CN108929034A - A kind of lanthanium titanate base glass sheet, and its preparation method and application - Google Patents
A kind of lanthanium titanate base glass sheet, and its preparation method and application Download PDFInfo
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- CN108929034A CN108929034A CN201811122351.4A CN201811122351A CN108929034A CN 108929034 A CN108929034 A CN 108929034A CN 201811122351 A CN201811122351 A CN 201811122351A CN 108929034 A CN108929034 A CN 108929034A
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- Prior art keywords
- glass
- lanthanium titanate
- titanate base
- raw material
- base glass
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000006121 base glass Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000011521 glass Substances 0.000 claims abstract description 89
- 239000002994 raw material Substances 0.000 claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 45
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000008188 pellet Substances 0.000 claims abstract description 19
- 238000007711 solidification Methods 0.000 claims abstract description 19
- 230000008023 solidification Effects 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- 230000003287 optical effect Effects 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 238000004093 laser heating Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 239000004065 semiconductor Substances 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000007731 hot pressing Methods 0.000 claims description 4
- 238000004020 luminiscence type Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 3
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000005098 hot rolling Methods 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 2
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims 1
- 229910001195 gallium oxide Inorganic materials 0.000 claims 1
- 239000011159 matrix material Substances 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 8
- 230000008025 crystallization Effects 0.000 abstract description 8
- 229910017592 La4Ti9O24 Inorganic materials 0.000 abstract 1
- 238000000048 melt cooling Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- 239000005084 Strontium aluminate Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910003669 SrAl2O4 Inorganic materials 0.000 description 5
- 239000002241 glass-ceramic Substances 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000005408 paramagnetism Effects 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000007496 glass forming Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000004579 marble Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003836 solid-state method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000004781 supercooling Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- QXJJQWWVWRCVQT-UHFFFAOYSA-K calcium;sodium;phosphate Chemical compound [Na+].[Ca+2].[O-]P([O-])([O-])=O QXJJQWWVWRCVQT-UHFFFAOYSA-K 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/127—Silica-free oxide glass compositions containing TiO2 as glass former
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
-
- G—PHYSICS
- G02—OPTICS
- G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
- G02C7/00—Optical parts
- G02C7/02—Lenses; Lens systems ; Methods of designing lenses
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Optics & Photonics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Ophthalmology & Optometry (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- General Health & Medical Sciences (AREA)
- Glass Compositions (AREA)
Abstract
The present invention relates to a kind of lanthanium titanate base glass sheet, and its preparation method and application, the glass includes LaO3/2、TiO2With other third oxides, glass phase La4Ti9O24, diameter >=10mm of lanthanium titanate base glass, refractive index is 2.0~2.5, and Abbe number is 15~25.The preparation method of the lanthanium titanate base glass includes: (1) by the La of formula ratio2O3、TiO2It is uniformly mixed with the powder of other third oxides and obtains raw mixture, pretreatment obtains the raw material solidified for no container；(2) the obtained raw material for being used for no container solidification handle without container solidification, obtain glass pellet；(3) glass powder is obtained after crushing glass pellet, and glass powder is subjected to pressurization heat treatment according to predetermined shape, obtains glass raw material.Method of the invention breaches the limitation of conventional melt cooling method, overcomes the problem for being easy crystallization during preparing lanthanium titanate base glass material, has successfully obtained lanthanium titanate base glass material.
Description
Technical field
The invention belongs to optical glass material technical fields, and in particular to a kind of lanthanium titanate base glass sheet and its preparation
Method and purposes, the lanthanium titanate base glass sheet are used for the fields such as camera lens material and up-conversion luminescence host material.
Background technique
In recent years, it with the continuous development and progress of digital camera, video camera, medical endoscope and microscope etc.,
The optical element for asking camera lens to use has better optical property, such as higher refractive index and lower dispersion.Conventional melt
The glass refraction that cooling method obtains is difficult have higher breakthrough, increasingly can not meet the demand in market.
Lanthanium titanate base glass material is that a kind of Novel mesh-free network formation body glass is made due to its special the Nomenclature Composition and Structure of Complexes
It is with excellent optical property.However, lanthanium titanate base glass can not be prepared with traditional melting cooling method, lanthanium titanate base glass
Dynamics window very little, glass forming ability is low.Currently, inhibiting the heterogeneous forming core of melt using no container solidification technology, making to melt
Body obtains high undercooling degree, can be quickly cooled down and obtain lanthanium titanate base glass material.But the glass size that this method is prepared
It is limited, it is generally only 3-5mm, limits its application development.
