CN102476918B - High-silica blue luminescent glass and preparation method thereof - Google Patents
High-silica blue luminescent glass and preparation method thereof Download PDFInfo
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- CN102476918B CN102476918B CN201010567158.9A CN201010567158A CN102476918B CN 102476918 B CN102476918 B CN 102476918B CN 201010567158 A CN201010567158 A CN 201010567158A CN 102476918 B CN102476918 B CN 102476918B
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Abstract
The invention belongs to the field of a luminescent material and discloses high-silica blue luminescent glass and a preparation method thereof. The high-silica blue luminescent glass comprises a high-silica nano micropore glass substrate and Re[1-x]TmxVO4 nano luminescent minicrystals which are uniformly distributed in the micropores of the high-silica nano micropore glass substrate, wherein Re is at least one of Y, La and Gd, and x ranges from 1*10<-4> to 0.05. According to the invention, the high-silica nano micropore glass is used as a luminescent ion substrate, and the Re[1-x]TmxVO4 nano luminescent minicrystals are distributed in the micropores of the luminescent ion substrate; and the high-silica nano micropore glass substrate has good ultraviolet light permeable property, which is extremely beneficial to absorption of luminescent particles on excitation wavelengths, thereby improving the luminescence efficiency.
Description
Technical field
The present invention relates to field of photovoltaic materials, relate in particular to a kind of high silica blue luminescent glass.The invention still further relates to the preparation method of high silica blue luminescent glass.
Background technology
Along with the continuous application of rare earth ion doped luminescent material in the fields such as illumination, demonstration, laser and light amplification and information, find that rare earth ion doped nano luminescent particle can produce more excellent luminescent properties in matrix material, but traditional solid-phase sintering method is difficult to prepare the incandescnet particle of nano-scale.Although some new preparation methods at present, such as hydrothermal synthesis method, sol-gel method etc. can obtain dispersed incandescnet particle preferably.But, along with the development of high-brightness light lighting equipment, high power laser light and technique of display, the requirement of the aspects such as chemical stability, physical strength, heat shock resistance, resistance to high-energy ion irradiation, exciting light transmitance and processability to luminescent material constantly improves.But traditional nano-phosphor and gelatinous material can not meet the requirement of above-mentioned performance gradually, cannot adapt to industrial production and life requirement.
Silica glass owing to thering is good chemical stability, thermal expansivity is little, heat shock resistance, low optical losses and high mechanical strength are suitable as the substrate material of rare earth luminous ion very much.But silica glass Rare Earth Ion doping content is not high, easy spontaneous cluster generation concentration quenching effect, is unfavorable for the miniaturization of device, greatly limits the application of silica glass.
Summary of the invention
In order to address the above problem, the invention provides a kind of high silica blue luminescent glass, include high silica nanometer micropore glass baseplate, and be evenly distributed in described high silica nanometer micropore glass baseplate in micropore, chemical general formula is Re
1-xtm
xvO
4nano luminescent crystallite; Wherein, Re is at least one being selected from Y (yttrium), La (lanthanum) or Gd (gadolinium), and the span of x is 1 × 10
-4～0.05.
Described high silica blue luminescent glass, wherein, high silica nanometer micropore glass baseplate comprises that weight percent component is: 94.0%～98.0% SiO
2, 1.0%～3.0% B
2o
3, 1.0%～3.0% Al
2o
3.
The present invention also provides the preparation method of above-mentioned high silica blue luminescent glass, and preparation flow is as follows:
According to chemical general formula Re
1-xtm
xvO
4in the stoichiometric ratio of each element, source compound, the source compound of Tm (thulium) and the source compound of V (vanadium) of Re are provided, then (in soaking solution, Tm ion volumetric molar concentration is 1 × 10 to be configured to soaking solution containing Re ion, Tm ion and V ion
-5～0.1mol/L, Re ion volumetric molar concentration is 0.1～2mol/L, V ion volumetric molar concentration is 0.1～2mol/L); Wherein, Re is at least one being selected from Y, La or Gd, and the span of x is 1 × 10
-4～0.05; The source compound of Re is at least one in nitrate, the muriate of Re or the vitriol of Re of Re; The source compound of Tm is at least one in nitrate, the muriate of Tm or the vitriol of Tm of Tm; The source compound of V is at least one in vanadylic sulfate or metavanadic acid ammonia;
High silica nanometer micropore glass baseplate is put into above-mentioned soaking solution and soak 10min～5h, preferably 30min～5h;
The high silica nanometer micropore glass baseplate soaking (its micro pore volume account for high silica nanometer micropore glass cumulative volume 25～40%) is put at 1000～1350 DEG C and carried out sintering processes 1～5h, cooling, make described high silica blue luminescent glass.
