CN105481245B - Composition of scintillation glass for preparing flash fiber panel and preparation method thereof - Google Patents
Composition of scintillation glass for preparing flash fiber panel and preparation method thereof Download PDFInfo
- Publication number
- CN105481245B CN105481245B CN201510823059.5A CN201510823059A CN105481245B CN 105481245 B CN105481245 B CN 105481245B CN 201510823059 A CN201510823059 A CN 201510823059A CN 105481245 B CN105481245 B CN 105481245B
- Authority
- CN
- China
- Prior art keywords
- glass
- scintillation
- fiber panel
- crucible
- composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- 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
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
- G21K4/00—Conversion screens for the conversion of the spatial distribution of X-rays or particle radiation into visible images, e.g. fluoroscopic screens
Abstract
The invention discloses a kind of composition of scintillation glass for being used to prepare flash fiber panel and preparation method thereof, said composition includes the component of following weight percentage：SiO210~20%；Al2O30~10%；B2O320~45%；La2O330~60%；Nb2O50~2%；Gd2O35~25%；Lu2O30~4%；BaO 0~5%；SnO20~2%；ZnO 0~5%.The present invention also provides a kind of above-mentioned preparation method for being used to prepare the scintillation glass of flash fiber panel, comprises the following steps：1. weighing each raw material by raw material components, all raw materials are mixed and ground uniformly, obtain batch；Melted 2. batch is poured into crucible, glass melt is made.3. glass melt is cast in the heat-resisting steel mold by preheating, then it is placed in Muffle furnace and is incubated, then cools down annealing；4. scintillation glass is obtained after cutting, surface grinding, polishing.The present invention has that chemical stability is good, passage of scintillation light luminous efficiency is high, can be with drawing optical fiber the advantages of.
Description
Technical field
The present invention relates to glass material field, and in particular to a kind of group for being used to prepare the scintillation glass of flash fiber panel
Compound and preparation method thereof.
Background technology
The high-energy rays such as X ray can be converted into visible ray by scintillator material, additionally it is possible to realize the high score to object observing
Resolution aerial image, research and develop the successfully continuous improvement with performance with scintillator material so that the mankind are in high-energy physics, biology
The activity of medical technology, space exploration, industrial detection and nuclear detection technology etc. is enhanced and developed, and particularly X is penetrated
The high energy such as line X-ray diagnosis X and observation obtain in the acquisition of information and transmitting system of various biomedical and industrial emphasis equipment
It is widely applied.Conventional scintillator material has inorganic scintillation crystal, scintillation glass and organic scintillator etc., but flashes
Requirement of the crystal to equipment in preparation process is higher, prepares difficulty, expensive, and crystal growth is slow, crystal growth
Cycle is grown, and its high-volume and large scale production difficulty are big；And although organic scintillator light output is very high, flash speed is fast,
The density of organic scintillator is low, intolerant to irradiation, therefore with excellent radiation-resistant property, rapid decay time, high-resolution imaging
Scintillator material be Recent study heat subject.
Flash fiber panel is that light material is cladding by the use of the scintillation glass material of high index of refraction as core material
Draw the optical fiber formed and pass through permutation and combination, it is by the softening of cladding glass that optics is fine under conditions of temperature-pressure
An entirety together bonded to each other is tieed up, it is one to grow up in the technical foundation of scintillator material and fibre faceplate
Kind of new function device, it has been provided simultaneously with the function of scintillator material and fibre faceplate, have total reflection, zero optical thickness with
And spatial resolution it is high the characteristics of, it, which can be realized, is converted into visible ray output image to high-energy rays such as hard X ray, realize pair
The high resolution space imaging of object observing, can also form the integrated diagnostic system of special large information capacity, realizing to be obtained
Information carry out high-fidelity transmission；And because flash fiber panel employs the Unique physical design of optical fiber, it can
To be made very thick, the energy of the high-energy ray such as X ray can fully be deposited on longer path, and transformation efficiency is high, drop
The dosage radiated during the high energy radial imagings such as low X ray, the resolution ratio of imaging is improved, overcome traditional crystal film detection
The contradiction that existing detection efficient and resolution ratio mutually restrict, solves that single scintillation glass material energy resolution ratio is low to ask
Topic；And flash fiber panel preparation method is simple, cost is cheap, and optical property is readily obtained guarantee, it is easy to accomplish high-volume,
Large-sized industrialized production, prepare large-sized flash fiber panel.And high index of refraction, high density, resistance to irradiation, light output
Height, die-away time is short, response is fast, twilight sunset is short, sensitive to hard X ray, chemical stability is good, devitrification resistance energy is excellent, heat resistanceheat resistant is rushed
The scintillation glass material for hitting function admirable is to prepare the core material glass material of flash fiber panel, and core material glass material
Chemical composition can change in a wide range, and optical property is readily obtained guarantee, can design different points as needed
Resolution, prepare the different flash fiber panel of various scintillation properties.