CN106082641, which is disclosed, converts lanthanium titanate base paramagnetism glass material and preparation method thereof, institute on a kind of green light
It states conversion lanthanium titanate base paramagnetism glass material on green light to be obtained by following component and preparation method: (1) being converted on the green light
Lanthanium titanate base paramagnetism glass material is by magnetic component Gd2O3It is introduced into lanthanium titanate sill；(2) green light will be constituted
After the powder mixing of each oxide of upper conversion lanthanium titanate base paramagnetism glass material, melted in furnace body of the gas suspension without container
Conversion lanthanium titanate base paramagnetism glass material on the green light is prepared in solidification.The lanthanium titanate base glass material has good
Good mechanical strength, thermal property and lower phonon energy has in fields such as short wavelength laser, optical waveguide, information storages
Have wide practical use, but limited using scantling made from no container solidification technology, limits its application development.
CN102432183B discloses a kind of Nanomicro-grade titanium oxide glass spheres and preparation method thereof, the glass marble of preparation
For diameter between 5nm~2000 μm, appearance is regular spherical, and preparation method is that single-phase crystalline state titanium oxide powder is uniformly supplied
Enter in a kind of high temperature line, powder is heated to fusing and forms drop, or even volatilization forms steam completely or partially；Drop is in height
Warm line end falls, and is first shrunk to spherical shape, and then cooling, solidification forms glass marble；Steam is first condensed into the spherical liquid of nanoscale
Drop, then cooling, solidification form nanometer glass ball, and drop necessarily is in contactless state in cooling and process of setting, no
It is in contact with wall or impurity in order to avoid triggering crystallization, preparation process is simple, is conducive to large-scale production, but scantling has
Limit, limits its application development.
CN107555800A discloses a kind of transparent Sr3Al2O6-SrAl2O4Glass ceramics and preparation method thereof, glass pottery
Porcelain is by Sr3Al2O6And SrAl2O4Two-phase material composition.With SrCO3-Al2O3For reaction system, formed by exploring acquisition glass
The stronger material component of ability obtains SrO-Al in conjunction with pneumatic suspension is heated by laser2O3The glass presoma of system, i.e. ball
Shape transparent glass；Transparent Sr is obtained using pressure sintering and dominated crystallization again3Al2O6-SrAl2O4Glass ceramics, the glass ceramics
For Sr3Al2O6And SrAl2O4The transparent glass ceramics of two phase compositions.The method quickly and efficiently obtains the transparent glass of bulk
Glass ceramics, but Sr3Al2O6-SrAl2O4The refractive index of glass ceramics is lower.
This field needs to develop a kind of large-sized lanthanium titanate base glass material, and makes the lanthanium titanate base glass material of preparation
Expect refractive index with higher, and macro-size is larger, can satisfy the demand of many optical fields.
Summary of the invention
In view of the deficiencies of the prior art, described one of the objects of the present invention is to provide a kind of lanthanium titanate base glass sheet
Lanthanium titanate base glass sheet includes LaO3/2、TiO2With other third oxides；Other described third oxides are in addition to LaO3/2、
TiO2Oxide in addition.
The main component that the present invention designs lanthanium titanate base glass is LaO3/2、TiO2With other third oxides, wherein other
The addition of third oxide can make glass network structure more complicated, increase sample crystallization activation energy, inhibit sample crystallization,
To increase the dynamics window of lanthanium titanate base glass, the forming ability of lanthanium titanate base glass is improved, lanthanium titanate is overcome
The problem of base glass can not be prepared with traditional melting cooling method.Other third oxides can promote the substrate to be had
The vitreum of good light permeability, if being added without other third oxides, glass forming ability is poor, and material translucency is made very
Difference.
The present invention is not specifically limited other third oxides, in addition to LaO3/2、TiO2Oxide in addition is theoretically all
It can be used as other third oxides of the invention.Preferably, other described third oxides are the oxidation that can form glassy state
Object.
Preferably, lanthanium titanate base glass sheet composition of the present invention presses mole percent, including following components:
LaO3/220.8mol%~40.8mol%
TiO249.2mol%~79.2mol%
Other thirds 0~20mol% of oxide, does not include 0；
The sum of described lanthanium titanate base glass sheet each component total moles are calculated as 100%.
