CN102730967B - Preparation method for sensitization-enhanced green light-emitting high-silica glass - Google Patents
Preparation method for sensitization-enhanced green light-emitting high-silica glass Download PDFInfo
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- CN102730967B CN102730967B CN201210219728.4A CN201210219728A CN102730967B CN 102730967 B CN102730967 B CN 102730967B CN 201210219728 A CN201210219728 A CN 201210219728A CN 102730967 B CN102730967 B CN 102730967B
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Abstract
A kind of preparation method of sensitization enhancing green light vagcor, borosilicate glass is melted first, controls heat treatment condition, limits split-phase degree, the cellular glass of nubbin Na+ ion is obtained after acidleach; Cellular glass is impregnated in again in the solution of the ion containing Tb and Eu and impregnates doping. It is subsequently placed in high temperature sintering under reducing atmosphere. Obtain fine and close sensitization enhancing green light vagcor. The present invention is realized due to the presence of Na+ in glass structure
Interionic energy transfer, and the excitation band of Tb3+ ion is moved near 320nm near original 245nm, the excitation bandwidth of Tb3+ ion is not only effectively increased, while also substantially increasing luminous intensity. It is expected to be applied to the every field such as scientific research, national defence, medical treatment with laser material as novel shining.
Description
Technical field
The present invention relates to green light vagcor, particularly a kind of sensitization strengthens the preparation method of green light vagcor.
Background technology
The hertzian wave of each wave band has different transport propertys in different media.Be similar to the optical transmission window existing in atmosphere, seawater is much smaller to its all band to the attenuation ratio of the blue green light in 450～550nm wave band.Therefore the blue-green Laser in this wave band, can be used for the New Equipments such as Underwater Target Detection, control, communication, has important meaning in scientific research and national defence field, and Ye Shige big country makes great efforts the problem of development.
Meanwhile, at the absorption peak wavelength of the biological tissues such as erythrocyte medically, near 542nm, more ripe commercial 532nm laser apparatus is not in this optimum position at present yet.Developing the laser apparatus that wavelength mates more, can greatly improve the detection sensitivity of corresponding medical facilities and the validity for the treatment of, is also therefore very significant.
Silicate glass, after anneal under certain temperature, can be point phase system that comprises boron-rich phase and Si-rich phase by homogeneous system transition.Between two-phase, be uniformly dispersed.By the acidleach under certain temperature and pressure, water logging processing, can, by boron-rich phase stripping, produce the high silica system with even vesicular structure, be called as high silica porous glass.Have this sintered glass in the solution that contains Tb ion, to flood doping, then in reducing atmosphere high temperature sintering, making in the Tb of other different valence state ion conversion is Tb
2+ion, can send strong green glow.This vagcor contains more than 94% silicon-dioxide, and composition approaches silica glass, has good chemistry, machinery and thermostability, especially has that especially resistance to sudden heating is strong, is suitable as laser glass.But the problem one existing is that luminous intensity is still not high enough; The 2nd, its maximum excitation wavelength is about 245nm, and the ultraviolet ray of this wavelength has obvious harm to human body, and alternative light source is also less and be difficult in actual applications integrated.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, the preparation method who provides a kind of sensitization to strengthen green light vagcor, to improve glass greening light intensity.
technical solution of the present invention is as follows:
1, sensitization strengthens a preparation method for green light vagcor, it is characterized in that the method comprises the following steps:
(1) preparation mixing raw material;
The composition of mixing raw material comprises the SiO of analytically pure 52～64mol%
2, the Na of 5～11 mol%
2cO
3, the H of 26～40 mol %
3bO
3, the Al (OH) of 0～3 mol %
3;
(2) proportioning raw materials of selected glass by proportioning raw materials weighing, put into platinum or corundum crucible after will raw material mixing, and the High Temperature Furnaces Heating Apparatus that is placed in 1400～1500 DEG C is founded 30～60min, then at the iron plate top casting cooling forming of 100～400 DEG C;
(3) described borosilicate glass is placed in to thermal treatment at 560～630 DEG C of temperature and within 10～40 hours, carries out phase-splitting;
(4) by the borosilicate glass after phase-splitting repeatedly acidleach make sintered glass:
Be mixed with H with hydrochloric acid or nitric acid and water
+concentration is the acid solution of 0.03～1mol/L, the borosilicate glass of getting after described acid solution and phase-splitting in the ratio of 10～50ml acid solution/gram glass is placed in autoclave jointly, be placed in 90～100 DEG C of baking ovens at temperature 12～48 hours, take out also and still change according to the above ratio fresh acid solution after naturally cooling, repeat 1～3 time; Then clean with distilled water, dry;
(5) above-mentioned sintered glass be impregnated in the mixing solutions containing Tb ion 0.01～0.60mol/L and Eu ion 0.01～0.30mol/L and soaks:
The raw material of preparing mixing solutions comprises at least one in the oxide compound of Tb and Eu, muriate, nitrate, vitriol; Solvent is the one in water, salpeter solution, hydrochloric acid soln;
Soak 10min and can make sintered glass reach absorption state of saturation, longer soak time does not affect product performance;
(6) sintered glass having flooded is put into the corundum crucible that is paved with graphite and gac, or passing into H
2atmosphere in, be progressively warming up to 1100～1200 DEG C with the temperature rise rates of 30～500 DEG C/h, sintering 1～5 hour; Then naturally cooling.
