CN104692658A - Method for fixing CdS and Se in borosilicate glass - Google Patents

Method for fixing CdS and Se in borosilicate glass Download PDF

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CN104692658A
CN104692658A CN201510089568.XA CN201510089568A CN104692658A CN 104692658 A CN104692658 A CN 104692658A CN 201510089568 A CN201510089568 A CN 201510089568A CN 104692658 A CN104692658 A CN 104692658A
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glass
cds
frit
borosilicate
matrix
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李宏
陈方祎
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a method for fixing CdS and Se in borosilicate glass. The method is characterized by comprising the following steps: firstly, uniformly mixing CdS and Se with ZnO, insulating at 300-400 DEG C for 0.5-2 hours, uniformly mixing with a borosilicate matrix glass material, and adding zinc powder to manufacture a weakly reducing atmosphere; then, putting the borosilicate matrix glass material in a furnace at 700-1000 DEG C, heating to 1200-1350 DEG C, insulating for 0.5-2 hours and discharging; finally, molding in a heat-resistance mold, annealing at 400-500 DEG C for 0.5-1.5 hours, and cooling along with the furnace to obtain bulk cadmium sulfide selenide colored glass. Volatilization of CdS and Se can be reduced by adopting the method. According to the method, a good solution is provided to manufacture of cadmium sulfide selenide quantum dot glass and cadmium sulfide selenide colored glass, and conditions are created to studies on characteristics and performance of quantum dots in the cadmium sulfide selenide quantum dot glass. The cadmium sulfide selenide quantum dot glass can be used in photo-electric fields of construction decoration, white light LED, solar cells and the like.

Description

A kind of method of fixation of Cd S and Se in borosilicate glass
Technical field
The present invention relates to coloured glass and Quantum Dot Glass and devitrified glass preparation field, be specifically related to a kind of method of fixation of Cd S and Se in borosilicate glass.
Background technology
In recent years, quantum dot relies on the photoelectric characteristic of himself uniqueness to be more and more subject to people's attention, and becomes the focus of research.Quantum dot, as the state-of-the art fluorescent material of one, has multiple advantage compared with traditional organic dye molecule, and wherein maximum advantage is Color tunable.The quanta point material of single kind just can produce the monochromatic ray of different colours, even white light according to its dimensional change.In addition, it also has exciting light spectrum width and continuous distribution, and emmission spectrum monochromaticity is good, stability high.CdS xse 1-xquantum dot can produce the light from yellow to red colour system train wave section, and due to the snappiness of glass basis network internal key, and glass is easy to preparation and compatible with optical fiber, so glass is very desirable semiconductor-quantum-point body material.Cadmium sulphoselenide glass occupies an important position in coloured glass, manufacture the glass that in yellow, red glass, color is the purest, absorption curves is the most precipitous at present, and the retention of color of selenium cadmium sulfide stained glass is poor, easily precipitate during volatile during the tinting material high temperature such as CdS, Se, low temperature, be difficult to accurately control glass colour, be also not easy to obtain Quantum Dot Glass.
For this reason, the present invention proposes a kind of method of fixation of Cd S and Se in borosilicate glass, basic problem is solved for manufacturing cadmium sulfoselenide coloured glass and Quantum Dot Glass and devitrified glass, adopt suitable cadmium sulfoselenide pretreatment mode, suitable blowing temperature (700 DEG C-1000 DEG C) and glass melting temperature (1200 DEG C-1350 DEG C, insulation 0.5-2 hour), ground fixation of Cd S and Se can being imitated, creating good condition for preparing selenium cadmium sulfide stained glass, Quantum Dot Glass and devitrified glass.
Do not retrieve and a kind of patent that fixation of Cd S is identical with the method for Se in borosilicate glass.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method providing fixation of Cd S and Se in borosilicate glass, to reduce the volatilization of CdS and Se, can obtain the cadmium sulphoselenide glass of colour stable.
