CN103923652A - Hollow structure calcium titanate luminescent material and preparation method thereof - Google Patents
Hollow structure calcium titanate luminescent material and preparation method thereof Download PDFInfo
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- CN103923652A CN103923652A CN201310014469.6A CN201310014469A CN103923652A CN 103923652 A CN103923652 A CN 103923652A CN 201310014469 A CN201310014469 A CN 201310014469A CN 103923652 A CN103923652 A CN 103923652A
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Abstract
Belonging to the field of luminescent materials, the invention discloses a hollow structure calcium titanate luminescent material and a preparation method thereof. The structural general formula of the luminescent material is Ca1-xTiO3:Prx, wherein x is greater than 0 and smaller than or equal to 0.01. The hollow structure calcium titanate luminescent material prepared by the invention adopts dispersed spheres as the template, the obtained calcium titanate has a spherical hollow structure, not only has a controllable shape, but also can effectively reduce the use amount of rare earth metals, thus reducing the product cost and greatly saving valuable rare earth resources.
Description
Technical field
The present invention relates to field of light emitting materials, relate in particular to a kind of hollow structure calcium titanate luminescent material and preparation method thereof.
Background technology
Several large class materials such as that red fluorescence powder comprises is sulfide-based, oxide-based, oxysulfide class and metatitanic acid salt, wherein, metatitanic acid salt material has the advantages such as higher stability, color developing is good, can be used for the occasion that fluorescent material job stability is had relatively high expectations, as the field emission display screen using under low voltage and high current density.The Typical Representative material C aTiO of metatitanic acid salt
3: the cie color coordinate of Pr is x=0.680 and y=0.311, very approaching with desirable ruddiness, is a kind of more satisfactory fluorescent material, has larger application prospect.
But mostly with high temperature solid-state method, prepare at present, the pattern of gained fluorescent material is inhomogeneous, thereby need repetitious ball milling to obtain suitable granularity (5-10 μ m), the defect that mechanical milling process produces and the impurity of introducing damage the luminous intensity of luminescent powder sometimes.
Summary of the invention
Problem to be solved by this invention is to provide that a kind of pattern is even, the good hollow structure calcium titanate luminescent material of luminous intensity.
Technical scheme of the present invention is as follows:
A hollow structure calcium titanate luminescent material, its general structure is Ca
1-xtiO
3: Pr
x; Wherein, the span of x is 0 < x≤0.01.
Described hollow structure calcium titanate luminescent material, preferably, the span of x is 0.001≤x≤0.005.
The present invention makes hollow structure calcium titanate luminescent material, and adopting the carbon bead disperseing is template, and the calcium titanate obtaining is spherical hollow structure, not only pattern is controlled, and the consumption that can effectively reduce rare earth metal, has reduced product cost, saves in a large number precious rare earth resources.
The present invention also provides the preparation method of above-mentioned hollow structure calcium titanate luminescent material, comprises the steps:
The sucrose that is 0.00075 ~ 0.15g/ml by concentration or the ethanolic soln of glucose are placed in reactor, after sealed reactor, at 120 ~ 200 ℃, react 5 ~ 36h, be cooled to centrifugation after room temperature, and the solid phase obtaining is washed, obtained carbon bead template after dry;
According to general structure, be Ca
1-xtiO
3: Pr
xin each element chemistry metering ratio, in the ethanolic soln of the tetrabutyl titanate that is 1mol/L toward concentration, adding concentration is the Pr (NO of 0.005 ~ 0.1mol/L
3)
3ca (the NO of solution and 0.1 ~ 1mol/L
3)
2solution, obtains mixing solutions; The pH value that regulates subsequently mixing solutions is 2 ~ 3; Then add again carbon bead template, stirring 0.5-6h, more then in the situation that stirring, slowly add oxalic acid sinking agent, and produce precipitation, follow stirring reaction 2-8h, then suction filtration dry, obtains Ca
1-xtiO (C
2o
4)
2: Pr
x@C presoma; Wherein, described carbon bead template and Ca
1-xtiO
3: Pr
xmol ratio be 0.025:1 ~ 10:1; @represents Ca
1-xtiO (C
2o
4)
2: Pr
xcoated C (carbon), C is also carbon bead template;
Described presoma is ground, and will grind powder pre-burning 1 ~ 6 hour at 500 ~ 800 ℃, after cooling, grind, and then calcine 1 ~ 10h in 800～1200 ℃, obtain Ca
1-xtiO
3: Pr
xluminescent material; Wherein, the pre-burning of described grinding powder and calcining are all under air atmosphere, in high temperature box furnace, carry out.