Technique effect of the present invention:
1, through a large amount of experiments, we find remaining a small amount of Na that has
+the purer sintered glass of high silica porous glass of ion more contributes to
interionic energy shifts.
2, under normal circumstances due to dissolubility difference, the Na in pristine glass
+plasma is distributed in a large number boron-rich phase and together runs off in acidleach process thereupon, is not substantially present in the high silica structure of Si-rich phase and formation thereof.So the present invention is by controlling component and the heat treated condition of pristine glass, to limit the degree of phase-splitting.After acidleach, form like this and in sintered glass, also still remain a small amount of Na
+ion.Contain Na at this simultaneously
+in the dipping solution of sintered glass, add Tb and Eu ion simultaneously.The Eu ion of different valence state changes Eu in reducing atmosphere
2+.Now due to Na
+the existence of ion, the electric dipole-dipole interaction between active ion is increased greatly, makes thus rare earth ion increased activity, is especially embodied in Eu
2+and Tb
3+between energy exchange obviously improve.Now Eu
2+can be used as sensitizing agent, by Tb
3+the excitation band of ion migrates near the 320nm of near ultraviolet region, strengthens luminescent properties simultaneously.Due to the Na relating in the method
+the microstructure of sintered glass is participated in and changed to ion directly, and the Na being doped into by dipping in traditional sintered glass
+just exist with the form of surface adsorption, thereby the latter is difficult to observe similar promotion sensitization phenomenon.
As seen from Figure 1, Tb
3+the emission peak wavelength of institute's green light, in 545nm left and right, approaches the absorption peak wavelength of biological tissue very much; Singly mix Tb
3+the green light vagcor of sensitization (Fig. 1 line B) luminous intensity under 320nm excites is not far smaller than 245nm and excites (Fig. 1 line A); Through Eu
2+green light vagcor after sensitization has than the former under 245nm excites (Fig. 1 line A) stronger luminous exciting of the near-ultraviolet light of 320nm under (Fig. 1 line C).Fig. 2 shows, Eu
2+after sensitization, (Fig. 2 line B) maximum excitation wavelength is by 245nm(Fig. 2 line A of sensitization sample not) transfer to 320nm place.This exciting light is safer to human body, and along with the maturation of LED technology, respective sources is also more various and easy-to-use.And in vagcor matrix, Eu
2+ion is also than common sensitization Tb
3+the Ce adopting
3+ion (as " a kind of preparation method of green luminous glass of doping with rare-earth ions " (Zhou Mingjie etc., disclosure of the invention number: 101898873A)) has the better characteristics of luminescence, is more conducive to strengthen the luminous intensity of product.Therefore the present invention is expected to the laserable material as Novel green laser, is applied to the every field such as scientific research, national defence, medical treatment.
Brief description of the drawings
Fig. 1 mixes 0.15mol/L Tb with the porous borosilicate glass list that similarly to Example 1 prepared by technique
3+the green light vagcor of not sensitization at 245nm(line A), 320nm(line B) and embodiment 1 prepared through Eu
2+green light vagcor after sensitization is at 320nm(line C) emission spectrum under exciting.
Fig. 2 mixes 0.15mol/L Tb with the porous borosilicate glass list that similarly to Example 1 prepared by technique
3+the green light vagcor (line A) of not sensitization and embodiment 1 prepared through Eu
2+green light vagcor (line B) after sensitization is in the excitation spectrum at monitoring 545nm place.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but should not limit the scope of the invention with this.
embodiment 1
Get analytically pure chemical reagent, according to SiO
263.72mol%, Na
2cO
39.80 mol%, H
3bO
3the proportioning preparation mixing raw material of 26.48 mol %.After mixed grinding is even, put into platinum crucible, after the high-temperature fusion 40min of 1450 DEG C, cooling forming on the iron plate of 400 DEG C, is prepared into borosilicate glass.