Further preferably, LaO3/225mol%~40mol%
TiO250mol%~75mol%
5~20mol% of other third oxides.
Preferably, other described third oxides include silica, zirconium oxide, aluminium oxide, barium monoxide, tungsten oxide, oxygen
Change gallium, calcium oxide, in bismuth oxide or niobium oxide any one or at least two combination, such as silica, zirconium oxide, oxidation
Aluminium, barium monoxide etc..
Preferably, LaO of the present invention3/2Mole percent be 20.8mol%~40.8mol%, such as
23.9mol%, 25mol%, 27.4mol%, 30.8mol%, 32.5mol%, 40.5mol% etc..
Preferably, TiO of the present invention2Mole percent be 49.2mol%~79.2mol%, such as
46.1mol%, 52.6mol%, 59.2mol%, 62.5mol%, 73mol%, 75mol%, 79mol% etc..
Preferably, the mole percent of other third oxides of the present invention be 0~20mol%, such as 0.1mol%,
1mol%, 5mol%, 8mol%, 10mol%, 15.2mol%, 18.9mol% etc..
When the mole percent of other third oxides is greater than 20mol%, the mole percent mistake of other third oxides
Greatly, cause the mole percent of glass phase too small, the refractive index of sample seriously reduces, and influences its application.
Preferably, La element and Ti elemental mole ratios are 4:9 in the glass phase of lanthanium titanate base glass sheet of the present invention.
The present invention is not particularly limited the macro-size of the lanthanium titanate base glass, can be optionally larger size
(such as 10mm or more) is also possible to smaller size (such as 10mm or less), and the selection of specific macro-size, which depends on, pressurizes
The size of the mold of heat treatment.
Preferably, diameter >=10mm of the lanthanium titanate base glass sheet, for example, 20mm, 30mm, 40mm, 50mm, 60mm,
80mm, 1cm, 2cm, 4cm, 5cm, 8cm etc..
The diameter of lanthanium titanate base glass sheet of the present invention can be understood as macroscopical ruler of the lanthanium titanate base glass
It is very little.
Preferably, the refractive index of the lanthanium titanate base glass sheet is 2.0~2.5, such as 2.1,2.2,2.3,2.4 etc..
Preferably, the Abbe number of the lanthanium titanate base glass sheet be 15~25, such as 16,17,18,19,20,21,22,
23,24 etc..
Preferably, transmitance >=40% of the lanthanium titanate base glass sheet, for example, 45%, 50%, 55%, 60%,
65%, 70% etc..
The second object of the present invention is to provide a kind of preparation method of lanthanium titanate base glass sheet, the preparation method includes
Following steps:
(1) by the La of formula ratio2O3、TiO2It is uniformly mixed with the powder of other third oxides and obtains raw mixture, in advance
Processing obtains the raw material solidified for no container；
(2) the obtained raw material for being used for no container solidification handle without container solidification, obtain glass pellet；
(3) glass powder is obtained after crushing glass pellet, and glass powder is subjected to pressurization heat treatment according to predetermined shape, is obtained
Glass raw material.
No container solidification technology can contact to avoid melt with chamber wall, inhibit heterogeneous forming core, melt made to obtain deep mistake
Cold degree, to obtain the lanthanium titanate base glass of amorphous, no container solidification technology, which overcomes, prepares lanthanium titanate using high temperature solid-state method
The problem of crystallization is easy in base glass process.
The present invention is heat-treated to have obtained lanthanium titanate base glass sheet using no container solidification-pressurization, and existing no container is solidifying
Solid product size be generally only 3~5mm, preparation method of the invention can break through cooling velocity pair in no container solidification technology
The size of lanthanium titanate base glass limits, and can successfully prepare pattern and the controllable large scale lanthanium titanate base glass of size, protect simultaneously
Stay its excellent optical property.
During no container solidifies, it is heated to the lanthanium titanate base glass of supercooling liquid phase region Δ T, is able to maintain non-
Crystalline structure, viscosity are reduced, are sufficiently softened, using plastic behavior of the amorphous more than glass transformation temperature, in external force
Under can be realized quick densifying, realize the lanthanium titanate base glass of predetermined shape Yu size (shape and size dependent on mold)
The preparation purpose of glass material, while remaining the performance of lanthanium titanate base glass high refractive index.