The present invention solves its technical problem and adopts following technical scheme:
A method of fixation of Cd S and Se in borosilicate glass, is characterized in that comprising the steps:
1) borosilicate matrix frit is prepared;
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO.The add-on of CdS is the 1-2% of borosilicate matrix frit quality, and the add-on of Se is the 0.2-0.7% of borosilicate matrix frit quality, and the add-on of ZnO is the 5-15% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 0.5-2 hour 300-400 DEG C of insulation, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, crucible is poured into after mixing, at 700-1000 DEG C, crucible is put into kiln, be warmed up to 1200 DEG C-1350 DEG C insulations discharging in 0.5-2 hour, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 400-500 DEG C of annealing 0.5-1.5 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
Described step 1) prepare borosilicate matrix frit and be:
1. by B 2o 3, SiO 2, Al 2o 3, Na 3alF 6, CaO and R 2o as raw material, incorporation zinc powder (Zn:0.5-3%), wherein B 2o 3by H 3bO 3introduce, R 2o is by R 2cO 3introduce, CaO is by CaCO 3introduce,
Component and the mass percent of borosilicate matrix frit are: SiO 2: 55-70%, R 2o:15-25%, B 2o 3: 2%-7%, Al 2o 3: 0.5-5%, Na 3alF 6: 0.5-5%, CaO:0.5-5%, Zn:0.5-3%, described R 2o refers to Li 2o, Na 2o, K 2a kind of or several mixing by any proportioning arbitrarily during O is any;
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3, CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit.
The step 1. middle H of described preparation borosilicate matrix frit 3bO 3introduction volume should consider the volatile quantity of its 10% (quality).
The present invention compared with prior art, there is following main advantage: owing to devising suitable borosilicate matrix glass composition, improve the melting technology of glass, at utmost optimize the method for fixation of Cd S and Se, the cadmium sulphoselenide glass of colour stable can being obtained, creating good condition for preparing selenium cadmium sulfide stained glass, Quantum Dot Glass and devitrified glass.Quantum dot, as a kind of novel fluorescent material, has multiple advantage compared with traditional organic dye molecule, and wherein maximum advantage is Color tunable.The quanta point material of single kind just can produce the monochromatic ray of different colours, even white light according to its dimensional change.In addition, it also has exciting light spectrum width and continuous distribution, and emmission spectrum monochromaticity is good, stability high.CdS xse 1-xquantum dot can produce the light from yellow to red colour system train wave section, can improve the problems such as the luminescent properties of white light LEDs.
Accompanying drawing explanation
Mass percent shared by each composition in X-ray fluorescence spectra analysis (XRF) test that table 1 is the embodiment of the present invention 1,2,3,4.
Fig. 1 is by being surveyed SeO in XRF data in the embodiment of the present invention 1,2,3,4 2mass percentage change curve.
Fig. 2 is by being surveyed SO in XRF data in the embodiment of the present invention 1,2,3,4 3mass percentage change curve.
Fig. 3 is by being surveyed CdO mass percentage change curve in XRF data in the embodiment of the present invention 1,2,3,4.
Fig. 4 is the apparent figure of the embodiment of the present invention 1,2,3,4 (from left to right) coloured glass sample.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but be not limited to described content below.
Embodiment 1:
In borosilicate glass, a method of fixation of Cd S and Se, comprises the steps:
1) borosilicate matrix frit is prepared:
1. by B 2o 3, SiO 2, Al 2o 3, Zn (namely mixing a small amount of zinc powder), Na 3alF 6, CaO and R 2o (is: Li 2o, Na 2o and K 2o) as raw material, wherein B 2o 3by H 3bO 3introduce, CaO is by CaCO 3introduce, Na 2o is by Na 2cO 3introduce, K 2o is by K 2cO 3introduce, Li 2o is by Li 2cO 3introduce,
Component and the mass percent of borosilicate matrix frit are: SiO 2: 60%, Na 2o:9%, K 2o:13%, Li 2o:3%, B 2o 3: 4%, Al 2o 3: 3.5%, Na 3alF 6: 2.5%, CaO:3%, Zn:2%.