This borosilicate glass is put into High Temperature Furnaces Heating Apparatus after 590 DEG C of thermal treatments in 20 hours, be cut into the sheet glass of 5mm × 5mm × 1mm.Glass is put into the autoclave of sealing, be placed in and at 98 DEG C of temperature, carry out three each acid treatment of 24 hours; Wherein for the first time with the ratio of 50ml acid solution/gram glass immerse the salpeter solution of 1mol/L, for the second time with the ratio of 10ml acid solution/gram glass immerse the salpeter solution of 1mol/L, the ratio of 10ml acid solution/gram glass immerses the salpeter solution of 0.3mol/L for the third time.Then this glass is taken out from autoclave, use distilled water wash clean, dry, just can obtain high silica porous glass.
Use Tb
4o
7and Eu
2o
3with the mixing solutions of salpeter solution preparation containing 0.15mol/L Tb ion and 0.01mol/L Eu ion.Aforementioned high silica porous glass is placed in to this mixing solutions and soaks after 1 hour and take out, put into the corundum crucible that is paved with graphite and gac, seal, be placed in High Temperature Furnaces Heating Apparatus.Heating schedule is: room temperature is raised to 100 through 180min
oc, then be raised to 300 through 60min
oc, then be raised to 800 through 60min
oc, then be raised to 1100 through 60min
oc, insulation 60min, then naturally cooling.Can make the green light vagcor that sensitization strengthens.
Embodiment 1 glass is carried out to spectrum test, and result enters shown in Fig. 1 Fig. 2, and Fig. 1 mixes 0.15mol/L Tb with the porous borosilicate glass list that similarly to Example 1 prepared by technique
3+not sensitization green light vagcor 245nm, 320nm and embodiment 1 prepared through Eu
2+the emission spectrum contrast of green light vagcor after sensitization under 320nm excites.
Fig. 2 mixes 0.15mol/L Tb with the porous borosilicate glass list that similarly to Example 1 prepared by technique
3+the green light vagcor of not sensitization and embodiment 1 prepared through Eu
2+green light vagcor after sensitization is in the excitation spectrum contrast at monitoring 545nm place.
Embodiment 2,
Get analytically pure chemical reagent, according to SiO
252.07mol%, Na
2cO
35.82 mol%, H
3bO
339.17 mol %, Al (OH)
3the proportioning preparation mixing raw material of 2.94mol%.Mixed grinding is put into corundum crucible after evenly, after the high-temperature fusion 60min of 1400 DEG C on the iron plate of 300 DEG C cooling forming, be prepared into borosilicate glass.
This borosilicate glass is put into High Temperature Furnaces Heating Apparatus after 560 DEG C of thermal treatments in 40 hours, be cut into the sheet glass of 5mm × 5mm × 1mm.Glass is put into the autoclave of sealing, be placed in and at 90 DEG C of temperature, carry out three each acid treatment of 12 hours; Wherein immerse the hydrochloric acid soln of 1mol/L, the hydrochloric acid soln of second to three immersion of the ratio with 10ml acid solution/gram glass 1mol/L with the ratio of 50ml acid solution/gram glass for the first time.Then this glass is taken out from autoclave, use distilled water wash clean, dry, just can obtain high silica porous glass.
Use Tb
2cl
7and Eu
2(SO
4)
3with the mixing solutions of water preparation containing 0.60mol/L Tb ion and 0.30mol/L Eu ion.Aforementioned high silica porous glass is placed in after this mixing solutions soaks 10min and is taken out, be placed in and pass into H
2high Temperature Furnaces Heating Apparatus in.Heating schedule is: room temperature is raised to 300 through 180min
oc, then be raised to 800 through 180min
oc, then be raised to 1150 through 240min
oc, insulation 120min, then naturally cooling.Can make the green light vagcor that sensitization strengthens.
Embodiment 3,
Get analytically pure chemical reagent, according to SiO
262.81mol%, Na
2cO
310.15 mol%, H
3bO
3the proportioning preparation mixing raw material of 27.04 mol %.Mixed grinding is put into corundum crucible after evenly, after the high-temperature fusion 30min of 1500 DEG C on the iron plate of 200 DEG C cooling forming, be prepared into borosilicate glass.