Compared with prior art, the present invention has the following advantages:
In vagcor of the present invention, be evenly distributed with Re
1-xtm
xvO
4luminescence nanocrystalline, has very high luminous efficiency.
Vagcor has the physical and chemical performance that is similar to silica glass, and its good chemical stability, little thermal expansivity, strong heat shock resistance, low optical losses and high mechanical strength are suitable as the substrate material of rare earth luminous ion very much.
The present invention selects high silica nanometer micropore glass as light emitting ionic substrate material, due to the special pore structure of high silica nanometer micropore glass, can make by micropore the nano luminescent crystallite of nano-scale, and nano luminescent crystallite can be disperseed well in the micropore of high silica nanometer micropore glass, the concentration quenching effect of having avoided cluster to cause.Because the volume of micropore accounts for 25～40% of high silica nanometer micropore glass cumulative volume, ensure like this can have in micropore the nano luminescent crystallite of sufficient amount, make glass of the present invention there is good luminescent properties.In addition, this high silica nanometer micropore glass matrix has good through performance to UV-light, is very beneficial for the absorption of incandescnet particle to excitation wavelength, thereby improves luminous efficiency.
High silica nanometer micropore glass is after sintering, and micropore shrinks nano luminescent crystallite is closed and forms closely knit devitrified glass, and the sealing of nano luminescent crystallite can keep the stability of product, and selects SiO in high silica nanometer micropore glass baseplate
2content be not less than 94%, its constituent class is similar to silica glass, has the excellent physical and the chemical property that are similar to silica glass, such as chemical stability is good, the high and low thermal expansivity of physical strength, heat shock resistance etc.These premium propertiess can be used in many special fields glass of the present invention, especially be applied in some severe environment, for example, illumination and demonstration under high temperature, high pressure, high vibration and wet environment, the solid-state laser field of superpower high repetition frequency, solar energy materials field of long-term outdoor work etc.
Brief description of the drawings
Fig. 1 is preparation technology's schema of the high silica blue luminescent glass of the present invention;
Figure 2 shows that the emmission spectrum of the prepared high silica blue luminescent glass of embodiment 2 under 310nm ultraviolet excitation; Its transmitting peak position is positioned at 476nm;
Figure 3 shows that the luminous excitation spectrum of high silica blue luminescent glass monitoring 476nm that embodiment 2 is prepared.
Embodiment
The invention provides a kind of high silica blue luminescent glass, include high silica nanometer micropore glass baseplate, and be evenly distributed on the Re in micropore in described high silica nanometer micropore glass baseplate
1-xtm
xvO
4nano luminescent crystallite, forms the closely knit vagcor of atresia that wraps up nano luminescent crystallite through sintered microporous contraction; Wherein, Re is at least one being selected from Y, La or Gd, and the span of x is 1 × 10
-4～0.05.
In high silica blue luminescent glass, high silica nanometer micropore glass baseplate by the component of following weight percent is mainly:
SiO
2 94.0％～98.0％
B
2O
3 1.0％～3.0％
Al
2O
3 1.0％～3.0％。
Manufacture the method for above-mentioned high silica blue luminescent glass, as shown in Figure 1, preparation flow is as follows:
Step S1, according to chemical general formula Re
1-xtm
xvO
4in the stoichiometric ratio of each element, source compound, the source compound of Tm and the source compound of V of Re are provided, be then configured to the soaking solution containing Re ion, Tm ion and V ion; Wherein, Re is at least one being selected from Y, La or Gd, and the span of x is 1 × 10
-4～0.05; Re exists with ionic state, and Tm exists with ionic state;
Step S2, to choose the high silica nanometer micropore glass with even UNICOM micropore be base material, puts it into and in soaking solution, soak 10min～5h, preferably 30min～5h;
Step S3, the high silica nanometer micropore glass after soaking is progressively warming up at 1000～1350 DEG C to sintering 1～5 hour, makes high silica blue luminescent glass.