Preferably, the process of step (2) the of the present invention no container solidification includes: to solidify no container using pneumatic suspension
In the sky, laser heating will be heated to molten condition to raw material stable suspersion without container coagulated raw material, and then it is small to obtain glass for cooling
Ball.
Preferably, the gas that the pneumatic suspension uses includes any one in oxygen, nitrogen, helium, argon gas or air
Kind or at least two combination, preferred oxygen.
Preferably, the laser heating includes CO2Laser heating and/or semiconductor laser heating, preferably CO2Laser
The combination of device heating and semiconductor laser heating.
Preferably, the melt temperature of the molten condition be 1500~3000 DEG C, such as 1600 DEG C, 1700 DEG C, 1900 DEG C,
2000 DEG C, 2200 DEG C, 2300 DEG C, 2500 DEG C, 2700 DEG C, 2800 DEG C, 2900 DEG C etc..
Preferably, the time of the molten condition is 1~5min, such as 2min, 3min, 4min etc..
Preferably, the rate of temperature fall of the cooling be 100~400 DEG C/s, such as 150 DEG C/s, 180 DEG C/s, 200 DEG C/s,
230 DEG C/s, 250 DEG C/s, 300 DEG C/s, 320 DEG C/s, 350 DEG C/s, 380 DEG C/s etc..
Cooling rate of temperature fall is easy crystallization in cooling procedure, is unable to get lanthanium titanate base glass less than 100 DEG C/s, melt
Glass, for current technology means, cooling rate of temperature fall maximum can only achieve 400 DEG C/s.
Preferably, the diameter of the glass pellet is 2~6mm, such as 3mm, 4mm, 5mm etc..
Preferably, step (3) the of the present invention pressurization heat treatment includes any in hot pressed sintering, SPS sintering or hot rolling
One kind, preferably hot pressed sintering.
Preferably, the partial size of the glass powder be 38~150 μm, such as 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm,
100 μm, 110 μm, 120 μm, 130 μm etc..
Preferably, the temperature of the pressurization heat treatment is in lanthanium titanate base glass material critical cooling rate.
Critical cooling rate of the present invention can be tested by differential scanning calorimetry (DSC) and be obtained.
Preferably, it is described by glass powder according to predetermined shape carry out pressurization heat treatment process include: to be placed in glass powder
Pressurization heat treatment is carried out in the mold of predetermined shape.
Preferably, it is described pressurization heat treatment temperature be 800~900 DEG C, such as 810 DEG C, 820 DEG C, 830 DEG C, 840 DEG C,
850 DEG C, 860 DEG C, 870 DEG C, 880 DEG C, 890 DEG C, 900 DEG C etc..
Preferably, it is described pressurization heat treatment heating rate be 5~20 DEG C/min, such as 6 DEG C/min, 7 DEG C/min, 8 DEG C/
Min, 10 DEG C/min, 12 DEG C/min, 15 DEG C/min, 17 DEG C/min, 19 DEG C/min etc..
Preferably, it is described pressurization heat treatment pressure be 10~90MPa, such as 15MPa, 20MPa, 30MPa, 40MPa,
50MPa, 55MPa, 60MPa, 65MPa, 70MPa, 80MPa etc..
Preferably, it is described pressurization heat treatment time be 10~60min, such as 15min, 20min, 25min, 30min,
35min, 40min, 45min, 50min, 55min, 58min etc..
Preferably, the environment of the pressurization heat treatment includes any one in vacuum environment, nitrogen environment or ar gas environment
Kind, preferably vacuum environment.
Preferably, pretreatment described in step (1) of the present invention includes calcining raw mixture, by calcined powder
End is pressed into block, be then split into predetermined size without container coagulated raw material.
Preferably, the temperature of the calcining be 1000~1500 DEG C, such as 1150 DEG C, 1200 DEG C, 1250 DEG C, 1300 DEG C,
1350 DEG C, 1400 DEG C, 1450 DEG C etc..
Preferably, the time of the calcining is 1~10h, such as 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h etc..
Preferably, the pressure of powder compacting is 5~15MPa, for example, 5MPa, 7.5MPa, 10MPa, 12.5MPa,
15MPa etc..
Preferably, the obtained quality without container coagulated raw material divided is 10~100mg/ block, such as 20mg/ block,
30mg/ block, 40mg/ block, 50mg/ block, 60mg/ block, 70mg/ block, 90mg/ block etc..