The performance of scintillation glass mainly includes density, scintillation properties, radiation-resistant property etc., to meet to apply in high-energy irradiation
The requirement of flash fiber panel in environment, the scintillation glass for preparing flash fiber panel should have following performance：
(1) having higher density, (density is more than 5.0g/cm3)：Density is bigger, cut-off sheet of the glass material to X ray
Neck is bigger, and cascade unit x0 and Mo Liai (Moliere) radius Rm is just smaller, and small Mo Liai radiuses can reduce by two phases
Overlapping or interference between adjacent photoelectron, is easy to " recognize ", small cascade unit can reduce the volume of detector, so as to reduce
Cost.
(2) radiation-resistant property is excellent：Glass under the irradiation of the high-energy rays such as X ray, by cause glass color and luster and thoroughly
The decline of lightness, prevent the fluorescence that it sends from passing through or absorbed in itself by glass material, or even cause material structure defect.
(3) short persistence：Electronics will send photoelectron, in order to avoid between photoelectron from high level to during low energy order transition
Interfere with each other or pollute, it is desirable to carry out quick detection, quick detection requires fast blink, i.e., response is fast, twilight sunset is short.
(4) excellent heat processing technique performance：Devitrification resistance can be excellent, can be subjected under glass transition temperature for a long time
Heat distortion, it is drawn into optical fiber；With high index of refraction, ensure the high efficiency of transmission fluorescence under optical fiber state, in viscosity with cladding
Glass matches, and is advantageous to optical fiber shaping, while have good chemical stability and thermal shock resistance.
It is flicker that rear-earth-doped ion is the centre of luminescence it has been reported that in the scintillation glass crossed, studying at present more
Glass, and Ce3+Doping scintillation glass is luminous strong so as to influence it because quenching effect makes its introduction volume by larger limitation
Degree；And some rare earth ions to the light basicity sensitivity of glass, can make the ultraviolet and visible absorbance cutoff wavelength of glass produce red shift,
So as to influence the ultraviolet and visible light permeability of glass, and these scintillation glass materials are mainly single conduct scintillator material
Material uses, and its energy resolution is poor, it is impossible to realizes and the high resolution space of object observing is imaged, up to the present do not have also
Open report applied to the scintillation glass of flash fiber panel.
The content of the invention
The present invention is in order to solve the higher deficiency of cost of manufacture present in prior art, there is provided one kind has chemistry steady
Qualitative good, passage of scintillation light luminous efficiency height, can be with the composition for being used to prepare the scintillation glass of flash fiber panel of drawing optical fiber
And preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of composition for being used to prepare the scintillation glass of flash fiber panel, include the group of following weight percentage
Point：
Currently preferred technical scheme, include the component of following weight percentage：
The preferred technical scheme of the present invention, for preparing the scintillation glass of flash fiber panel, including following weight hundred
Divide the component of content：
1.75≤n of refractive index of the scintillation glassD≤1.85；In the mean coefficient of linear thermal expansion of 30~300 DEG C of scopes
For 63 × 10-7/ DEG C~90 × 10-7/℃；It is 600 DEG C~700 DEG C to expand softening point temperature scope.
The scintillation glass matches as the core material material for preparing flash fiber panel, the scintillation glass with cladding glass
Draw optical fibers, for preparing flash fiber panel.
The present invention also provides a kind of above-mentioned preparation method for being used to prepare the scintillation glass of flash fiber panel, including with
Lower step：
1. weighing each raw material by raw material components, all raw materials are mixed and ground uniformly, obtain batch；
2. the batch is poured into crucible, then crucible is put into glass furnace glass melt is made.
3. the glass melt is cast in the heat-resisting steel mold by preheating, then glass melt will be cast with again
Heat-resisting steel mold is placed in 500-700 DEG C of Muffle furnace and is incubated, then is annealed with stove cooling natural cooling；
4. the glass after annealing is passed through into cutting, surface grinding, polishes post-processing into sample, as scintillation glass.
The crucible is platinum crucible.
Crucible is put into glass furnace, is melting into glass melt, fusion temperature 1400~1500 under reducing atmosphere
DEG C, 6~9 hours are incubated after fusing, the gas in the reducing atmosphere includes the mixed gas or carbon monoxide of hydrogen and nitrogen.