In above-mentioned preparation method's step S1, the source compound of Re is its soluble salt, as in the vitriol of the muriate of the nitrate of Re, Re or Re at least one; The source compound of Tm is its soluble salt, as in the vitriol of the muriate of the nitrate of Tm, Tm or Tm at least one; The source compound of V is its soluble vanadium compound, as, vanadylic sulfate or metavanadic acid ammonia; In described soaking solution, Tm ion volumetric molar concentration is 1 × 10
-5～0.1mol/L, Re ion (comprises Y
3+, La
3+and Gd
3+total number of ions) volumetric molar concentration is 0.1～2mol/L, V ion volumetric molar concentration is 0.1～2mol/L.
In above-mentioned preparation method's step S3, described sintering processes also comprises: be first warmed up to 400 DEG C with the speed of 10 DEG C/min, then be warmed up to 900 DEG C with the speed of 15 DEG C/min, be warmed up to 1000～1350 DEG C afterwards with 5 DEG C/min speed.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
Take the six nitric hydrate yttrium (Y (NO of 0.099mol
3)
36H
2o), the vanadylic sulfate (VOSO of 0.1mol
4) and the six nitric hydrate thulium (Tm (NO of 0.001mol
3)
3) 6H
2o is dissolved in the distilled water of 100ml, is mixed with and contains 0.99mol/L Y
3+, 1mol/L vanadium ion and 0.01mol/L Tm
3+soaking solution.By high silica nanometer micropore glass (94.0%SiO
2, 3.0%B
2o
3, 3.0%Al
2o
3; And micro pore volume account for high silica nanometer micropore glass cumulative volume 25%) be dipped in soaking solution and take out after 10min, at room temperature dry in the air and insert in High Temperature Furnaces Heating Apparatus to surface drying, the temperature-rise period of High Temperature Furnaces Heating Apparatus is: be first raised to 400 DEG C with the speed of 10 DEG C/min, again with the speed to 900 DEG C of 15 DEG C/min, afterwards with 5 DEG C/min speed to 1300 DEG C, at 1300 DEG C, to the micropore glass heat preservation sintering 2h after soaking, glass cools to room temperature with the furnace and takes out.Through cutting and polishing, making containing chemical general formula is Y
0.99tm
0.01vO
4the high silica blue luminescent glass of nano luminescent crystallite.
Embodiment 2
Take the six nitric hydrate yttrium (Y (NO of 0.1mol
3)
36H
2o), take the gadolinium nitrate hexahydrate (Gd (NO of 0.09mol
3)
36H
2o), the vanadylic sulfate (VOSO of 0.2mol
4) and the six nitric hydrate thulium (Tm (NO of 0.01mol
3)
3) 6H
2o is dissolved in the distilled water of 100ml, is mixed with and contains 1mol/L Y
3+, 0.9mol/L Gd
3+, 2mol/L vanadium ion and 0.1mol/L Tm
3+soaking solution.By high silica nanometer micropore glass (96.0%SiO
2, 3.0%B
2o
3, 1.0%Al
2o
3; And micro pore volume account for high silica nanometer micropore glass cumulative volume 30%) be dipped in soaking solution and take out after 4h, at room temperature dry in the air and insert in High Temperature Furnaces Heating Apparatus to surface drying, the temperature-rise period of High Temperature Furnaces Heating Apparatus is: be first raised to 400 DEG C with the speed of 10 DEG C/min, again with the speed to 900 DEG C of 15 DEG C/min, afterwards with 5 DEG C/min speed to 1150 DEG C, at 1150 DEG C, to the micropore glass heat preservation sintering 3h after soaking, glass cools to room temperature with the furnace and takes out.Through cutting and polishing, making containing chemical general formula is Y
0.5gd
0.45tm
0.05vO
4the high silica blue luminescent glass of nano luminescent crystallite.