This borosilicate glass is put into High Temperature Furnaces Heating Apparatus after 630 DEG C of thermal treatments in 10 hours, be cut into the sheet glass of 5mm × 5mm × 1mm.Glass is put into the autoclave of sealing, with the ratio of 50ml acid solution/gram glass immerse 1mol/L salpeter solution, be placed in the acid treatment of carrying out at 100 DEG C of temperature one time 48 hours.Then this glass is taken out from autoclave, use distilled water wash clean, dry, just can obtain sintered glass.
Use Tb
4o
7and Eu (NO
3)
3with the mixing solutions of salpeter solution preparation containing 0.01mol/L Tb ion and 0.01mol/L Eu ion.Aforementioned high silica porous glass is placed in after this mixing solutions soaks 30min and is taken out, put into the corundum crucible that is paved with graphite and gac, seal.Heating schedule is: room temperature is raised to 300 through 180min
oc, then be raised to 800 through 120min
oc, then be raised to 1200 through 180min
oc, insulation 300min, then naturally cooling.Can make the green light vagcor that sensitization strengthens.
Embodiment 4,
Get analytically pure chemical reagent, according to SiO
263.72mol%, Na
2cO
39.80 mol%, H
3bO
3the proportioning preparation mixing raw material of 26.48 mol %.Mixed grinding is put into corundum crucible after evenly, after the high-temperature fusion 50min of 1430 DEG C on the iron plate of 100 DEG C cooling forming, be prepared into borosilicate glass.
This borosilicate glass is put into High Temperature Furnaces Heating Apparatus after 630 DEG C of thermal treatments in 20 hours, be cut into the sheet glass of 5mm × 5mm × 1mm.Glass is put into the autoclave of sealing, be placed in and at 95 DEG C of temperature, carry out three each acid treatment of 18 hours; Wherein for the first time with the ratio of 50ml acid solution/gram glass immerse the hydrochloric acid soln of 1mol/L, for the second time with the ratio of 30ml acid solution/gram glass immerse the hydrochloric acid soln of 0.7mol/L, the ratio of 10ml acid solution/gram glass immerses the hydrochloric acid soln of 0.3mol/L for the third time.Then this glass is taken out from autoclave, use distilled water wash clean, dry, just can obtain high silica porous glass.
Use Tb
2(NO
3)
7and Eu
2(SO
4)
3with the mixing solutions of salpeter solution preparation containing 0.09mol/L Tb ion and 0.03mol/L Eu ion.Aforementioned high silica porous glass is placed in after this mixing solutions soaks 20min and is taken out, put into the corundum crucible that is paved with graphite and gac, seal, be placed in High Temperature Furnaces Heating Apparatus.Heating schedule is: room temperature is raised to 100 through 180min
oc, then be raised to 300 through 60min
oc, then be raised to 800 through 60min
oc, then be raised to 1100 through 60min
oc, insulation 60min, then naturally cooling.Can make the green light vagcor that sensitization strengthens.
Embodiment 5,
Get analytically pure chemical reagent, according to SiO
252.07mol%, Na
2cO
35.82 mol%, H
3bO
339.17 mol %, Al (OH)
3the proportioning preparation mixing raw material of 2.94mol%.Mixed grinding is put into platinum crucible after evenly, after the high-temperature fusion 40min of 1480 DEG C on the iron plate of 400 DEG C cooling forming, be prepared into borosilicate glass.
This borosilicate glass is put into High Temperature Furnaces Heating Apparatus after 590 DEG C of thermal treatments in 30 hours, be cut into the sheet glass of 5mm × 5mm × 1mm.Glass is put into the autoclave of sealing, be placed in and at 92 DEG C of temperature, carry out three each acid treatment of 36 hours; Wherein immerse the hydrochloric acid soln of 1mol/L, the hydrochloric acid soln of second to three immersion of the ratio with 30ml acid solution/gram glass 0.5mol/L with the ratio of 50ml acid solution/gram glass for the first time.Then this glass is taken out from autoclave, use distilled water wash clean, dry, just can obtain high silica porous glass.
Use Tb
4(SO
4)
7and EuCl
3with the mixing solutions of hydrochloric acid soln preparation containing 0.45mol/L Tb ion and 0.15mol/L Eu ion.Aforementioned high silica porous glass is placed in after this mixing solutions soaks 10min and is taken out, be placed in and pass into H
2high Temperature Furnaces Heating Apparatus in.Heating schedule is: room temperature is raised to 300 through 180min
oc, then be raised to 800 through 180min
oc, then be raised to 1150 through 240min
oc, insulation 120min, then naturally cooling.Can make the green light vagcor that sensitization strengthens.