Preferably, step (4) are carried out after step (3) of the present invention: glass raw material is made annealing treatment.
Preferably, the temperature of the annealing is 600~800 DEG C, such as 620 DEG C, 650 DEG C, 680 DEG C, 700 DEG C, 720
DEG C, 750 DEG C, 780 DEG C etc..
Preferably, the time of the annealing be 1~15h, such as 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h,
11h, 12h, 13h, 14h etc..
As optimal technical scheme, lanthanium titanate base glass sheet preparation method of the present invention includes the following steps:
(1) by the La of formula ratio2O3、TiO2It is uniformly mixed with the powder of other third oxides, at 1000~1500 DEG C
Calcine 1~10h after, calcined powder is pressed into block under 5~15MPa pressure, be then split into quality be 10~
100mg/ block without container coagulated raw material；
(2) will without container coagulated raw material, pneumatic suspension makes its stable suspersion in the sky in oxygen, CO2Laser is heated to
1500~3000 DEG C make no container coagulated raw material 1~5min of molten condition, then with the rate of temperature fall of 100~400 DEG C/s into
Row cooling treatment obtains the glass pellet that diameter is 2~6mm；
(3) glass powder that partial size is 38~150 μm is obtained after crushing glass pellet, under vacuum conditions, by glass powder
800~1000 DEG C are risen to the heating rate of 5~20 DEG C/min according to predetermined shape, and carries out heat under 10~90MPa pressure
Pressure 10~60min of sintering, obtains glass raw material；
(4) glass raw material is made annealing treatment to 1~15h at 600~800 DEG C.
The three of the object of the invention are to provide a kind of purposes of lanthanium titanate base glass sheet as described in the first purpose, the titanium
Sour lanthanum base glass sheet is applied to optical material field, is preferably used as the lens materials, camera lens material and up-conversion luminescence of glasses
Host material.
Camera lens material can be applied to digital camera, video camera, medical endoscope and microscopical lens element material；
Up-conversion luminescence host material can be applied to the transparent encapsulated layer of Organic Light Emitting Diode (OLED), high-density optical storage,
The fields such as optical-fibre communications and Three-dimensional Display.
Compared with prior art, the invention has the following beneficial effects:
(1) other third oxides are added in the present invention in lanthanium titanate base glass, can improve the power of lanthanium titanate base glass
Window is learned, the Forming ability of lanthanium titanate base glass is promoted, overcomes lanthanium titanate base glass that can not be prepared with traditional melting cooling method
The problem of, while the presence of other third oxides makes the lanthanium titanate base glass have good translucency.
(2) present invention using no container solidification technology can contact to avoid melt with chamber wall, inhibit heterogeneous forming core, gram
The problem for preparing using high temperature solid-state method and being easy crystallization in lanthanium titanate base glass process is taken；It, will simultaneously after no container solidifies
No container solidification products carry out pressurization heat treatment in supercooling liquid phase region, retain the noncrystalline state of lanthanium titanate base glass glass, thus
It breaches no container solidification technology and (being generally only 3~5mm) is limited to the size of lanthanium titanate base glass, realize preparation preboarding
The purpose of shape and the lanthanium titanate base glass material of size, while remaining the performance of lanthanium titanate base glass high refractive index, refractive index
It is 2.0~2.5, Abbe number is 15~25, transmitance >=40%.