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3(i.e. Na 2cO 3and K 2cO 3), CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit;
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO; The add-on of the add-on of CdS to be the add-on of 1.5%, Se of borosilicate matrix frit quality be 0.5%, ZnO of borosilicate matrix frit quality is 8% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 2 hours 350 DEG C of insulations, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, pour crucible into after mixing, at 700 DEG C, crucible is put into kiln, be warmed up to 1250 DEG C of insulations discharging in 2 hours, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 450 DEG C of annealing 1 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
Embodiment 1 gained glass is carried out XRF test, and result is as shown in table 1, and wherein Cd, S, Se element all occupies certain amount, as SeO 2: 0.20% (wt%), SO 3: 0.22% (wt%), CdO:0.90% (wt%), because raw material contains trace impurity, so also containing the element such as micro Fe, P, Ba in glass.
From data in table 1, the content of Se element increases along with blowing temperature and increases, and S and Cd element variation rule is not clearly, form glass colour and show selenium ruby look, namely obtain selenium ruby glass, as shown in Figure 4.
From the color of Fig. 4 glass, high temperature blowing secures CdS and Se effectively, inhibits their volatilization, makes CdS be easy to form ultramicro-crystal.And as can be seen from the color of glass, in glass, having formed a certain amount of CdSe ultramicro-crystal, yes first defines a certain amount of CdS ultramicro-crystal, Se subsequently for that 2-enter in CdS lattice, progressively replace S 2-, along with CdSe/CdS ratio constantly increases, the redness presented is also more and more darker, so high temperature blowing is conducive to fixation of Cd S and Se, forms the mixed crystal of CdS and CdSe, thus can realize the target of Quantum Dot Glass and devitrified glass Color tunable.
Fig. 1, Fig. 2, Fig. 3 are SeO in the XRF test result of the embodiment of the present invention 1,2,3,4 2, SO 3, CdO data mass percentage change curve.
Embodiment 2:
In borosilicate glass, a method of fixation of Cd S and Se, comprises the steps:
1) borosilicate matrix frit is prepared:
1. by B 2o 3, SiO 2, Al 2o 3, Zn (namely mixing a small amount of zinc powder), Na 3alF 6, CaO and R 2o (Li 2o, Na 2o and K 2o) as raw material, wherein B 2o 3by H 3bO 3introduce, Na 2o is by Na 2cO 3introduce, K 2o is by K 2cO 3introduce, CaO is by CaCO 3introduce, Li 2o is by Li 2cO 3introduce,
Component and the mass percent of borosilicate matrix frit are: SiO 2: 60%, Na 2o:9%, K 2o:13%, Li 2o:3%, B 2o 3: 4%, Al 2o 3: 3.5%, Na 3alF 6: 2.5%, CaO:3%, Zn:2%.
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3, CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit;
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO, the add-on of CdS is 1.5% of borosilicate matrix frit quality, the add-on of Se is the add-on of 0.5%, ZnO of borosilicate matrix frit quality is 8% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 2 hours 350 DEG C of insulations, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, pour crucible into after mixing, at 800 DEG C, crucible is put into kiln, be warmed up to 1250 DEG C of insulations discharging in 2 hours, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 450 DEG C of annealing 1 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
Embodiment 2 gained glass is carried out XRF test, and result is as shown in table 1, and wherein Cd, S, Se element all occupies certain amount, as SeO 2: 0.25% (wt%), SO 3: 0.20% (wt%), CdO:1.03% (wt%), because raw material contains trace impurity, so also containing the element such as micro Fe, P, Ba in glass.
From data in table 1, the content of Se element increases along with blowing temperature and increases, and S and Cd element variation rule is not clearly, form glass colour and show selenium ruby look, namely obtain selenium ruby glass, as shown in Figure 4.