It is that the mixed gas of hydrogen and nitrogen directly is passed through into dress that described hydrogen and the mixed gas reducing atmosphere of nitrogen, which obtain process,
Have in the crucible of batch, the acquisition process of CO gas reducing atmosphere is to put the small crucible equipped with carbon dust or graphite powder
2 hours are incubated in melting furnace.
The step 3. in, the preheating temperature of the heat-resisting steel mold is 400-600 DEG C, and it is small that 2-4 is incubated in Muffle furnace
When.
The step 4. in, the size after sample processing is 10mm × 10mm × 3mm.
Compared with prior art, it is an advantage of the invention that：
(1) there is high index of refraction (nDIt can reach 1.85), (density is more than 5.0g/cm to high density3), there is well transparent
Degree and radiation-resistant property；
(2) preparation technology is simple, chemical constituent is easy to adjustment, glass forming ability is strong, chemical stability is good, devitrification resistance
Energy is excellent, flash speed is fast, die-away time is short, passage of scintillation light luminous efficiency is high and has the viscosity to match with cladding glass
Characteristic, fibre-optical drawing is easily achieved, can be used for preparing flash fiber panel；
(3) emission peak is located near to the 550nm of human eye sensitivity, can be with CCD (charge coupling device) spectral response
Matching well, is prepared into flash fiber panel, is assembled into detector, can greatly improve to the detection efficient of high-energy ray and
The imaging resolution of device, realize to the position resolution of radiation source and aerial image detection, can be widely applied to X ray biology
The high energy X-ray detection X such as medical imaging and diagnosis, Application of Nuclear Technology, safety inspection and industrial detection field etc., is such as prepared into
Flash fiber panel is used in XRF screen, and the absorption to X ray is strong, in the absence of the scattering of transmitting light, therefore, has important
Application value and good application prospect.
Brief description of the drawings
Fig. 1 is the schematic cross-section of flash fiber panel prepared by scintillation glass of the present invention；
Fig. 2 is the schematic cross-section of the optical fiber of present invention composition flash fiber panel.
In figure：1 flash fiber panel, 2 optical fibers, 3 core material glass, 4 cladding glass.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings, but not as a limitation of the invention.
Referring to Fig. 1 and Fig. 2, core material glass 3 is externally provided with cladding glass 4, forms the optical fiber 2 of flash fiber panel, more
The individual permutation and combination of optical fiber 2 is into flash fiber panel 1.
Present invention offer is a kind of to be used to prepare scintillation glass of flash fiber panel and preparation method thereof, is matched somebody with somebody by following weight
The component composition of ratio：
In the present invention, SiO2It is the main body that glass forms skeleton, is the composition to be played a major role in glass skeleton.SiO2Contain
Amount is less than 10 weight %, is not easy to obtain the glass of excellent optical performance, while can reduce the chemical-resistant stability of glass；SiO2Contain
When amount is higher than 20 weight %, the high-temperature viscosity of glass can increase, and cause glass smelting temperature too high.Therefore, SiO2Weight hundred
It is 10~20 weight % to divide ratio, preferably 12~15 weight %.
Al2O3Belong to the intermediate oxide of glass, Al3+There are two kinds of co-ordination states, i.e., in tetrahedron or octahedron,
When oxygen is enough in glass, aluminum-oxygen tetrahedron [AlO is formed4], continuous network is formed with silicon-oxy tetrahedron, when oxygen in glass
When insufficient, alumina octahedral [AlO is formed6], it is in for network outer body in the hole of silica structure network, so necessarily containing
In the range of amount can and SiO2It is the main body that glass network is formed, suppresses the generation of glass phase-separating, improve the drawing of glass fibre
Condition.Al2O3Content is less than 3 weight %, the chemical resistance deficiency of glass, while can increase the crystallization tendency of glass；Al2O3Contain
Amount, which is more than 10 weight %, can dramatically increase glass high-temperature viscosity, raise the glass melting temperature of glass.Therefore, Al2O3Weight percent
Than for 0~10 weight %, preferably 0~7 weight %, more preferably 2~4 weight %.
