CN105712633A - Glass ceramic for laser protection and preparation method of glass ceramic - Google Patents

Glass ceramic for laser protection and preparation method of glass ceramic Download PDF

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CN105712633A
CN105712633A CN201610022496.1A CN201610022496A CN105712633A CN 105712633 A CN105712633 A CN 105712633A CN 201610022496 A CN201610022496 A CN 201610022496A CN 105712633 A CN105712633 A CN 105712633A
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glass
lasing safety
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CN105712633B (en
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何峰
谢峻林
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Wuhan University of Technology WUT
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    • 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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a glass ceramic material for laser protection and a preparation method of the glass ceramic material. Base glass of the glass ceramic material comprises the following oxidized components: SiO2 (54wt%-64wt%), Al2O3 (18wt%-22wt%), Li2O (3wt%-5wt%), SrO (3wt%-5wt%), MgO (3wt%-5wt%), B2O3 (0.5wt%-1.5wt%), Na2O (0.4wt%-0.8wt%), TiO2 (2wt%-3wt%), ZrO2 (2wt%-3wt%), Er2O3 (2wt%-3wt%), Bi2O3 (0.5wt%-1.5wt%), Co2O3 (0.2wt%-0.4wt%) and Sb2O3 (0.1wt%-0.3wt%). The obtained glass ceramic has specific absorption capability at various laser bands in a range from 300-1,000 nm (expect 805-815 nm and 975-985 nm), so that the transmissivity of laser in the bands is lower than 20%.