Detailed description of the invention
Fig. 1 is that 1 hot pressed sintering of the embodiment of the present invention obtains the XRD spectrum of sample；
Fig. 2 is the sample photo that hot pressed sintering obtains in the embodiment of the present invention 1；
Fig. 3 is that hot pressed sintering obtains the refraction index test result of sample in the embodiment of the present invention 1.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) by raw material powder La2O3、TiO2LaO is pressed with silica3/2:TiO2: oxidation silicon mol ratio is 30.8:59.2:
10.0 weigh, and calcine 2h at 1200 DEG C after evenly mixing, calcined powder is pressed into block under the pressure of 10MPa,
Being then split into quality is 40mg without container coagulated raw material；
(2) will without container coagulated raw material, pneumatic suspension makes its stable suspersion in the sky in oxygen, semiconductor laser and
CO2Laser is heated to 2200 DEG C simultaneously makes no container coagulated raw material molten condition 2min, then with the cooling speed of 300 DEG C/s
Rate carries out cooling treatment, obtains the glass pellet that diameter is 3mm；
(3) glass powder that partial size is 50 μm is obtained after crushing glass pellet to be under vacuum conditions placed in glass powder directly
Diameter is to rise to 860 DEG C in the graphite jig of 20mm with the heating rate of 10 DEG C/min, and hot pressing burning is carried out under 60MPa pressure
30min is tied, glass raw material is obtained；
(4) glass raw material is made annealing treatment into 10h at 700 DEG C, obtaining diameter as shown in Figure 2 is the colorless and transparent of 20mm
Shape lanthanium titanate base glass sheet carries out XRD test to the lanthanium titanate base glass sheet, as a result as shown in Figure 1, sheet material is with good
Good amorphous performance carries out refraction index test to the lanthanium titanate base glass sheet, and as a result refractive index as shown in Figure 3 is 2.20.
Embodiment 2
The difference from embodiment 1 is that LaO in step (1)3/2:TiO2:SiO2Molar ratio is 27.4:52.6:20.
Embodiment 3
The difference from embodiment 1 is that LaO in step (1)3/2:TiO2:SiO2Molar ratio is 32.5:62.5:5.
Embodiment 4
The difference from embodiment 1 is that LaO in step (1)3/2:TiO2:SiO2Molar ratio is 23.9:46.1:30.
Embodiment 5
The difference from embodiment 1 is that by SiO in step (1)2Equimolar replaces with ZrO2。
Embodiment 6
The difference from embodiment 1 is that by SiO in step (1)2Equimolar replaces with Al2O3。
Embodiment 7
The difference from embodiment 1 is that the temperature of hot pressed sintering is 800 DEG C in step (3).
Embodiment 8
The difference from embodiment 1 is that the temperature of hot pressed sintering is 900 DEG C in step (3).
Embodiment 9
The difference from embodiment 1 is that the pressure of hot pressed sintering is 10MPa in step (3).
Embodiment 10
The difference from embodiment 1 is that the pressure of hot pressed sintering is 90MPa in step (3).
Embodiment 11
The difference from embodiment 1 is that the time of hot pressed sintering is 10min in step (3).
Embodiment 12
The difference from embodiment 1 is that the time of hot pressed sintering is 60min in step (3).
Embodiment 13
The difference from embodiment 1 is that glass powder is placed in the graphite jig that diameter is 10mm in step (3).
Embodiment 14
The difference from embodiment 1 is that glass powder is placed in the graphite jig that diameter is 30mm in step (3).
Embodiment 15
(1) by raw material powder La2O3、TiO2LaO is pressed with silica3/2:TiO2: oxidation silicon mol ratio is 30.8:59.2:
10.0 weigh, and calcine 10h at 1000 DEG C after evenly mixing, calcined powder are pressed into block under 5MPa pressure, so
Being divided into quality afterwards is 10mg without container coagulated raw material；
(2) will without container coagulated raw material, pneumatic suspension makes its stable suspersion in the sky in oxygen, semiconductor laser and
CO2Laser is heated to 3000 DEG C simultaneously makes no container coagulated raw material molten condition 1min, then with the cooling speed of 300 DEG C/s
Rate carries out cooling treatment, obtains the glass pellet that diameter is 3mm；
(3) glass powder that partial size is 150 μm is obtained after crushing glass pellet to be under vacuum conditions placed in glass powder
Diameter is to rise to 860 DEG C in the graphite jig of 20mm with the heating rate of 5 DEG C/min, and hot pressing burning is carried out under 60MPa pressure
30min is tied, glass raw material is obtained；
(4) glass raw material is made annealing treatment into 1h at 800 DEG C, obtains the lanthanium titanate base glass sheet that diameter is 20mm.