B2O3And network former, and the composition of glass skeleton is formed, while be a kind of reduction glass smelting again
The cosolvent of viscosity, the glass melting temperature of glass can be reduced, improve glass fibre draw conditions.Boron oxygen triangle body [BO3] and boron
Oxygen tetrahedron [BO4] it is structural component, boron may be with triangle body [BO at different conditions3] or boron oxygen tetrahedron [BO4] exist,
In high temperature melting condition, it is generally more difficult to form boron oxygen tetrahedron, and can only be deposited in a manner of trihedral, but in low temperature,
B under certain condition3+Have and capture free oxygen and form tetrahedral trend, make close structure and improve the low temperature viscosity of glass, but by
There is the characteristic that high temperature reduces glass viscosity and low temperature improves glass viscosity in it, also determine that its content range is smaller.B2O3's
Content is less than 20 weight %, can not play a part of hydrotropy, while reduce the chemical stability of glass；B2O3Content be more than 45
Weight %, can reduce the refractive index of glass, while the split-phase of glass is inclined to increase.Therefore, B2O3Percentage by weight for 20~
45 weight %, preferably 25~35 weight %, more preferably 28~32 weight %.
La2O3It is lanthanide rare earth oxide, the refractive index and density of glass can be increased, be advantageous to light emitting ionic in glass
It is scattered, concentration quenching effect is reduced, improves the flashing performance of glass, La2O3Percentage by weight be 30~60 weight %,
Preferably 30~50 weight %, more preferably 36~38 weight %.But La2O3Content can cause glass when being more than 60 weight %
Thermal coefficient of expansion increase.
Nb2O5And rare earth oxide, the refractive index and density of glass can be increased, while the glass melting temperature of glass is reduced,
Nb2O5Percentage by weight be 0~2 weight %, preferably 1 weight %.Nb2O5Content can cause glass when being more than 2 weight %
Split-phase and thermal coefficient of expansion increase.
Gd2O3And rare earth oxide, the refractive index and density of glass can be increased, improve the flashing performance of glass,
Gd2O3Percentage by weight be 5~25 weight %, preferably 8~15 weight %, more preferably 13~14 weight %.But Gd2O3
Content can cause luminous intensity to reduce and concentration quenching effect when being more than 25 weight %.
Lu2O3And rare earth oxide, the refractive index and density of glass can be increased, while be advantageous to Gd3+Ion disperses,
Concentration quenching effect can be reduced, improves the flashing performance of glass, Lu2O3Percentage by weight be 0~4 weight %, preferably
For 1~3 weight %.Lu2O3Content can cause the cost of glass to increase when being more than 4 weight %.
BaO is glass structure network modifying oxide, can improve the density of glass, is advantageous to improve the resistance to spoke of scintillation glass
According to ability and radiationless loss is reduced, BaO percentage by weight is 0~5 weight %, preferably 2~4 weight %.BaO content
More than 5 weight %, glass chemical-resistant stability can be reduced, increases the tendency towards devitrification of glass.
ZnO is the glass melting temperature for reducing glass, Zn2+With stable valence state, the centre of luminescence is also used as, is carried
The performances such as the rate of decay and fluorescence intensity of high glass, ZnO percentage by weight are 0~5 weight %, preferably 1~4 weight
Measure %.ZnO content is more than 5 weight %, can reduce glass chemical-resistant stability and optical property.
SnO2It is the refining quality and glass uniformity for improving glass, it can be used as fining agent, and heat absorbing glass melts
Melt the minute bubbles in liquid, SnO2Percentage by weight be 0~2 weight %, preferably 1 weight %.SnO2Content be more than 2 weights
% is measured, the transmitance of glass can be reduced.
According to flash fiber panel (including fibre faceplate, optical fiber image inverter, optical fiber cone etc.), particularly for medical treatment etc.
The flash fiber panel in field is free from the boron of alkali metal oxide to the Property requirements of glass used, preferable glass types
Lanthanum silicate glass, the scintillation glass have that high index of refraction, high density, radiation-resistant property are good, flash speed is fast, twilight sunset is short, right
Hard X ray is sensitive, devitrification resistance energy is excellent, thermal shock resistance is excellent, chemical stability is good, passage of scintillation light luminous efficiency is high, can
The advantages that with drawing optical fiber.The scintillation glass of the present invention belongs to boron lanthanum silicate glass, in glass without alkali metal oxide with
And heavy metallic oxide such as As influential on scintillation properties2O3、Sb2O3、PbO、CdO、Bi2O3Deng even if containing and its pettiness
Amount be also due to other frits and brought into.
The present invention also provides a kind of preparation method for being used to prepare the scintillation glass of flash fiber panel, and preparation method is such as
Under：
(1) preparation of glass batch：By raw material, described component and content carry out recipe calculation and cooperation as requested
The preparation of material, glass batch is made after being sufficiently mixed and grinding uniformly.