Description

Devitrified glass for lasing safety and preparation method thereof
Technical field
The invention belongs to technical field of composite materials, be specifically related to a kind of for lasing safety microcrystal glass material and preparation method thereof.
Background technology
Laser has good directionality, brightness is high, monochromaticity is good and the feature such as high-energy-density.Laser work based on laser instrument Industry is persistent rapidly in global evolution, be now widely used in commercial production, communication, information processing, health care, military affairs, The aspect such as cultural education and scientific research.Laser weapon is that a kind of laser beam utilizing directional transmissions is directly injured target or is allowed to lose efficacy Directed energy weapon.Laser weapon constitutes threat greatly to human body and equipment, and eyes are the organs that human body is most sensitive to laser, Owing to the focussing force of light can be made energy density on retina increase 10 by eye5Times, therefore low dose exposure just can cause retina Major injury and cause visual deterioration until blind.How to carry out effective lasing safety and become the problem that people extremely pay close attention to.
Existing absorption-type laser protective material, absorbs incident laser by absorbing medium and makes laser energy weaken, to reach anti-sharp The purpose of light.This protective material has shaped plastics and glass mould two kinds.Shaped plastics is to add to absorb the organic of laser in optical plastic Dyestuff, advantage be make optical density height, light weight, price is low, it is convenient to prepare；Shortcoming be the most aging, case hardness is low, chemically-resistant Agents difference, easily there is photobleaching.Glass mould is to add inorganic dyestuff during glass melting to make, and which overcomes plastics and prevents The shortcoming of protective material, but absorbent wavelength is little, currently also has the method using low smelting heat that glass mould can be made to realize equally Multiband protects.The common drawback of the absorption protective glasses of both is: be easily caused destruction itself owing to absorbing laser energy；Light Sharp cut-off performance bad, cause visible light transmissivity the highest, impact observe.
Summary of the invention
It is an object of the invention to the deficiency for existing absorption-type laser protective material, it is provided that a kind of Multi-wavelength Laser Protective crystallite glass Glass material and preparation method thereof.
For reaching above-mentioned purpose, use technical scheme as follows:
For the devitrified glass of lasing safety, the oxidation panel of its parent glass becomes: SiO2(54wt%-64wt%), Al2O3(18 Wt%-22wt%), Li2O (3wt%-5wt%), SrO (3wt%-5wt%), MgO (3wt%-5wt%), B2O3(0.5 Wt%-1.5wt%), Na2O (0.4wt%-0.8wt%), TiO2(2wt%-3wt%), ZrO2(2wt%-3wt%), Er2O3 (2wt%-3wt%), Bi2O3(0.5wt%-1.5wt%), Co2O3(0.2wt%-0.4wt%), Sb2O3(0.1wt%-0.3 Wt%)；Correspond used raw material be respectively as follows: silicon dioxide, alumina powder, lithium carbonate, strontium carbonate, magnesium carbonate, Boric acid, soda, titanium oxide, zirconium oxide, Erbia, bismuth oxide, cobalt sesquioxide and antimony oxide.
By such scheme, the oxidation panel of preferred parent glass becomes: SiO2(54wt%), Al2O3(22wt%), Li2O(4.3 Wt%), SrO (5wt%), MgO (5wt%), B2O3(1.5wt%), Na2O (0.4wt%), TiO2(3wt%), ZrO2(2wt%), Er2O3(2wt%), Bi2O3(0.5wt%), Co2O3(0.2wt%), Sb2O3(0.1wt%).
By such scheme, the oxidation panel of preferred parent glass becomes: SiO2(59wt%), Al2O3(20wt%), Li2O(4 Wt%), SrO (3wt%), MgO (3wt%), B2O3(0.5wt%), Na2O (0.5wt%), TiO2(2wt%), ZrO2(3wt%), Er2O3(3wt%), Bi2O3(1.5wt%), Co2O3(0.3wt%), Sb2O3(0.2wt%).
By such scheme, the oxidation panel of preferred parent glass becomes: SiO2(64wt%), Al2O3(18wt%), Li2O(3 Wt%), SrO (3wt%), MgO (3wt%), B2O3(1wt%), Na2O (0.5wt%), TiO2(2.5wt%), ZrO2(2wt%), Er2O3(2wt%), Bi2O3(0.5wt%), Co2O3(0.2wt%), Sb2O3(0.3wt%).
The above-mentioned devitrified glass preparation method for lasing safety, comprises the following steps:
1) raw material is mixed to get glass batch, melts at 1580-1620 DEG C and be incubated 4-6h；Cast molding in a mold, Putting in Muffle furnace and anneal, annealing temperature is limited to 580-620 DEG C up and down；Obtain annealed glass sheet material；
2) annealed glass sheet material is carried out in Muffle furnace coring and crystallization and thermal treatment；Gained glass Tg temperature is directly risen to from room temperature More than spending, 50-80 DEG C carries out coring, and the time is 4-6h；Then temperature being warming up to 780-880 DEG C and carry out crystallization, the time is 4-6h； The devitrified glass for lasing safety is i.e. obtained after cooling.
Devitrified glass has the most excellent many performance as the structural material that a class is special.The highly crystal grain chi of crystallization devitrified glass Very little can control, in the range of tens to hundreds of nanometer, obtains ultra-fine grain structure.In lithium strontium aluminum silicon transparent glass-ceramics, Due to abundant coring, parent glass forms substantial amounts of strontium titanates nucleus, β-quartz solid solution crystalline phase at nucleus Epitaxial growth, Form average grain size about 60nm uniform ultra-fine grain structure.Owing to crystallite dimension is much smaller than visible wavelength, and β- The birefringence of quartz solid solution is relatively low, and this devitrified glass light transmittance is the highest.The most crucially at lithium strontium aluminum silicon transparent microcrystal glass In the component of glass, by adding Erbia, can to control glass to the absorption of different-waveband laser and be glass for bismuth oxide, cobalt oxide Glass colours, so that this microcrystal glass material has lasing safety ability.This technology of preparing can prepare different specification size Microcrystal glass material is for the protection of human eye with equipment.
Comparing existing absorption-type laser protective material, the present invention has the advantage that
Principal crystalline phase in the devitrified glass that the present invention prepares is nano level β-quartz solid solution crystalline phase, and a small amount of nanoscale Spodumene crystallite phase, the expansion coefficient of this lasing safety devitrified glass is in 0.5-5 × 10-6℃-1.The low coefficient of expansion makes The performance with extraordinary heat shock resistance and mechanical shock.
The nano crystalline glass of the present invention has certain transparent characteristic, devitrified glass in the range of 300～1000nm (except 805～ 815nm, 975～985nm) multiple laser wavelength at obtain specific absorbability so that the laser absorbance of band above It is below 20%.
Accompanying drawing explanation
Fig. 1: embodiment 1 devitrified glass transmittance curve in the range of 300～1000nm.