Embodiment 16
(1) by raw material powder La2O3、TiO2LaO is pressed with silica3/2:TiO2: oxidation silicon mol ratio is 30.8:59.2:
10.0 weigh, and calcine 1h at 1500 DEG C after evenly mixing, calcined powder are pressed into block under 15MPa pressure, so
Being divided into quality afterwards is 100mg without container coagulated raw material；
(2) will without container coagulated raw material, pneumatic suspension makes its stable suspersion in the sky in oxygen, semiconductor laser and
CO2Laser is heated to 1500 DEG C simultaneously makes no container coagulated raw material molten condition 5min, then with the cooling speed of 300 DEG C/s
Rate carries out cooling treatment, obtains the glass pellet that diameter is 3mm；
(3) glass powder that partial size is 38 μm is obtained after crushing glass pellet to be under vacuum conditions placed in glass powder directly
Diameter is to rise to 860 DEG C in the graphite jig of 20mm with the heating rate of 20 DEG C/min, and hot pressing burning is carried out under 60MPa pressure
30min is tied, glass raw material is obtained；
(4) glass raw material is made annealing treatment into 15h at 600 DEG C, obtains the lanthanium titanate base glass sheet that diameter is 20mm.
Comparative example 1
The difference from embodiment 1 is that by raw material powder La2O3And TiO2By LaO3/2:TiO2Molar ratio is 30.8:
69.2。
Comparative example 2
The difference from embodiment 1 is that silica equimolar is replaced with iron oxide.
Performance test:
The lanthanium titanate base glass sheet being prepared is performed the following performance tests:
(1) refractive index is measured by ellipsometer.
(2) Abbe number is according to νd=(nd-1)/(nF-nC) be calculated, wherein nd、nFAnd nCBe respectively 587.6nm,
The refractive index of sample at 486.1nm and 656.3nm.
(3) transmitance is measured by ultraviolet-uisible spectrophotometer.
The performance test results are as shown in table 1:
Table 1
It can be seen from Table 1 that embodiment 1-16 is in La2O3And TiO2Middle addition silica, the lanthanium titanate base glass of generation
Not only there is good optical property, while realizing the controllable of pattern and size, breach size limitation in the prior art,
Large-sized lanthanium titanate base glass has successfully been made.
It can be seen from Table 1 that embodiment 4 is relative to embodiment 1, refractive index is lower, and Abbe number is higher, transmitance compared with
It is low, it may be possible to since dioxide-containing silica is more in the lanthanium titanate base glass of preparation, cationic polarizability and oxygen bulk density drop
Low, so the refractive index that sample is made is lower, Abbe number is higher, and transmitance is lower.
It can be seen from Table 1 that comparative example 1 is lower relative to 1 transmitance of embodiment, it may be possible to due to La2O3-TiO2Two
The glass forming ability of first glass is poor, so transmitance is very low.
It can be seen from Table 1 that comparative example 2 is lower relative to 1 refractive index of embodiment, Abbe number is higher and transmitance compared with
It is low, it may be possible to since iron oxide can not increase the glass forming ability of sample, so the optical property that sample is made is poor.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (10)
1. a kind of lanthanium titanate base glass sheet, which is characterized in that the lanthanium titanate base glass sheet includes LaO3/2、TiO2And other
Third oxide；
Other described third oxides are in addition to LaO3/2、TiO2Oxide in addition.
2. lanthanium titanate base glass sheet as described in claim 1, which is characterized in that the lanthanium titanate base glass sheet composition is pressed
Mole percent, including following components:
LaO3/220.8mol%~40.8mol%
TiO249.2mol%~79.2mol%
Other thirds 0~20mol% of oxide, does not include 0；
The sum of described lanthanium titanate base glass sheet each component total moles are calculated as 100%；
Further preferably, LaO3/225mol%~40mol%
TiO250mol%~75mol%
5~20mol% of other third oxides；
Preferably, other described third oxides include silica, zirconium oxide, aluminium oxide, barium monoxide, tungsten oxide, gallium oxide,
In calcium oxide, bismuth oxide or niobium oxide any one or at least two combination.
3. lanthanium titanate base glass sheet as claimed in claim 1 or 2, La member in the glass phase of the lanthanium titanate base glass sheet
Element is 4:9 with Ti elemental mole ratios；
Preferably, diameter >=10mm of the lanthanium titanate base glass sheet；
Preferably, the refractive index of the lanthanium titanate base glass sheet is 2.0~2.5；
Preferably, the Abbe number of the lanthanium titanate base glass sheet is 15~25；
Preferably, transmitance >=40% of the lanthanium titanate base glass sheet.