(2) glass batch is founded：Platinum crucible is put into after glass batch obtained above is sufficiently mixed uniformly
In, melted in the glass furnace being placed under reducing atmosphere, the glass founded under reducing atmosphere condition can effectively improve glass
Flashing efficiency, the acquisition of reducing atmosphere is that the mixed gas of nitrogen and hydrogen directly is passed into the earthenware equipped with batch
In crucible, 1400~1500 DEG C of fusion temperature, 6~9 hours being incubated after fusing, during insulation carries out manually stirring 3 times to glass metal,
To improve the refining quality of glass metal and clear quality.
(3) glass metal of fusing is cast in heat-resisting steel mold of 400-600 DEG C by preheating, after then solidifying
Glass specimen move in 600 DEG C of Muffle furnace and anneal, insulation closed electric furnace after 3 hours, then furnace cooling Temperature fall
To room temperature.
(4) by after above-mentioned cooling glass by cutting, surface grinding, polishing post-processing into 10mm × 10mm ×
3mm sample is scintillation glass sample.
It is a kind of to the present invention to be used to prepare parameter and assay method and the instrument that the scintillation glass of flash fiber panel is determined
Device is as follows：
(1) refractive index nD[refractive index of glass during λ=589.3nm], glass refraction nDSurveyed using refraction index test instrument
It is fixed；
(2) 30~300 DEG C of mean thermal expansion coefficients α30/300[10-7/ DEG C], measured using horizontal expander instrument, with average line
The coefficient of expansion represents, is measured using method as defined in ISO7991；
(3) density (at room temperature)；Measured using Archimedes's drainage；
(4) launch wavelength, with excitation of X-rays sample, the flashing spectrum of scintillation glass produced by the present invention is obtained.
Raw materials used and ingredient requirement is as follows in following examples：
Wherein SiO2Introduce that (high-purity, ＞ 99.9%, 150 μm of oversizes are less than 1%, 45 μm of screenings by quartz sand
For less than 30%, Fe2O3Content is less than 0.01wt%), Al2O3Introduce by aluminium hydroxide and (analyze pure, 50 μm of average grain diameter),
B2O3(400 μm of oversizes are that less than 10%, 63 μm of screenings is less than 10%), La are introduced by boric anhydride2O3Pass through three oxidations two
Lanthanum introduces (5N), Nb2O5(5N), Gd are introduced by niobium pentaoxide2O3(5N), Lu are introduced by gadolinium sesquioxide2O3Pass through three
Aoxidize two lutetiums and introduce (5N), BaO is introduced by barium carbonate (analyzing pure, purity >=99.0%), and ZnO passes through zinc oxide (analysis is pure)
Introduce, SnO2It is to be introduced by tin ash (chemistry is pure).
Embodiment 1
First, raw material is selected by the glass ingredient of 1 embodiment of table 1, its dispensing is met the glass chemistry composition of table 1, pass through
Obtained glass batch, is subsequently poured into platinum crucible after being sufficiently mixed and grinding uniformly, in also Primordial Qi at a temperature of 1450 DEG C
Melted in glass furnace in atmosphere, directly the mixed gas of nitrogen and hydrogen is passed into the crucible equipped with batch and obtained
Reducing atmosphere, 8 hours are incubated after fusing, during insulation carries out manually stirring 3 times to glass metal, to improve the fusing matter of glass metal
Amount and clear quality, after glass batch is fused into the glass melt of homogeneous, glass melt is poured into the size of 500 DEG C of preheating
For castable in 70mm × 10mm × 10mm heat-resisting steel mold, then the glass specimen after solidification is moved in 600 DEG C
Made annealing treatment in Muffle furnace, insulation closed electric furnace after 3 hours, then furnace cooling Temperature fall is to room temperature, after cooling
By cutting, surface grinding, polishing post-processing, into 10mm × 10mm × 3mm sample, scintillation glass sample is made in glass
Test performance is as shown in table 2, and (1) refractive index is 1.83；(2) 30~300 DEG C of average coefficient of linear expansion 68 × 10-7/℃；(3)
Density 5.6g/cm3；(4) launch wavelength 460nm.
Embodiment 2
Raw material is selected by the glass ingredient of 1 embodiment of table 2, its dispensing is met the glass chemistry composition of table 1, by fully mixed
Glass batch is made after merging grinding uniformly, is subsequently poured into platinum crucible, in Carbon monoxide reduction at a temperature of 1400 DEG C
Melted in glass furnace in atmosphere, the acquisition process of CO gas reducing atmosphere is by equipped with carbon dust or graphite powder
Small crucible is placed in melting furnace and is incubated 2 hours.9 hours are incubated after fusing, during insulation carries out manually stirring 3 times to glass metal,
To improve the refining quality of glass metal and clear quality, after glass batch is fused into the glass melt of homogeneous, glass is melted
Castable in the heat-resisting steel mold that the size that body pours into 400 DEG C of preheating is 70mm × 10mm × 10mm, then by after solidification
Glass specimen is moved in 500 DEG C of Muffle furnace and made annealing treatment, and insulation closed electric furnace after 4 hours, then furnace cooling is certainly
Room temperature so is cooled to, the glass after cooling is by cutting, surface grinding, polishing post-processing into 10mm × 10mm × 3mm's
Sample, obtained scintillation glass sample test performance is as shown in table 2, and (1) refractive index is 1.81；(2) 30~300 DEG C of average line is swollen
Swollen coefficient 75 × 10-7/℃；(3) density 5.6g/cm3；(4) launch wavelength 450nm.