Detailed description of the invention
Following example explain technical scheme further, but not as limiting the scope of the invention.
Embodiment 1
One lasing safety microcrystal glass material of the present invention and preparation method thereof is as follows:
A. the oxidation panel of parent glass becomes: SiO2(54wt%), Al2O3(22wt%), Li2O (4.3wt%), SrO (5 Wt%), MgO (5wt%), B2O3(1.5wt%), Na2O (0.4wt%), TiO2(3wt%), ZrO2(2wt%), Er2O3(2wt%), Bi2O3(0.5wt%), Co2O3(0.2wt%), Sb2O3(0.1wt%).Correspond and used Raw material be chemical pure industrial chemicals, correspond to respectively: silicon dioxide, alumina powder, lithium carbonate, strontium carbonate, magnesium carbonate, Boric acid, soda, titanium oxide, zirconium oxide, Erbia, bismuth oxide, cobalt sesquioxide and antimony oxide.
B. carry out preparing glass charge with above-mentioned industrial chemicals, including burdening calculation, weigh, the process such as mixing.
C. putting in corundum crucible by glass batch, melt in silicon molybdenum stove, temperature range is 1580 DEG C, is incubated 4 Hour.The vitreous humour melted is cast into plate-like in the graphite jig of heat, is then placed in Muffle furnace annealing, annealing Temperature is limited to 580-620 DEG C up and down.
D. the glass board material annealed is put in Muffle furnace, carry out coring and crystallization and thermal treatment, i.e. directly rise to glass from room temperature More than Tg temperature 50 DEG C of coring carrying out glass, the time is 6 hours, then temperature is warming up to 780 DEG C and carries out crystallization, time Between be 6 hours.
E. through Overheating Treatment, completing coring, after the process of crystallization, glass-ceramic panel is by i.e. obtaining crystallite after cooling down to room temperature Glass, the principal crystalline phase in devitrified glass is nano level β-quartz solid solution crystalline phase, and a small amount of nano level spodumene crystallite Phase, the expansion coefficient of this lasing safety devitrified glass is 5 × 10-6℃-1。
F. obtained devitrified glass is ground, polishes so that it is surface reaches optics two grades.
The present embodiment product carries out laser transmittance test, and result is referring to the drawings shown in 1.(remove in the range of 300～1000nm 805～815nm, 975～985nm) multiple laser wavelength at obtain specific absorbability；And the laser transmission of this wave band Rate is below 20%.Personnel, the equipment different demands to lasing safety wavelength can be met well.
Embodiment 2
A. the oxidation panel of parent glass becomes: SiO2(59wt%), Al2O3(20wt%), Li2O (4wt%), SrO (3wt%), MgO (3wt%), B2O3(0.5wt%), Na2O (0.5wt%), TiO2(2wt%), ZrO2(3wt%), Er2O3 (3wt%), Bi2O3(1.5wt%), Co2O3(0.3wt%), Sb2O3(0.2wt%).Correspond used former Material is chemical pure industrial chemicals, corresponds to respectively: silicon dioxide, alumina powder, lithium carbonate, strontium carbonate, magnesium carbonate, boron Acid, soda, titanium oxide, zirconium oxide, Erbia, bismuth oxide, cobalt sesquioxide and antimony oxide.
B. carry out preparing glass charge with above-mentioned industrial chemicals, including burdening calculation, weigh, the process such as mixing.
C. putting in corundum crucible by glass batch, melt in silicon molybdenum stove, temperature range is 1600 DEG C, is incubated 5 Hour.The vitreous humour melted is cast into plate-like in the graphite jig of heat, is then placed in Muffle furnace annealing, annealing Temperature is limited to 580-620 DEG C up and down.
D. the glass board material annealed is put in Muffle furnace, carry out coring and crystallization and thermal treatment, i.e. directly rise to glass from room temperature More than Tg temperature 70 DEG C of coring carrying out glass, the time is 5 hours, then temperature is warming up to 830 DEG C and carries out crystallization, time Between be 5 hours.
E. through Overheating Treatment, completing coring, after the process of crystallization, glass-ceramic panel is by i.e. obtaining crystallite after cooling down to room temperature Glass, the principal crystalline phase in devitrified glass is nano level β-quartz solid solution crystalline phase, and a small amount of nano level spodumene crystallite Phase, the expansion coefficient of this lasing safety devitrified glass is 2 × 10-6℃-1。
F. obtained devitrified glass is ground, polishes so that it is surface reaches optics two grades.Transparent nano crystallite can be made Glass obtains specific in the range of 300～1000nm at multiple laser wavelength (except 805～815nm, 975～985nm) Absorbability.The laser absorbance of band above is below 20%.Personnel, equipment can be met well to lasing safety ripple Long different demands.
Embodiment 3
A. the oxidation panel of parent glass becomes: SiO2(64wt%), Al2O3(18wt%), Li2O (3wt%), SrO (3wt%), MgO (3wt%), B2O3(1wt%), Na2O (0.5wt%), TiO2(2.5wt%), ZrO2(2wt%), Er2O3 (2wt%), Bi2O3(0.5wt%), Co2O3(0.2wt%), Sb2O3(0.3wt%).Correspond used former Material is chemical pure industrial chemicals, corresponds to respectively: silicon dioxide, alumina powder, lithium carbonate, strontium carbonate, magnesium carbonate, boron Acid, soda, titanium oxide, zirconium oxide, Erbia, bismuth oxide, cobalt sesquioxide and antimony oxide.
B. carry out preparing glass charge with above-mentioned industrial chemicals, including burdening calculation, weigh, the process such as mixing.
C. putting in corundum crucible by glass batch, melt in silicon molybdenum stove, temperature range is 1620 DEG C, is incubated 6 Hour.The vitreous humour melted is cast into plate-like in the graphite jig of heat, is then placed in Muffle furnace annealing, annealing Temperature is limited to 580-620 DEG C up and down.
D. the glass board material annealed is put in Muffle furnace, carry out coring and crystallization and thermal treatment, i.e. directly rise to glass from room temperature More than Tg temperature 80 DEG C of coring carrying out glass, the time is 4 hours, then temperature is warming up to 880 DEG C and carries out crystallization, time Between be 6 hours.
E. through Overheating Treatment, completing coring, after the process of crystallization, glass-ceramic panel is by i.e. obtaining crystallite after cooling down to room temperature Glass, the principal crystalline phase in devitrified glass is nano level β-quartz solid solution crystalline phase, and a small amount of nano level spodumene crystallite Phase, the expansion coefficient of this lasing safety devitrified glass is 0.5 × 10-6℃-1。
F. obtained devitrified glass is ground, polishes so that it is surface reaches optics two grades.Transparent nano crystallite can be made Glass obtains specific in the range of 300～1000nm at multiple laser wavelength (except 805～815nm, 975～985nm) Absorbability.The laser absorbance of band above is below 20%.Personnel, equipment can be met well to lasing safety ripple Long different demands.

