mentioned charging is put into the small-sized high frequency induction heating device identical with embodiment 1, in the heating chamber of high frequency induction heating device, feed Cl simultaneously
2Gas carries out atmosphere protection, and the airshed that wherein feeds chlorine is 20ml/ minute, is rapidly heated to 1000 ℃ of insulations 10 minutes, makes raw materials melt become liquid, coldly then removes to obtain glass sample;
(3), above-mentioned glass sample is carried out differential thermal analysis, and to obtain its muriatic phase separation temperature be 410 ℃, under 400 ℃ of temperature sample heated, i.e. phase-splitting processing 5 hours is carried out cutting and polishing to it then, obtains muriate phase-splitting glass.
Claims (4)
1, a kind of preparation method of rare earth doping transparent halogenide phase separation glass is characterized in that through following process steps:
A, in glove box by following molar percentage batching, and carry out the mixing of component:
AlF
3 25～40mol％
MF
2 5～63mol％
MX
2 1～15mol％
YF
3 10～20mol％
ReF
3 0.1～1mol％
Wherein, M is the divalent alkaline-earth metal ION Mg
2+, Sr
2+, Ba
2+In one or more, Re is trivalent rare earth ions Sm
3+, Tb
3+, Eu
3+Or Ce
3+In one or more, X is univalent halide-ions Cl
-And Br
-In one or both;
B, above-mentioned compound is warming up to 800～1000 ℃, is incubated 10～45 minutes, make raw materials melt become liquid, be cooled to room temperature then, obtain rear-earth-doped halide glass;
C, step B gained glass is carried out differential thermal analysis obtain its halid phase separation temperature, in the positive and negative 20 ℃ of scopes of this phase separation temperature, rare earth doping transparent halogenide phase separation glass is carried out phase-splitting to be handled 0.5～5 hour, then it is carried out cutting and polishing, promptly get rare earth doping transparent halogenide phase separation glass.
2, the preparation method of rare earth doping transparent halogenide phase separation glass according to claim 1 is characterized in that employed glove box condition is; Glove box is vacuumized, and control glove box body vacuum tightness is not higher than 1 * 10
-1Torr, limit case vacuum tightness is not higher than 5 * 10
-2Torr, oxygen content below the moisture value 1.47ppb, charge into nitrogen or the argon gas identical with ambient atmosphere air pressure then in glove box below 100ppb.
3, the preparation method of rare earth doping transparent halogenide phase separation glass according to claim 1 is characterized in that purity 〉=99.95% of described each component.
4, the preparation method of rare earth doping transparent halogenide phase separation glass according to claim 1; it is characterized in that the heat temperature raising among the described step B can carry out under the condition that feeds chlorine do protection gas; and the chlorine flowrate that feeds is 2ml～20ml/ minute, with the Cl that prevents to add in the component
-, become Cl
2After the volatilization, influence quality product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810058766XA CN101328016A (en) | 2008-07-29 | 2008-07-29 | Preparation of rare earth doping transparent halogenide phase separation glass |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810058766XA CN101328016A (en) | 2008-07-29 | 2008-07-29 | Preparation of rare earth doping transparent halogenide phase separation glass |
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| Publication Number | Publication Date |
|---|---|
| CN101328016A true CN101328016A (en) | 2008-12-24 |
Family
ID=40204068
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|---|---|---|---|
| CNA200810058766XA Pending CN101328016A (en) | 2008-07-29 | 2008-07-29 | Preparation of rare earth doping transparent halogenide phase separation glass |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114180831A (en) * | 2021-12-29 | 2022-03-15 | 中国建筑材料科学研究总院有限公司 | Photoetching glass and microstructure processing method thereof |
-
2008
- 2008-07-29 CN CNA200810058766XA patent/CN101328016A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114180831A (en) * | 2021-12-29 | 2022-03-15 | 中国建筑材料科学研究总院有限公司 | Photoetching glass and microstructure processing method thereof |
| CN114180831B (en) * | 2021-12-29 | 2024-04-02 | 中国建筑材料科学研究总院有限公司 | Photoetching glass and microstructure processing method thereof |
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Open date: 20081224 |