In above-mentioned steps, the span of x is 0 < x≤0.01.
The preparation method of described hollow structure calcium titanate luminescent material, preferably, the reactor in described carbon bead template preparation process is teflon-lined reactor.
The preparation method of described hollow structure calcium titanate luminescent material preferably, is to use successively deionized water and dehydrated alcohol repetitive scrubbing repeatedly to the washing of described separated solid phase.
The preparation method of described hollow structure calcium titanate luminescent material, preferably, carries out at 60 ~ 80 ℃ the dry of the solid phase after described washing.
The preparation method of described hollow structure calcium titanate luminescent material, preferably, when the pH value to described mixing solutions regulates, adopts HNO
3carry out.
The preparation method of described hollow structure calcium titanate luminescent material, preferably, the relative Ca of mole dosage of described sinking agent
2+and TiO
2+mole dosage excessive 25%; Sinking agent utilizes the TiO of hydrolysis in the butyl (tetra) titanate aqueous solution
2+with C
2o
4 2-form TiO (C
2o
4)
2 2-the feature of complex ion, first forms complex ion, then makes it react generation CaTi O (C with Ca
2o
4)
2presoma.
The preparation method of described hollow structure calcium titanate luminescent material, preferably, the span of x is 0.001≤x≤0.005.
The preparation method of hollow structure calcium titanate luminescent material of the present invention, first adopts hydrothermal method to prepare carbon bead, and then take carbon bead and prepare Ca as template adopts oxalate precipitation method
1-xtiO (C
2o
4)
2: Pr
x@C precursor powder, and then through calcining, in calcination process, carbon bead will be converted into CO
2overflow, finally obtain hollow structure Ca
1-xtiO
3: Pr
xluminescent material.
The preparation method of hollow structure calcium titanate luminescent material of the present invention, processing step is few, relatively simple; Processing condition are not harsh, easily reach, and cost is low; Do not introduce other impurity, the luminescent material quality obtaining is high, can be widely used in the preparation of luminescent material.
Accompanying drawing explanation
Fig. 1 is that hollow structure calcium titanate luminescent material and the contrast luminescent material of embodiment 2 preparations is the luminescent spectrum comparison diagram under the cathode-ray exciting under 1.5KV at acceleration voltage; Wherein, curve 1 is the hollow structure calcium titanate luminescent material Ca of the hollow structure that makes of embodiment 3
0.998tiO
3: Pr
0.002luminescent spectrum, curve 2 is contrast luminescent material Ca
0.998tiO
3: Pr
0.002luminescent spectrum.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
The precipitator method are prepared Ca
0.999tiO
3: Pr
0.001
Take 4g glucose and be dissolved in the sorbitol solution that dehydrated alcohol obtains 40mL, this solution is proceeded in 50mL band teflon-lined reactor, after adding a cover and screwing, in 120 ℃ of reaction 36h, prepare the solution of carbon bead, this solution of centrifugation obtains solid formation, with deionized water and dehydrated alcohol, washs respectively 2 times, and dry at 60 ℃, obtain carbon bead template.
In tetrabutyl titanate being dissolved into ethanol under magnetic agitation, obtain 1mol/L clear solution, then according to stoichiometric ratio, pipette 4mL1mol/L tetrabutyl titanate, then add 0.4mL0.01mol/L Pr (NO
3)
3with 39.96mL0.1mol/L Ca (NO
3)
2, adopt HNO
3regulator solution pH value is 2, adds carbon bead template 480mg, stirs 0.5h, then in the situation that stirring, slowly adds 20mL0.5mol/L sinking agent oxalic acid, produces precipitation, then stirring reaction 8h.Then suction filtration dry, obtains Ca
0.999tiO (C
2o
4)
2: Pr
0.001@C presoma;
Presoma is ground, be put in high temperature box furnace in air in 500 ℃ of pre-burnings 6 hours, after cooling, grind, and then in 700 ℃ of calcining 10h, obtain Ca
0.999tiO
3: Pr
0.001luminescent material.