From the color of Fig. 4 glass, high temperature blowing secures CdS and Se effectively, inhibits their volatilization, makes CdS be easy to form ultramicro-crystal.And as can be seen from the color of glass, in glass, having formed a certain amount of CdSe ultramicro-crystal, yes first defines a certain amount of CdS ultramicro-crystal, Se subsequently for that 2-enter in CdS lattice, progressively replace S 2-, along with CdSe/CdS ratio constantly increases, the redness presented is also more and more darker, so high temperature blowing is conducive to fixation of Cd S and Se, forms the mixed crystal of CdS and CdSe, thus can realize the target of Quantum Dot Glass and devitrified glass Color tunable.
Fig. 1, Fig. 2, Fig. 3 are SeO in the XRF test result of the embodiment of the present invention 1,2,3,4 2, SO 3, CdO data mass percentage change curve.
Embodiment 3:
In borosilicate glass, a method of fixation of Cd S and Se, comprises the steps:
1) borosilicate matrix frit is prepared:
1. by B 2o 3, SiO 2, Al 2o 3, Zn (namely mixing a small amount of zinc powder), Na 3alF 6, CaO and R 2o (is: Li 2o, Na 2o and K 2o) as raw material, wherein B 2o 3by H 3bO 3introduce, CaO is by CaCO 3introduce, Na 2o is by Na 2cO 3introduce, K 2o is by K 2cO 3introduce, Li 2o is by Li 2cO 3introduce,
Component and the mass percent of borosilicate matrix frit are: SiO 2: 60%, Na 2o:9%, K 2o:13%, Li 2o:3%, B 2o 3: 4%, Al 2o 3: 3.5%, Na 3alF 6: 2.5%, CaO:3%, Zn:2%.
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3(i.e. Na 2cO 3and K 2cO 3), CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit;
The step 1. middle H of described preparation borosilicate matrix frit 3bO 3introduction volume should consider the volatile quantity of its 10% (quality);
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO, the add-on of CdS is 1.5% of borosilicate matrix frit quality, the add-on of Se is the add-on of 0.5%, ZnO of borosilicate matrix frit quality is 8% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 2 hours 350 DEG C of insulations, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, pour crucible into after mixing, at 900 DEG C, crucible is put into kiln, be warmed up to 1250 DEG C of insulations discharging in 2 hours, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 450 DEG C of annealing 1 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
Embodiment 3 gained glass is carried out XRF test, and result is as shown in table 1, and wherein Cd, S, Se element all occupies certain amount, as SeO 2: 0.30% (wt%), SO 3: 0.22% (wt%), CdO:0.90% (wt%), because raw material contains trace impurity, so also containing the element such as micro Fe, P, Ba in glass.
From data in table 1, the content of Se element increases along with blowing temperature and increases, and S and Cd element variation rule is not clearly, form glass colour and show selenium ruby look, namely obtain selenium ruby glass, as shown in Figure 4.
From the color of Fig. 4 glass, high temperature blowing secures CdS and Se effectively, inhibits their volatilization, makes CdS be easy to form ultramicro-crystal.And as can be seen from the color of glass, in glass, having formed a certain amount of CdSe ultramicro-crystal, yes first defines a certain amount of CdS ultramicro-crystal, Se subsequently for that 2-enter in CdS lattice, progressively replace S 2-, along with CdSe/CdS ratio constantly increases, the redness presented is also more and more darker, so high temperature blowing is conducive to fixation of Cd S and Se, forms the mixed crystal of CdS and CdSe, thus can realize the target of Quantum Dot Glass and devitrified glass Color tunable.
Fig. 1, Fig. 2, Fig. 3 are SeO in the XRF test result of the embodiment of the present invention 1,2,3,4 2, SO 3, CdO data mass percentage change curve.
Embodiment 4:
In borosilicate glass, a method of fixation of Cd S and Se, comprises the steps:
1) borosilicate matrix frit is prepared:
1. by B 2o 3, SiO 2, Al 2o 3, Zn (namely mixing a small amount of zinc powder), Na 3alF 6, CaO and R 2o (Li 2o, Na 2o and K 2o) as raw material, wherein B 2o 3by H 3bO 3introduce, Na 2o is by Na 2cO 3introduce, K 2o is by K 2cO 3introduce, CaO is by CaCO 3introduce, Li 2o is by Li 2cO 3introduce,
Component and the mass percent of borosilicate matrix frit are: SiO 2: 60%, Na 2o:9%, K 2o:13%, Li 2o:3%, B 2o 3: 4%, Al 2o 3: 3.5%, Na 3alF 6: 2.5%, CaO:3%, Zn:2%.