Embodiment 3
Raw material is selected by the glass ingredient of 1 embodiment of table 3, its dispensing is met the glass chemistry composition of table 1, by fully mixed
Glass batch is made after merging grinding uniformly, is subsequently poured into platinum crucible, at a temperature of 1500 DEG C in reducing atmosphere
Melted in glass furnace, directly the mixed gas of nitrogen and hydrogen is passed into the crucible equipped with batch and obtains also Primordial Qi
Atmosphere, 6 hours are incubated after fusing, during insulation carries out artificial stirring 3 times to glass metal, with improve the refining quality of glass metal with it is clear
Clear quality, it is 70mm by the size that glass melt pours into 600 DEG C of preheating after glass batch is fused into the glass melt of homogeneous
Castable in × 10mm × 10mm heat-resisting steel mold, then moves to the glass specimen after solidification in 700 DEG C of Muffle furnace
In made annealing treatment, insulation closed electric furnace after 2 hours, then furnace cooling Temperature fall arrives room temperature, and glass after cooling passes through
Cutting, surface grinding, polishing post-processing are crossed into 10mm × 10mm × 3mm sample, scintillation glass sample test is made
Can as shown in table 2, (1) refractive index is 1.85；(2) 30~300 DEG C of average coefficient of linear expansion 68 × 10-7/℃；(3) density
5.8g/cm3；(4) launch wavelength 470nm.
Embodiment 4
By the glass ingredient of 1 embodiment of table 4 select raw material, make its dispensing meet table 1 glass chemistry composition, and take with
The identical melting process system of embodiment 1 and test condition, the basic performance of sample is shown in table 2.(1) refractive index is 1.83；
(2) 30~300 DEG C of average coefficient of linear expansion 70 × 10-7/℃；(3) density 5.4g/cm3；(4) launch wavelength 460nm.
Embodiment 5
By the glass ingredient of 1 embodiment of table 5 select raw material, make its dispensing meet table 1 glass chemistry composition, and take with
The identical melting process system of embodiment 1 and test condition, the basic performance of sample is shown in table 2.(1) refractive index is 1.81；
(2) 30~300 DEG C of average coefficient of linear expansion 72 × 10-7/℃；(3) density 5.6g/cm3；(4) launch wavelength 430nm.
Embodiment 6
By the glass ingredient of 1 embodiment of table 6 select raw material, make its dispensing meet table 1 glass chemistry composition, and take with
The identical melting process system of embodiment 1 and test condition, the basic performance of sample is shown in table 2.(1) refractive index is 1.81；
(2) 30~300 DEG C of average coefficient of linear expansion 72 × 10-7/℃；(3) density 5.3g/cm3；(4) launch wavelength 430nm.
Embodiment 7
By the glass ingredient of 1 embodiment of table 7 select raw material, make its dispensing meet table 1 glass chemistry composition, and take with
The identical melting process system of embodiment 1 and test condition, the basic performance of sample is shown in table 2.(1) refractive index is 1.79；
(2) 30~300 DEG C of average coefficient of linear expansion 63 × 10-7/℃；(3) density 5.1g/cm3；(4) launch wavelength 460nm.
Embodiment 8
By the glass ingredient of 1 embodiment of table 8 select raw material, make its dispensing meet table 1 glass chemistry composition, and take with
The identical melting process system of embodiment 1 and test condition, the basic performance of sample is shown in table 2.(1) refractive index is 1.85；
(2) 30~300 DEG C of average coefficient of linear expansion 65 × 10-7/℃；(3) density 5.5g/cm3；(4) launch wavelength 460nm.