Embodiment 6,
Get analytically pure chemical reagent, according to SiO
262.81mol%, Na
2cO
310.15 mol%, H
3bO
3the proportioning preparation mixing raw material of 27.04 mol %.Mixed grinding is put into platinum crucible after evenly, after the high-temperature fusion 30min of 1450 DEG C on the iron plate of 300 DEG C cooling forming, be prepared into borosilicate glass.
This borosilicate glass is put into High Temperature Furnaces Heating Apparatus after 570 DEG C of thermal treatments in 30 hours, be cut into the sheet glass of 5mm × 5mm × 1mm.Glass is put into the autoclave of sealing, be placed in and at 100 DEG C of temperature, carry out twice each acid treatment of 24 hours; Wherein immerse the salpeter solution of 1mol/L, immerse for the second time the salpeter solution of 1mol/L with the ratio of 20ml acid solution/gram glass with the ratio of 40ml acid solution/gram glass for the first time.Then this glass is taken out from autoclave, use distilled water wash clean, dry, just can obtain sintered glass.
Use Tb
2(NO
3)
7and Eu (NO
3)
3with the mixing solutions of water preparation containing 0.03mol/L Tb ion and 0.03mol/L Eu ion.Aforementioned high silica porous glass is placed in after this mixing solutions soaks 40min and is taken out, put into the corundum crucible that is paved with graphite and gac, seal.Heating schedule is: room temperature is raised to 300 through 180min
oc, then be raised to 800 through 120min
oc, then be raised to 1200 through 180min
oc, insulation 300min, then naturally cooling.Can make the green light vagcor that sensitization strengthens.
Claims (1)
1. sensitization strengthens a preparation method for green light vagcor, it is characterized in that the method comprises the following steps:
(1) preparation mixing raw material;
The composition of mixing raw material comprises the SiO of analytically pure 52～64mol%
2, the Na of 5～11mol%
2cO
3, the H of 26～40mol%
3bO
3, the Al (OH) of 0～3mol%
3;
(2) proportioning raw materials of selected glass is also by proportioning raw materials weighing, after being mixed, raw material puts into platinum or corundum crucible, the High Temperature Furnaces Heating Apparatus that is placed in 1400～1500 DEG C is founded 30～60min, then obtains borosilicate glass at the iron plate top casting cooling forming of 100～400 DEG C;
(3) described borosilicate glass is placed in to thermal treatment at 560～630 DEG C of temperature and within 10～40 hours, carries out phase-splitting;
(4) by the borosilicate glass after phase-splitting repeatedly acidleach make sintered glass:
Be mixed with H with hydrochloric acid or nitric acid and water
+concentration is the acid solution of 0.03～1mol/L, the borosilicate glass of getting after described acid solution and phase-splitting in the ratio of 10～50ml acid solution/gram glass is placed in autoclave jointly, be placed in 90～100 DEG C of baking ovens at temperature 12～48 hours, take out also and still change according to the above ratio fresh acid solution after naturally cooling, repeat 1～3 time; Then clean with distilled water, dry;
(5) above-mentioned sintered glass be impregnated in the mixing solutions containing Tb ion 0.01～0.60mol/L and Eu ion 0.01～0.30mol/L and soaks:
The raw material of preparing mixing solutions comprises at least one in the oxide compound of Tb and Eu, muriate, nitrate, vitriol; Solvent is water, salpeter solution or hydrochloric acid soln; Soak 10min and can make sintered glass reach absorption state of saturation, longer soak time does not affect product performance;
(6) sintered glass having flooded is put into the corundum crucible that is paved with graphite and gac, or passing into H
2atmosphere in, be warming up to 1100～1200 DEG C with the temperature rise rate of 30～500 DEG C/h, sintering 1～5 hour; Then naturally cooling.
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|---|---|---|---|
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| CN108467196B (en) * | 2018-03-27 | 2020-10-27 | 华南理工大学 | Red-green-blue light all-inorganic perovskite quantum dot and porous glass composite luminescent material and preparation method thereof |
| CN114249531B (en) * | 2021-12-17 | 2024-01-19 | 陕西华特新材料股份有限公司 | Preparation method of high silica glass melt capable of improving liquid level melting capacity |
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