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3, CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit;
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO, the add-on of CdS is 1.5% of borosilicate matrix frit quality, the add-on of Se is the add-on of 0.5%, ZnO of borosilicate matrix frit quality is 8% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 2 hours 350 DEG C of insulations, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, pour crucible into after mixing, at 1000 DEG C, crucible is put into kiln, be warmed up to 1250 DEG C of insulations discharging in 2 hours, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 450 DEG C of annealing 1 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
Embodiment 4 gained glass is carried out XRF test, and result is as shown in table 1, and wherein Cd, S, Se element all occupies certain amount, as SeO 2: 0.30% (wt%), SO 3: 0.25% (wt%), CdO:0.87% (wt%), because raw material contains trace impurity, so also containing the element such as micro Fe, P, Ba in glass.
From data in table 1, the content of Se element increases along with blowing temperature and increases, and S and Cd element variation rule is not clearly, form glass colour and show selenium ruby look, namely obtain selenium ruby glass, as shown in Figure 4.
From the color of Fig. 4 glass, high temperature blowing secures CdS and Se effectively, inhibits their volatilization, makes CdS be easy to form ultramicro-crystal.And as can be seen from the color of glass, in glass, having formed a certain amount of CdSe ultramicro-crystal, yes first defines a certain amount of CdS ultramicro-crystal, Se subsequently for that 2-enter in CdS lattice, progressively replace S 2-, along with CdSe/CdS ratio constantly increases, the redness presented is also more and more darker, so high temperature blowing is conducive to fixation of Cd S and Se, forms the mixed crystal of CdS and CdSe, thus can realize the target of Quantum Dot Glass and devitrified glass Color tunable.
Fig. 1, Fig. 2, Fig. 3 are SeO in the XRF test result of the embodiment of the present invention 1,2,3,4 2, SO 3, CdO data mass percentage change curve.Can find out, blowing temperature is very large on the impact of fixation of Cd S and Se.Generally speaking, blowing temperature is higher, and glass colour is darker, and the content of Se element constantly increases.For fixation of Cd S and Se, the most difficult fixing be Se, because Se will volatilize at about 600 DEG C, so blowing is conducive to fixation of Cd S and Se under high temperature, but blowing temperature can not be too high, if directly arrive glass melting temperature 1250 DEG C to start blowing, frit is difficult to reaction thoroughly, so for native system glass, 900 DEG C or 1000 DEG C of blowings are reasonable blowing temperature.
Embodiment 5:
In borosilicate glass, a method of fixation of Cd S and Se, comprises the steps:
1) borosilicate matrix frit is prepared:
1. by B 2o 3, SiO 2, Al 2o 3, Zn (namely mixing a small amount of zinc powder), Na 3alF 6, CaO and R 2o as raw material, wherein B 2o 3by H 3bO 3introduce, R 2o (refers to Li 2o) by Li 2cO 3introduce, CaO is by CaCO 3introduce,
Component and the mass percent of borosilicate matrix frit are: SiO 2: 70%, R 2o:20%, B 2o 3: 3%, Al 2o 3: 4.5%, Na 3alF 6: 1%, CaO:1%, Zn:0.5%, described R 2o refers to Li 2o;
The step 1. middle H of described preparation borosilicate matrix frit 3bO 3introduction volume should consider its (H 3bO 3) volatile quantity of 10% (quality).
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3, CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit.