Embodiment 2
The precipitator method are prepared Ca
0.998tiO
3: Pr
0.002
Take 0.05g sucrose dissolved and in dehydrated alcohol, obtain the sucrose alcohol solution of 40mL, this solution is proceeded in 50mL band teflon-lined reactor, after adding a cover and screwing, in 160 ℃ of reaction 20h, prepare the solution of carbon bead, this solution of centrifugation obtains solid formation, with deionized water and dehydrated alcohol, washs respectively 3 times, and dry at 80 ℃, obtain carbon bead template.
In tetrabutyl titanate being dissolved into ethanol under magnetic agitation, obtain 1mol/L clear solution, then according to stoichiometric ratio, pipette 4mL1mol/L tetrabutyl titanate, then add 0.4mL0.02mol/L Pr (NO
3)
3with 19.96mL0.2mol/L Ca (NO
3)
2, adopt HNO
3regulator solution pH value is 3, adds carbon bead template 200mg, stirs 2h, then in the situation that stirring, slowly adds 20mL0.5mol/L sinking agent oxalic acid, produces precipitation, then stirring reaction 4h.Then suction filtration dry, obtains Ca
0.998tiO (C
2o
4)
2: Pr
0.002@C presoma;
Presoma is ground, be put in high temperature box furnace calcining at constant temperature 4h at 700 ℃, after cooling, grind, and then in 1000 ℃ of calcining 4h, obtain Ca
0.998tiO
3: Pr
0.002luminescent material.
Fig. 1 is that hollow structure calcium titanate luminescent material and the contrast luminescent material of embodiment 3 preparations is the luminescent spectrum comparison diagram under the cathode-ray exciting under 1.5KV at acceleration voltage; Wherein, curve 1 is the hollow structure calcium titanate luminescent material Ca of the hollow structure that makes of embodiment 3
0.998tiO
3: Pr
0.002luminescent spectrum, curve 2 is contrast luminescent material Ca
0.998tiO
3: Pr
0.002luminescent spectrum.
As can be seen from Figure 2, the emission peak at 612nm place, the luminous intensity of luminescent material prepared by the present embodiment has strengthened 17%.
Embodiment 3
The precipitator method are prepared Ca
0.995tiO
3: Pr
0.005
Take 0.003g glucose and be dissolved in the sorbitol solution that dehydrated alcohol obtains 40mL, this solution is proceeded in 50mL band teflon-lined reactor, after adding a cover and screwing, in 150 ℃ of reaction 10h, prepare the solution of carbon bead, this solution of centrifugation obtains solid formation, with deionized water and dehydrated alcohol, washs respectively 2 times, and dry at 70 ℃, obtain carbon bead template.
In tetrabutyl titanate being dissolved into ethanol under magnetic agitation, obtain 1mol/L clear solution, then according to stoichiometric ratio, pipette 4mL1mol/L tetrabutyl titanate, then add 2mL0.01mol/L Pr (NO
3)
3with 7.96mL0.5mol/L Ca (NO
3)
2, adopt HNO
3regulator solution pH value is 3, adds carbon bead template 4.8mg, stirs 0.5h, then in the situation that stirring, slowly adds sinking agent oxalic acid, produces precipitation, then stirring reaction 8h.Then suction filtration dry, obtains Ca
0.995tiO (C
2o
4)
2: Pr
0.005@C presoma;
Presoma is ground, be put in high temperature box furnace calcining at constant temperature 6h at 500 ℃, after cooling, grind, and then in 1200 ℃ of calcining 1h, obtain Ca
0.995tiO
3: Pr
0.005luminescent material.