Claims (5)

1. for the devitrified glass of lasing safety, it is characterised in that the oxidation panel of parent glass becomes: SiO2(54wt%-64wt%), Al2O3(18wt%-22wt%), Li2O (3wt%-5wt%), SrO (3wt%-5wt%), MgO (3wt%-5wt%), B2O3(0.5wt%-1.5wt%), Na2O (0.4wt%-0.8wt%), TiO2(2wt%-3wt%), ZrO2(2wt%-3wt%), Er2O3(2wt%-3wt%), Bi2O3(0.5wt%-1.5wt%), Co2O3(0.2wt%-0.4wt%), Sb2O3(0.1wt%-0.3 Wt%)；Correspond used raw material be respectively as follows: silicon dioxide, alumina powder, lithium carbonate, strontium carbonate, magnesium carbonate, Boric acid, soda, titanium oxide, zirconium oxide, Erbia, bismuth oxide, cobalt sesquioxide and antimony oxide.
2. as claimed in claim 1 for the devitrified glass of lasing safety, it is characterised in that the oxidation panel of parent glass becomes: SiO2 (54wt%), Al2O3(22wt%), Li2O (4.3wt%), SrO (5wt%), MgO (5wt%), B2O3(1.5wt%), Na2O (0.4wt%), TiO2(3wt%), ZrO2(2wt%), Er2O3(2wt%), Bi2O3(0.5wt%), Co2O3 (0.2wt%), Sb2O3(0.1wt%).
3. as claimed in claim 1 for the devitrified glass of lasing safety, it is characterised in that the oxidation panel of parent glass becomes: SiO2 (59wt%), Al2O3(20wt%), Li2O (4wt%), SrO (3wt%), MgO (3wt%), B2O3(0.5wt%), Na2O (0.5wt%), TiO2(2wt%), ZrO2(3wt%), Er2O3(3wt%), Bi2O3(1.5wt%), Co2O3 (0.3wt%), Sb2O3(0.2wt%).
4. as claimed in claim 1 for the devitrified glass of lasing safety, it is characterised in that the oxidation panel of parent glass becomes: SiO2 (64wt%), Al2O3(18wt%), Li2O (3wt%), SrO (3wt%), MgO (3wt%), B2O3(1wt%), Na2O (0.5wt%), TiO2(2.5wt%), ZrO2(2wt%), Er2O3(2wt%), Bi2O3(0.5wt%), Co2O3 (0.2wt%), Sb2O3(0.3wt%).
5. any one of claim 1-4 is for the devitrified glass preparation method of lasing safety, it is characterised in that comprise the following steps:
1) described raw material is mixed to get glass batch, melts at 1580-1620 DEG C and be incubated 4-6h；Cast in a mold Molding, puts in Muffle furnace and anneals, and annealing temperature is limited to 580-620 DEG C up and down；Obtain annealed glass sheet material；
2) annealed glass sheet material is carried out in Muffle furnace coring and crystallization and thermal treatment；Gained glass Tg temperature is directly risen to from room temperature More than spending, 50-80 DEG C carries out coring, and the time is 4-6h；Then temperature being warming up to 780-880 DEG C and carry out crystallization, the time is 4-6h； The devitrified glass for lasing safety is i.e. prepared after cooling.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109336398A (en) * 2018-11-05 2019-02-15 华南理工大学 A kind of application of microcrystal glass material
CN114212985A (en) * 2021-12-14 2022-03-22 华南理工大学 Preparation method of microcrystalline glass based on defect-induced spatially selective crystallization

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109336398A (en) * 2018-11-05 2019-02-15 华南理工大学 A kind of application of microcrystal glass material
CN114212985A (en) * 2021-12-14 2022-03-22 华南理工大学 Preparation method of microcrystalline glass based on defect-induced spatially selective crystallization

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