The composition of the 1-8 glass of the embodiment of the present invention of table 1
The performance of glass made from the 1-8 of the embodiment of the present invention of table 2
The data obtained by embodiment are it is known that the present invention is used to prepare flash fiber panel scintillation glass with height
Refractive index, high density, thermal shock resistance is excellent, and radiation-resistant property is good, and emission peak is located near to the 550nm of human eye sensitivity,
It can be suitable for preparing flash fiber panel (including fibre faceplate, optical fiber image inverter, optical fiber cone etc.) with drawing optical fiber.Should
Scintillation glass have excellent devitrification resistance energy, light output are high, die-away time is short, response is fast, twilight sunset is short, to hard X ray sensitivity,
Good chemical stability and optical property, the advantages of passage of scintillation light luminous efficiency is high.
One kind of embodiment described above, simply more preferably embodiment of the invention, those skilled in the art
The usual variations and alternatives that member is carried out in the range of technical solution of the present invention should all include within the scope of the present invention.
Claims (8)
1. a kind of composition for being used to prepare the scintillation glass of flash fiber panel, it is characterised in that contained by following weight percent
The component composition of amount：
1.75≤n of refractive index of the scintillation glassD≤1.85；30~300 DEG C of scopes mean coefficient of linear thermal expansion for 63 ×
10-7/ DEG C~90 × 10-7/℃；It is 600 DEG C~700 DEG C to expand softening point temperature scope.
2. the composition according to claim 1 for being used to prepare the scintillation glass of flash fiber panel, it is characterised in that bag
Include the component of following weight percentage：
3. the method that the composition described in usage right requirement 1 or 2 prepares the scintillation glass for flash fiber panel, its feature
It is, comprises the following steps：
1. weighing each raw material by raw material components, all raw materials are mixed and ground uniformly, obtain batch；
2. the batch is poured into crucible, then crucible is put into glass furnace glass melt is made；
3. the glass melt is cast in the heat-resisting steel mold by preheating, then the heat-resisting of glass melt will be cast with again
Steel mold is placed in 500-700 DEG C of Muffle furnace and is incubated, then is annealed with stove cooling natural cooling；
4. the glass after annealing is passed through into cutting, surface grinding, polishes post-processing into sample, as scintillation glass.
4. according to the method for claim 3, it is characterised in that the crucible is platinum crucible.
5. according to the method for claim 3, it is characterised in that the step 2. in, crucible is put into glass furnace,
Glass melt is melting under reducing atmosphere, 1400~1500 DEG C of fusion temperature, 6~9 hours is incubated after fusing.
6. according to the method for claim 3, it is characterised in that the step 3. in, the preheating temperature of the heat-resisting steel mold
Spend for 400-600 DEG C, 2-4 hours are incubated in Muffle furnace.
7. according to the method for claim 3, it is characterised in that the step 4. in, the size after sample processing is
10mm×10mm×3mm。
8. according to the method for claim 5, it is characterised in that gas in the reducing atmosphere includes hydrogen and nitrogen
Mixed gas or carbon monoxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510823059.5A CN105481245B (en) | 2015-11-23 | 2015-11-23 | Composition of scintillation glass for preparing flash fiber panel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510823059.5A CN105481245B (en) | 2015-11-23 | 2015-11-23 | Composition of scintillation glass for preparing flash fiber panel and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105481245A CN105481245A (en) | 2016-04-13 |
| CN105481245B true CN105481245B (en) | 2017-12-05 |
Family
ID=55668576
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510823059.5A Active CN105481245B (en) | 2015-11-23 | 2015-11-23 | Composition of scintillation glass for preparing flash fiber panel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105481245B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106443754B (en) * | 2016-11-16 | 2019-02-01 | 奕瑞影像科技（太仓）有限公司 | Radioscopic image capturing apparatus |
| CN106698925A (en) * | 2017-02-22 | 2017-05-24 | 吉林师范大学 | Terbium ion-activated scintillating optical fiber panel and preparation method thereof |
| CN110128006B (en) * | 2019-06-21 | 2022-05-10 | 鲁米星特种玻璃科技股份有限公司 | Environment-friendly high-refractive-index ultraviolet-transmitting glass and preparation method thereof |
| CN114772922B (en) * | 2022-04-14 | 2024-01-26 | 中国建筑材料科学研究总院有限公司 | Scintillator glass for electromagnetic energy device, preparation method thereof, melting device and application |