Embodiment 4
The precipitator method are prepared Ca
0.99tiO
3: Pr
0.01
Take 5g glucose and be dissolved in the sorbitol solution that dehydrated alcohol obtains 40mL, this solution is proceeded in 50mL band teflon-lined reactor, after adding a cover and screwing, in 180 ℃ of reaction 24h, prepare the solution of carbon bead, this solution of centrifugation obtains solid formation, with deionized water and dehydrated alcohol, washs respectively 2 times, and dry at 60 ℃, obtain carbon bead template.
In tetrabutyl titanate being dissolved into ethanol under magnetic agitation, obtain 1mol/L clear solution, then according to stoichiometric ratio, pipette 4mL1mol/L tetrabutyl titanate, then add 0.8mL0.005mol/LPr (NO
3)
3with 3.96mL1mol/L Ca (NO
3)
2, adopt HNO
3regulator solution pH value is 3, adds carbon bead template 1.2mg, stirs 0.5-6h, then in the situation that stirring, slowly adds 10mL1mol/L sinking agent oxalic acid, produces precipitation, then stirring reaction 2-8h.Then suction filtration dry, obtains Ca
0.99tiO (C
2o
4)
2: Pr
0.01@C presoma;
Presoma is ground, be put in high temperature box furnace calcining at constant temperature 1h at 700 ℃, after cooling, grind, and then in 900 ℃ of calcining 10h, obtain Ca
0.99tiO
3: Pr
0.01luminescent material.
Embodiment 5
The precipitator method are prepared Ca
0.996tiO
3: Pr
0.004
Take 6g sucrose dissolved and in dehydrated alcohol, obtain the sucrose alcohol solution of 40mL, this solution is proceeded in 50mL band teflon-lined reactor, after adding a cover and screwing, in 200 ℃ of reaction 5h, prepare the solution of carbon bead, this solution of centrifugation obtains solid formation, with deionized water and dehydrated alcohol, washs respectively 2 times, and dry at 75 ℃, obtain carbon bead template.
In tetrabutyl titanate being dissolved into ethanol under magnetic agitation, obtain 1mol/L clear solution, then according to stoichiometric ratio, pipette 4mL1mol/L tetrabutyl titanate, then add 0.32mL0.05mol/LPr (NO
3)
3with 19.92mL0.2mol/L Ca (NO
3)
2, adopt HNO
3regulator solution pH value is 2.5, adds carbon bead template 100mg, stirs 4h, then in the situation that stirring, slowly adds 20mL0.5mol/L sinking agent oxalic acid, produces precipitation, then stirring reaction 5h.Then suction filtration dry, obtains Ca
0.996tiO (C
2o
4)
2: Pr
0.004@C presoma;
Presoma is ground, be put in high temperature box furnace calcining at constant temperature 3h at 600 ℃, after cooling, grind, and then in 700 ℃ of calcining 5h, obtain Ca
0.996tiO
3: Pr
0.004luminescent material.
Embodiment 6
The precipitator method are prepared Ca
0.994tiO
3: Pr
0.006
Take 5.705g sucrose dissolved and in dehydrated alcohol, obtain the sucrose alcohol solution of 40mL, this solution is proceeded in 50mL band teflon-lined reactor, after adding a cover and screwing, in 140 ℃ of reaction 15h, prepare the solution of carbon bead, this solution of centrifugation obtains solid formation, with deionized water and dehydrated alcohol, washs respectively 2 times, and dry at 80 ℃, obtain carbon bead template.
In tetrabutyl titanate being dissolved into ethanol under magnetic agitation, obtain 1mol/L clear solution, then according to stoichiometric ratio, pipette 4mL1mol/L tetrabutyl titanate, then add 0.24mL0.1mol/L Pr (NO
3)
3with 19.88mL0.2mol/L Ca (NO
3)
2, adopt HNO
3regulator solution pH value is 2, adds carbon bead template 150mg, stirs 3h, then in the situation that stirring, slowly adds 10mL1mol/L sinking agent oxalic acid, produces precipitation, then stirring reaction 6h.Then suction filtration dry, obtains Ca
0.994tiO (C
2o
4)
2: Pr
0.006@C presoma;
Presoma is ground, be put in high temperature box furnace calcining at constant temperature 2h at 550 ℃, after cooling, grind, and then in 800 ℃ of calcining 8h, obtain Ca
0.994tiO
3: Pr
0.006luminescent material.