Embodiment 3
Take the lanthanum nitrate hexahydrate (La (NO of 0.09999mol
3)
36H
2o), the metavanadic acid ammonia (NH of 0.1mol
4vO
3) and 10
-5the six nitric hydrate thulium (Tm (NO of mol
3)
3) 6H
2o is dissolved in the distilled water of 1000ml, is mixed with and contains 0.09999mol/L La
3+, 0.1mol/L vanadium ion and 10
-5mol/L Tm
3+soaking solution.By high silica nanometer micropore glass (98.0%SiO
2, 1.0%B
2o
3, 1.0%Al
2o
3; And micro pore volume account for high silica nanometer micropore glass cumulative volume 35%) be dipped in soaking solution and take out after 30min, at room temperature dry in the air and insert in High Temperature Furnaces Heating Apparatus to surface drying, the temperature-rise period of High Temperature Furnaces Heating Apparatus is: be first raised to 400 DEG C with the speed of 10 DEG C/min, again with the speed to 900 DEG C of 15 DEG C/min, afterwards with 5 DEG C/min speed to 1200 DEG C, at 1200 DEG C, to the micropore glass heat preservation sintering 4h after soaking, glass cools to room temperature with the furnace and takes out.Through cutting and polishing, making containing chemical general formula is La
0.9999tm
0.0001vO
4the high silica blue luminescent glass of nano luminescent crystallite.
Embodiment 4
Take the lanthanum nitrate hexahydrate (La (NO of 0.03475mol
3)
36H
2o), the gadolinium nitrate hexahydrate of 0.015mol (Gd (NO
3)
36H
2o), the vanadylic sulfate (VOSO of 0.5mol
4) and the six nitric hydrate thulium (Tm (NO of 0.00025mol
3)
3) 6H
2o is dissolved in the distilled water of 100ml, is mixed with and contains 0.3475mol/LLa
3+, 0.15mol/L Gd
3+, 0.5mol/L vanadium ion and 0.0025mol/L Tm
3+soaking solution.By high silica nanometer micropore glass (96.0%SiO
2, 1.0%B
2o
3, 3.0%Al
2o
3; And micro pore volume account for high silica nanometer micropore glass cumulative volume 40%) be dipped in soaking solution and take out after 3h, at room temperature dry in the air and insert in High Temperature Furnaces Heating Apparatus to surface drying, the temperature-rise period of High Temperature Furnaces Heating Apparatus is: be first raised to 400 DEG C with the speed of 10 DEG C/min, again with the speed to 900 DEG C of 15 DEG C/min, afterwards with 5 DEG C/min speed to 1250 DEG C, at 1250 DEG C, to the micropore glass heat preservation sintering 5h after soaking, glass cools to room temperature with the furnace and takes out.Through cutting and polishing, making containing chemical general formula is La
0.695gd
0.3tm
0.005vO
4the high silica blue luminescent glass of nano luminescent crystallite.
Embodiment 5
Take the gadolinium nitrate hexahydrate (Gd (NO of 0.14985mol
3)
36H
2o), the vanadylic sulfate (VOSO of 0.15mol
4) and the six nitric hydrate thulium (Tm (NO of 0.00015mol
3)
3) 6H
2o is dissolved in the distilled water of 100ml, is mixed with and contains 1.4985mol/L Gd
3+, 1.5mol/L vanadium ion and 0.0015mol/L Tm
3+soaking solution.By high silica nanometer micropore glass (96.0%SiO
2, 2.0%B
2o
3, 2.0%Al
2o
3; And micro pore volume account for high silica nanometer micropore glass cumulative volume 27%) be dipped in soaking solution and take out after 1h, at room temperature dry in the air and insert in High Temperature Furnaces Heating Apparatus to surface drying, the temperature-rise period of High Temperature Furnaces Heating Apparatus is: be first raised to 400 DEG C with the speed of 10 DEG C/min, again with the speed to 900 DEG C of 15 DEG C/min, afterwards with 5 DEG C/min speed to 1350 DEG C, at 1350 DEG C, to the micropore glass heat preservation sintering 2h after soaking, glass cools to room temperature with the furnace and takes out.Through cutting and polishing, making containing chemical general formula is Gd
0.999tm
0.001vO
4the high silica blue luminescent glass of nano luminescent crystallite.