| CN115536283B (en) * | 2022-09-09 | 2023-10-24 | 中国建筑材料科学研究总院有限公司 | High refractive index fiber core glass for optical fiber image transmission element and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5747397A (en) * | 1996-11-04 | 1998-05-05 | Bay Glass Research | Optical glass |
| CN101293736A (en) * | 2007-04-23 | 2008-10-29 | 亚洲光学股份有限公司 | Optical glass |
| CN101712530A (en) * | 2008-09-30 | 2010-05-26 | Hoya株式会社 | Optical glass |
| CN103482867A (en) * | 2013-08-30 | 2014-01-01 | 中国建筑材料科学研究总院 | Environment-friendly high-refractivity glass for optical fiber faceplate and optical element |
| CN103693847A (en) * | 2013-11-06 | 2014-04-02 | 中国科学院上海光学精密机械研究所 | Gadolinium borosilicate scintillating glass and preparation method thereof |
-
2015
- 2015-11-23 CN CN201510823059.5A patent/CN105481245B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5747397A (en) * | 1996-11-04 | 1998-05-05 | Bay Glass Research | Optical glass |
| CN101293736A (en) * | 2007-04-23 | 2008-10-29 | 亚洲光学股份有限公司 | Optical glass |
| CN101712530A (en) * | 2008-09-30 | 2010-05-26 | Hoya株式会社 | Optical glass |
| CN103482867A (en) * | 2013-08-30 | 2014-01-01 | 中国建筑材料科学研究总院 | Environment-friendly high-refractivity glass for optical fiber faceplate and optical element |
| CN103693847A (en) * | 2013-11-06 | 2014-04-02 | 中国科学院上海光学精密机械研究所 | Gadolinium borosilicate scintillating glass and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105481245A (en) | 2016-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105481245B (en) | Composition of scintillation glass for preparing flash fiber panel and preparation method thereof | |
| CN105293905B (en) | A kind of flash fiber panel and preparation method thereof | |
| CN105967514B (en) | Lanthanide flint optical glass | |
| Boulos et al. | Structure and properties of silver borate glasses | |
| CN106517772B (en) | The light and preparation method thereof of fibre faceplate is prepared for pulling plate molding | |
| CN103482867B (en) | A kind of environment-friendly type glass of high refractive index for fibre faceplate and optical element | |
| CN111393023B (en) | High-definition optical fiber image inverter and preparation method and application thereof | |
| CN110240402B (en) | Environment-friendly deep ultraviolet-transmitting borosilicate glass and preparation method and application thereof | |
| Marzouk et al. | Optical, structural and thermal properties of sodium metaphosphate glasses containing Bi2O3 with interactions of gamma rays | |
| CN111410423B (en) | Light absorption frit glass for optical fiber image transmission element and preparation method thereof | |
| WO2023147757A1 (en) | Light absorption material glass for high-contrast optical fiber inverter, and preparation method therefor | |
| CN106565085B (en) | Optical glass composition, optical glass and its preparation method and application | |
| WO2023147756A1 (en) | Preparation method and use for φ40 mm large-size high-contrast optical fiber inverter | |
| CN115536283B (en) | High refractive index fiber core glass for optical fiber image transmission element and preparation method thereof | |
| CN108609848A (en) | A kind of ultra high density boron germanium tellurate scintillation glass and preparation method thereof | |
| Huang et al. | Characterization of Fe2O3 doping on structure, optical and luminescence properties of magnesium aluminosilicate-based glasses | |
| CN110255898B (en) | Deep ultraviolet transparent glass, preparation method, application and melting device thereof | |
| CN116253507B (en) | High-refractive-index radiation-resistant glass material, and preparation method and application thereof | |
| CN110451798A (en) | A kind of divalent europium activation lithium borate salts scintillation glass and preparation method thereof | |
| CN103951206B (en) | Rare earth ion doped BaGdBr5Devitrified glass and preparation method thereof | |
| CN103951240B (en) | Rare earth ion doped Cs2liLaCl6devitrified glass and preparation method thereof | |
| CN115453680A (en) | 3 micron optical fiber component and preparation method thereof | |
| CN110128006B (en) | Environment-friendly high-refractive-index ultraviolet-transmitting glass and preparation method thereof | |
| CN103951223B (en) | Rare earth ion doped Ba2CsI5Devitrified glass and preparation method thereof | |
| CN103951198B (en) | Rare earth ion doped Cs2LiGdBr6Devitrified glass and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 100024 No. 1, East Lane, Chaoyang District, Beijing, Guanzhuang Patentee after: CHINA BUILDING MATERIALS ACADMEY Address before: 100024 No. 1, East Lane, Chaoyang District, Beijing, Guanzhuang Patentee before: CHINA BUILDING MATERIALS ACADEMY |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220130 Address after: 277102 No. 67, Renmin West Road, Shizhong District, Zaozhuang City, Shandong Province Patentee after: China building materials Photon Technology Co.,Ltd. Address before: 100024 No. 1, East Lane, Chaoyang District, Beijing, Guanzhuang Patentee before: CHINA BUILDING MATERIALS ACADMEY |