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 hollow structure calcium titanate luminescent material, is characterized in that, its general structure is Ca
1-xtiO
3: Pr
x; Wherein, the span of x is 0 < x≤0.01.
2. hollow structure calcium titanate luminescent material according to claim 1, is characterized in that, the span of x is 0.001≤x≤0.005.
3. a preparation method for hollow structure calcium titanate luminescent material, is characterized in that, comprises the steps:
The sucrose that is 0.00075 ~ 0.15g/ml by concentration or the ethanolic soln of glucose are placed in reactor, after sealed reactor, at 120 ~ 200 ℃, react 5 ~ 36h, be cooled to centrifugation after room temperature, and the solid phase obtaining is washed, obtained carbon bead template after dry;
According to general structure, be Ca
1-xtiO
3: Pr
xin each element chemistry metering ratio, in the ethanolic soln of the tetrabutyl titanate that is 1mol/L toward concentration, adding concentration is the Pr (NO of 0.005 ~ 0.1mol/L
3)
3ca (the NO of solution and 0.1 ~ 1mol/L
3)
2solution, obtains mixing solutions; The pH value that regulates subsequently mixing solutions is 2 ~ 3; Then add again carbon bead template, stirring 0.5-6h, more then in the situation that stirring, slowly add oxalic acid sinking agent, and produce precipitation, follow stirring reaction 2-8h, then suction filtration dry, obtains Ca
1-xtiO (C
2o
4)
2: Pr
x@C presoma; Wherein, described carbon bead template and Ca
1-xtiO
3: Pr
xmol ratio be 0.025:1 ~ 10:1;
Described presoma is ground, and will grind powder pre-burning 1 ~ 6 hour at 500 ~ 800 ℃, after cooling, grind, and then calcine 1 ~ 10h in 800～1200 ℃, obtain Ca
1-xtiO
3: Pr
xluminescent material;
In above-mentioned steps, the span of x is 0 < x≤0.01.
4. the preparation method of hollow structure calcium titanate luminescent material according to claim 3, is characterized in that, the reactor in described carbon bead template preparation process is teflon-lined reactor.
5. the preparation method of hollow structure calcium titanate luminescent material according to claim 3, is characterized in that, to the washing of described separated solid phase, is to use successively deionized water and dehydrated alcohol repetitive scrubbing repeatedly.
6. the preparation method of hollow structure calcium titanate luminescent material according to claim 3, is characterized in that, the dry of the solid phase after described washing carried out at 60 ~ 80 ℃.
7. the preparation method of hollow structure calcium titanate luminescent material according to claim 3, is characterized in that, when the pH value to described mixing solutions regulates, adopts HNO
3carry out.
8. the preparation method of hollow structure calcium titanate luminescent material according to claim 3, is characterized in that, the relative Ca of mole dosage of described sinking agent
2+and TiO
2+mole dosage excessive 25%.
9. the preparation method of hollow structure calcium titanate luminescent material according to claim 3, is characterized in that, the pre-burning of described grinding powder and calcining all under air atmosphere, carry out in high temperature box furnace.
10. the preparation method of hollow structure calcium titanate luminescent material according to claim 3, is characterized in that, the span of x is 0.001≤x≤0.005.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104971710A (en) * | 2015-07-24 | 2015-10-14 | 成都理工大学 | Photocatalyst with luminescent property and preparation method and application thereof |
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| CN102337136B (en) * | 2010-07-21 | 2013-08-07 | 海洋王照明科技股份有限公司 | Metal-nanoparticle-doped oxide luminescent material with hollow structure and preparation method thereof |
| CN102477294B (en) * | 2010-11-25 | 2014-04-02 | 海洋王照明科技股份有限公司 | Calcium titanate luminescent material and preparation method thereof |
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