Embodiment 6
Take the six nitric hydrate yttrium (Y (NO of 0.01mol
3)
36H
2o), take the lanthanum nitrate hexahydrate (La (NO of 0.0049mol
3)
36H
2o), the gadolinium nitrate hexahydrate of 0.005mol (Gd (NO
3)
36H
2o), the vanadylic sulfate (VOSO of 0.02mol
4) and the six nitric hydrate thulium (Tm (NO of 0.0001mol
3)
3) 6H
2o is dissolved in the distilled water of 100ml, is mixed with and contains 0.1mol/L Y
3+, 0.049mol/L La
3+, 0.05mol/L Gd
3+, 0.2mol/L vanadium ion and 0.001mol/L Tm
3+soaking solution.By high silica nanometer micropore glass (97.0%SiO
2, 1.5%B
2o
3, 1.5%Al
2o
3; And micro pore volume account for high silica nanometer micropore glass cumulative volume 38%) be dipped in soaking solution and take out after 5h, at room temperature dry in the air and insert in High Temperature Furnaces Heating Apparatus to surface drying, the temperature-rise period of High Temperature Furnaces Heating Apparatus is: be first raised to 400 DEG C with the speed of 10 DEG C/min, again with the speed to 900 DEG C of 15 DEG C/min, afterwards with 5 DEG C/min speed to 1350 DEG C, at 1000 DEG C, to the micropore glass heat preservation sintering 3h after soaking, glass cools to room temperature with the furnace and takes out.Through cutting and polishing, making containing chemical general formula is Y
0.5la
0.245gd
0.25tm
0.005vO
4the high silica blue luminescent glass of nano luminescent crystallite.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (10)
1. a high silica blue luminescent glass, is characterized in that, includes high silica nanometer micropore glass baseplate in this high silica blue luminescent glass, and be evenly distributed in described high silica nanometer micropore glass baseplate in micropore, chemical general formula is Re
1-xtm
xvO
4nano luminescent crystallite; Wherein, Re is that Y and La and Gd, Re are that Gd and La or Re are La, and the span of x is 1 × 10
-4～0.05.
2. high silica blue luminescent glass according to claim 1, is characterized in that, described high silica nanometer micropore glass baseplate comprises that weight percent component is: 94.0%～98.0% SiO
2, 1.0%～3.0% B
2o
3, 1.0%～3.0% Al
2o
3.
3. a preparation method for high silica blue luminescent glass, comprises the steps:
According to chemical general formula Re
1-xtm
xvO
4in the stoichiometric ratio of each element, source compound, the source compound of Tm and the source compound of V of Re are provided, be then configured to the soaking solution containing Re ion, Tm ion and V ion; Wherein, Re is that Y and La and Gd, Re are that Gd and La or Re are La, and the span of x is 1 × 10
-4～0.05;
High silica nanometer micropore glass baseplate is put into above-mentioned soaking solution to be soaked;
The high silica nanometer micropore glass baseplate soaking is put at 1000～1350 DEG C and carried out sintering processes 1～5h, make described high silica blue luminescent glass.
4. the preparation method of high silica blue luminescent glass according to claim 3, is characterized in that, at least one in the vitriol of the nitrate that the source compound of Re is Re, the muriate of Re or Re; The source compound of Tm is at least one in nitrate, the muriate of Tm or the vitriol of Tm of Tm; The source compound of V is at least one in vanadylic sulfate or metavanadic acid ammonia.
5. according to the preparation method of the high silica blue luminescent glass described in claim 3 or 4, it is characterized in that, in described soaking solution, Tm ion volumetric molar concentration is 1 × 10
-5～0.1mol/L, Re ion volumetric molar concentration is 0.1～2mol/L, V ion volumetric molar concentration is 0.1～2mol/L.
6. the preparation method of high silica blue luminescent glass according to claim 3, is characterized in that, described high silica nanometer micropore glass baseplate comprises that weight percent component is: 94.0%～98.0% SiO
2, 1.0%～3.0% B
2o
3, 1.0%～3.0% Al
2o
3.
7. according to the preparation method of the high silica blue luminescent glass described in claim 3 or 6, it is characterized in that, in described high silica nanometer micropore glass baseplate, the micro pore volume on this high silica nanometer micropore glass baseplate accounts for 25～40% of high silica nanometer micropore glass cumulative volume.
8. the preparation method of high silica blue luminescent glass according to claim 3, is characterized in that, described high silica nanometer micropore glass baseplate is put into above-mentioned soaking solution soak time 10min～5h.
9. the preparation method of high silica blue luminescent glass according to claim 8, is characterized in that, described high silica nanometer micropore glass baseplate is put into above-mentioned soaking solution soak time 30min～5h.
10. the preparation method of high silica blue luminescent glass according to claim 3, it is characterized in that, described sintering processes also comprises: be first warmed up to 400 DEG C with the speed of 10 DEG C/min, then be warmed up to 900 DEG C with the speed of 15 DEG C/min, be warmed up to 1000～1350 DEG C afterwards with 5 DEG C/min speed.
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