4. a kind of preparation method of the lanthanium titanate base glass sheet as described in one of claim 1-3, which is characterized in that the system
Preparation Method includes the following steps:
(1) by the La of formula ratio2O3、TiO2It is uniformly mixed with the powder of other third oxides and obtains raw mixture, pre-processed
Obtain the raw material solidified for no container；
(2) the obtained raw material for being used for no container solidification handle without container solidification, obtain glass pellet；
(3) glass powder is obtained after crushing glass pellet, and glass powder is subjected to pressurization heat treatment according to predetermined shape, obtains glass
Raw material.
5. preparation method as claimed in claim 4, which is characterized in that the process of step (2) the no container solidification includes: to adopt
Make no container coagulated raw material stable suspersion in the sky with pneumatic suspension, laser heating will be heated to molten without container coagulated raw material
State, then cooling obtains glass pellet；
Preferably, the gas that the pneumatic suspension uses include in oxygen, nitrogen, helium, argon gas or air any one or
At least two combination；
Preferably, the laser heating includes CO2Laser heating and/or semiconductor laser heating；
Preferably, the melt temperature of the molten condition is 1500~3000 DEG C；
Preferably, the time of the molten condition is 1~5min；
Preferably, the rate of temperature fall of the cooling is 100~400 DEG C/s；
Preferably, the diameter of the glass pellet is 2~6mm.
6. preparation method as described in claim 4 or 5, which is characterized in that step (3) the pressurization heat treatment includes that hot pressing is burnt
Knot, SPS sintering or hot rolling in any one；
Preferably, the partial size of the glass powder is 38~150 μm；
Preferably, the temperature of the pressurization heat treatment is in lanthanium titanate base glass material critical cooling rate；
Preferably, it is described by glass powder according to predetermined shape carry out pressurization heat treatment process include: glass powder is placed in it is predetermined
Pressurization heat treatment is carried out in the mold of shape；
Preferably, the temperature of the pressurization heat treatment is 800~900 DEG C；
Preferably, the heating rate of the pressurization heat treatment is 5~20 DEG C/min；
Preferably, the pressure of the pressurization heat treatment is 10~90MPa；
Preferably, the time of the pressurization heat treatment is 10~60min；
Preferably, the environment of the pressurization heat treatment includes any one in vacuum environment, nitrogen environment or ar gas environment.
7. the preparation method as described in one of claim 4-6, which is characterized in that pretreatment described in step (1) includes will be former
Material mixture calcined, calcined powder is pressed into block, be then split into predetermined size without container coagulated raw material；
Preferably, the temperature of the calcining is 1000~1500 DEG C；
Preferably, the time of the calcining is 1~10h；
Preferably, the pressure of the powder compacting is 5~15MPa；
Preferably, the obtained quality without container coagulated raw material of dividing is 10~100mg/ block.
8. the preparation method as described in one of claim 4-7, which is characterized in that carry out step (4) after step (3): by glass
Glass raw material are made annealing treatment；
Preferably, the temperature of the annealing is 600~800 DEG C；
Preferably, the time of the annealing is 1~15h.
9. the preparation method of the lanthanium titanate base glass sheet as described in one of claim 4-8, which is characterized in that the preparation side
Method includes the following steps:
(1) by the La of formula ratio2O3、TiO2It is uniformly mixed with the powder of other third oxides, is calcined at 1000~1500 DEG C
After 1~10h, calcined powder is pressed into block under 5~15MPa pressure, being then split into quality is 10~100mg/
Block without container coagulated raw material；
(2) will without container coagulated raw material, pneumatic suspension makes its stable suspersion in the sky in oxygen, semiconductor laser and CO2Swash
Light device is heated to 1500~3000 DEG C simultaneously makes no container coagulated raw material 1~5min of molten condition, then with 100~400 DEG C/
The rate of temperature fall of s carries out cooling treatment, obtains the glass pellet that diameter is 2~6mm；
(3) it is 38~150 μm of glass powder that partial size is obtained after crushing glass pellet, under vacuum conditions, by glass powder according to
Predetermined shape rises to 800~900 DEG C with the heating rate of 5~20 DEG C/min, and hot pressed sintering is carried out under 10~90MPa pressure
10~60min obtains glass raw material；
(4) glass raw material is made annealing treatment to 1~15h at 600~800 DEG C.
10. a kind of purposes of the lanthanium titanate base glass sheet as described in one of claim 1-3, which is characterized in that the lanthanium titanate
Base glass sheet is applied to optical material field, is preferably used as the lens materials, camera lens material and up-conversion luminescence matrix of glasses
Material.
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Application publication date: 20181204 |