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO, the add-on of CdS is 2% of borosilicate matrix frit quality, the add-on of Se is the add-on of 0.7%, ZnO of borosilicate matrix frit quality is 15% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 0.5 hour 300 DEG C of insulations, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, crucible is poured into after mixing, at 700 DEG C, crucible is put into kiln, be warmed up to 1200 DEG C of insulations discharging in 0.5 hour, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 400 DEG C of annealing 0.5 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
The present embodiment at utmost optimizes fixation of Cd S and Se, can obtain the cadmium sulphoselenide glass of colour stable.
Embodiment 6:
In borosilicate glass, a method of fixation of Cd S and Se, comprises the steps:
1) borosilicate matrix frit is prepared:
1. by B 2o 3, SiO 2, Al 2o 3, Zn (namely mixing a small amount of zinc powder), Na 3alF 6, CaO and R 2o as raw material, wherein B 2o 3by H 3bO 3introduce, R 2o is by Na 2cO 3introduce, CaO is by CaCO 3introduce.
Component and the mass percent of borosilicate matrix frit are: SiO 2: 70%, R 2o:25%, B 2o 3: 2%, Al 2o 3: 0.5%, Na 3alF 6: 0.5%, CaO:0.5%, Zn:1.5%, described R 2o refers to Na 2o.
The step 1. middle H of described preparation borosilicate matrix frit 3bO 3introduction volume should consider the volatile quantity of its 10% (quality).
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3, CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit.
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO, the add-on of CdS is 2% of borosilicate matrix frit quality, the add-on of Se is the add-on of 0.7%, ZnO of borosilicate matrix frit quality is 15% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 2 hours 400 DEG C of insulations, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, pour crucible into after mixing, at 1000 DEG C, crucible is put into kiln, be warmed up to 1350 DEG C of insulations discharging in 2 hours, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 500 DEG C of annealing 1.5 hours, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
The present embodiment at utmost optimizes fixation of Cd S and Se, can obtain the cadmium sulphoselenide glass of colour stable.
Embodiment 7:
In borosilicate glass, a method of fixation of Cd S and Se, comprises the steps:
1) borosilicate matrix frit is prepared:
1. by B 2o 3, SiO 2, Al 2o 3, Zn (namely mixing a small amount of zinc powder), Na 3alF 6, CaO and R 2o as raw material, wherein B 2o 3by H 3bO 3introduce, R 2o is by K 2cO 3introduce, CaO is by CaCO 3introduce.
Component and the mass percent of borosilicate matrix frit are: SiO 2: 55%, R 2o:25%, B 2o 3: 3.5%, Al 2o 3: 5%, Na 3alF 6: 5%, CaO:3.5%, Zn:3%, described R 2o refers to K 2o.
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3, CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit.
The step 1. middle H of described preparation borosilicate matrix frit 3bO 3introduction volume should consider the volatile quantity of its 10% (quality).
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO, the add-on of CdS is 1% of borosilicate matrix frit quality, the add-on of Se is the add-on of 0.2%, ZnO of borosilicate matrix frit quality is 5% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 0.5 hour 300 DEG C of insulations, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, crucible is poured into after mixing, at 700 DEG C, crucible is put into kiln, be warmed up to 1200 DEG C of insulations discharging in 0.5 hour, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 400 DEG C of annealing 0.5 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
The present embodiment at utmost optimizes fixation of Cd S and Se, can obtain the cadmium sulphoselenide glass of colour stable.
Table 1
Each raw material cited by the present invention and the bound value of each raw material, and the bound value of each processing parameter, can realize the present invention, not enumerate embodiment at this.

Claims (3)

1. a method of fixation of Cd S and Se in borosilicate glass, is characterized in that comprising the steps:
1) borosilicate matrix frit is prepared;
2) cadmium sulfoselenide pre-treatment:
1. the component of cadmium sulfoselenide pre-treatment material comprises CdS, Se and ZnO, the add-on of CdS is the 1-2% of borosilicate matrix frit quality, the add-on of Se is the 0.2-0.7% of borosilicate matrix frit quality, and the add-on of ZnO is the 5-15% of borosilicate matrix frit quality;
2. CdS, Se and ZnO raw material taken fully is ground in ceramic mortar, mix rear mistake 60 mesh sieve, pour crucible into, take out after 0.5-2 hour 300-400 DEG C of insulation, obtain CdS, Se and ZnO compound;
3) cadmium sulfoselenide coloured glass is prepared:
1. borosilicate matrix frit and good CdS, Se and ZnO compound of pre-treatment are all poured in ceramic mortar and fully grind, crucible is poured into after mixing, at 700-1000 DEG C, crucible is put into kiln, be warmed up to 1200 DEG C-1350 DEG C insulations discharging in 0.5-2 hour, obtained glass metal;
2. glass metal is poured in heat-resisting die shaping, and to send in retort furnace in 400-500 DEG C of annealing 0.5-1.5 hour, cool to room temperature with the furnace, obtain block cadmium sulfoselenide coloured glass.
2. the method for a kind of fixation of Cd S and Se in borosilicate glass according to claim 1, is characterized in that, described step 1) prepares borosilicate matrix frit and is:
1. by B 2o 3, SiO 2, Al 2o 3, Na 3alF 6, CaO and R 2o, as raw material, mixes zinc powder, wherein B 2o 3by H 3bO 3introduce, R 2o is by R 2cO 3introduce, CaO is by CaCO 3introduce,
Component and the mass percent of borosilicate matrix frit are: SiO 2: 55-70%, R 2o:15-25%, B 2o 3: 2%-7%, Al 2o 3: 0.5-5%, Na 3alF 6: 0.5-5%, CaO:0.5-5%, Zn:0.5-3%, described R 2o refers to Li 2o, Na 2o, K 2a kind of or several mixing by any proportioning arbitrarily during O is any;
2. the H will taken 3bO 3, SiO 2, Al 2o 3, Na 3alF 6, R 2cO 3, CaCO 3raw material fully grinds in ceramic mortar, mixes, and then crosses 60 mesh sieves, obtains borosilicate matrix frit.
3. the method for a kind of fixation of Cd S and Se in borosilicate glass according to claim 2, is characterized in that, the step 1. middle H of described preparation borosilicate matrix frit 3bO 3introduction volume should consider its 10%(quality) volatile quantity.
CN201510089568.XA 2015-02-27 2015-02-27 Method for fixing CdS and Se in borosilicate glass Pending CN104692658A (en)

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CN106865980A (en) * 2017-03-08 2017-06-20 武汉理工大学 A kind of praseodymium doped CdS quantum dot glass and preparation method thereof
CN106946456A (en) * 2017-04-28 2017-07-14 武汉理工大学 A kind of CdS quantum dot doped-glass and preparation method thereof
CN107445481A (en) * 2017-09-08 2017-12-08 蚌埠玻璃工业设计研究院 A kind of anti-blue light high transmission glass and preparation method thereof
CN109180011A (en) * 2018-08-09 2019-01-11 蚌埠淮畔精密机械有限公司 A kind of PbTe/CdTe double quantum point is co-doped with borosilicate glass and its preparation process
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106865980A (en) * 2017-03-08 2017-06-20 武汉理工大学 A kind of praseodymium doped CdS quantum dot glass and preparation method thereof
CN106946456A (en) * 2017-04-28 2017-07-14 武汉理工大学 A kind of CdS quantum dot doped-glass and preparation method thereof
CN107445481A (en) * 2017-09-08 2017-12-08 蚌埠玻璃工业设计研究院 A kind of anti-blue light high transmission glass and preparation method thereof
CN109180011A (en) * 2018-08-09 2019-01-11 蚌埠淮畔精密机械有限公司 A kind of PbTe/CdTe double quantum point is co-doped with borosilicate glass and its preparation process
CN109180011B (en) * 2018-08-09 2020-06-02 苏州融睿电子科技有限公司 PbTe/CdTe double quantum dot co-doped borosilicate glass and preparation process thereof
CN112028477A (en) * 2020-09-04 2020-12-04 彩虹集团（邵阳）特种玻璃有限公司 Quantum dot luminescent glass and preparation method and application thereof

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