CN103923657B - Orthophosphate luminescence material having hollow structure, and preparation method thereof - Google Patents
Orthophosphate luminescence material having hollow structure, and preparation method thereof Download PDFInfo
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- CN103923657B CN103923657B CN201310011218.2A CN201310011218A CN103923657B CN 103923657 B CN103923657 B CN 103923657B CN 201310011218 A CN201310011218 A CN 201310011218A CN 103923657 B CN103923657 B CN 103923657B
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- hollow structure
- luminescent material
- preparation
- acid salt
- orthophosphoric acid
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Abstract
The invention belongs to the field of luminescence materials, and discloses an orthophosphate luminescence material having a hollow structure, and a preparation method thereof, wherein the structure general formula of the luminescence material is Ba3-xGd(PO4)3:Dyx, and x is more than 0 and is less than or equal to 0.2. According to the orthophosphate luminescence material having the hollow structure, the dispersed carbon spheres are adopted as the template so as to obtain the hollow structure having the spherical orthophosphate, such that the morphology can be controlled, and the luminescence efficiency is enhanced.
Description
Technical field
The present invention relates to field of light emitting materials, particularly relate to a kind of hollow structure orthophosphoric acid salt luminescent material and preparation method thereof.
Background technology
Present commercial luminescent material is prepared with high temperature solid-state method mostly, pyroreaction big energy-consuming and size distribution is uneven, and powder pattern is different, need by the method for ball milling to obtain the fluorescent material of 2-8 micron grain size, and making powder granule size inconsistent, pattern is imperfect, causes coating uneven.People are by using sol-gel method, hydrothermal synthesis method, and the methods such as complex coacervation method prepare fluorescent material, and these methods can make up the deficiency of high temperature solid phase synthesis, but the luminous intensity of the fluorescent material of these method gained is not as high temperature solid phase synthesis.Obtain size, target that morphology controllable and the luminescent material of good luminous performance are researchist's effort always.
Summary of the invention
Problem to be solved by this invention is to provide that a kind of pattern is even, luminous intensity good hollow structure orthophosphoric acid salt luminescent material.
Technical scheme of the present invention is as follows:
A kind of hollow structure orthophosphoric acid salt luminescent material, its general structure is Ba
3-xgd (PO
4)
3: Dy
x; Wherein, the span of x is 0 < x≤0.2.
Described hollow structure orthophosphoric acid salt luminescent material, preferably, the span of x is 0.02≤x≤0.1.
The present invention obtains hollow structure orthophosphoric acid salt luminescent material, and the carbon bead adopting dispersion is template, and the orthophosphoric acid salt obtained is spherical hollow structure, not only morphology controllable, and effectively can reduce the consumption of rare earth metal, reduce product cost, a large amount of rare earth resources saving preciousness.
The present invention also provides the preparation method of above-mentioned hollow structure orthophosphoric acid salt luminescent material, comprises the steps:
Be that the sucrose of 0.00075 ~ 0.15g/ml or the ethanolic soln of glucose are placed in reactor by concentration, at 120 ~ 200 DEG C, 5 ~ 36h is reacted after sealed reactor, be cooled to centrifugation after room temperature, and the solid phase obtained is washed, obtain carbon bead template after drying;
Be Ba according to general structure
3-xgd (PO
4)
3: Dy
xin each element chemistry metering ratio, provide the salts solution of Ba, Gd and Dy to mix respectively, obtain mixing solutions; The pH value of mixing solutions is regulated to be 1 ~ 3 subsequently; Then add carbon bead template again, stir 0.5-6h, more then slowly add (NH when stirring
4)
2hPO
4sinking agent, produces precipitation, then stirring reaction 2-8h, and then suction filtration is also dry, obtains Ba
3-xgd (PO
4)
3: Dy
x@C presoma; Wherein, described carbon bead template and Ba
3-xgd (PO
4)
3: Dy
xmol ratio be 0.025:1 ~ 10:1; Ba
3-xgd (PO
4)
3: Dy
x@C represents Ba
3-xgd (PO
4)
3: Dy
xcoated C, C are also carbon bead template;
Described presoma is ground, and powder pre-burning 1 ~ 6 hour at 600 ~ 1000 DEG C will be ground, grinding after cooling, and then in 1100 ~ 1300 DEG C of calcining 1 ~ 6h, obtain Ba
3-xgd (PO
4)
3: Dy
xluminescent material; Wherein, pre-burning and the calcining of described grinding powder are all in air atmosphere, carry out in high temperature box furnace.
In above-mentioned steps, the span of x is 0 < x≤0.2.
The preparation method of described hollow structure orthophosphoric acid salt luminescent material, preferably, the reactor in described carbon bead template preparation process is teflon-lined reactor.
The preparation method of described hollow structure orthophosphoric acid salt luminescent material preferably, is use deionized water and dehydrated alcohol repetitive scrubbing successively repeatedly to the washing of the solid phase that described centrifugation obtains.
The preparation method of described hollow structure orthophosphoric acid salt luminescent material, preferably, carries out at 60 ~ 80 DEG C the drying of the solid phase after described washing.
The preparation method of described hollow structure orthophosphoric acid salt luminescent material, preferably, the salts solution of described Ba is respectively barium acetate or nitrate of baryta that concentration is 0.5 ~ 5mol/L; The salts solution of described Gd is respectively gadolinium acetate or Gadolinium trinitrate that concentration is 0.2 ~ 2mol/L; The salts solution of described Dy is respectively acetic acid dysprosium or Dysprosium trinitrate that concentration is 0.01 ~ 0.5mol/L;
The preparation method of described hollow structure orthophosphoric acid salt luminescent material, preferably, when regulating the pH value of described mixing solutions, adopts HNO
3carry out.
The preparation method of described hollow structure orthophosphoric acid salt luminescent material, preferably, the relative Ba of mole dosage of described sinking agent
2+and Gd
3+mole dosage excessive 25%; The effect of sinking agent is sedimentation Ba
2+and Gd
3+, its principle is as follows:
3Ba
2++3HPO
4 2-＋9H
＋＋6NH
4 ＋=Ba
3(PO
4)
2↓+PO
4 3-＋6NH
3
Gd
3++HPO
4 2-＋3H
＋＋2NH
4 ＋=Gd(PO
4)↓＋2NH
3。
The preparation method of described hollow structure orthophosphoric acid salt luminescent material, preferably, the span of x is 0.02≤x≤0.1.
The preparation method of hollow structure orthophosphoric acid salt luminescent material of the present invention, first adopts hydrothermal method to prepare carbon bead, and then with carbon bead for template adopts the precipitator method to prepare Ba
3-xgd (PO
4)
3: Dy
x@C precursor powder, and then through calcining, in calcination process, carbon bead will be converted into CO
2effusion, finally obtains hollow structure Ba
3-xgd (PO
4)
3: Dy
xluminescent material.
The preparation method of hollow structure orthophosphoric acid salt luminescent material of the present invention, processing step is few, relatively simply; Processing condition are not harsh, easily reach, and cost is low; Do not introduce other impurity, the luminescent material quality obtained is high, can be widely used in the preparation of luminescent material.
Accompanying drawing explanation
Fig. 1 is the embodiment 2 hollow structure orthophosphoric acid salt luminescent material prepared and the luminescent spectrum comparison diagram contrasted under the cathode-ray exciting of luminescent material under acceleration voltage is 1.5KV; Wherein, curve 1 is the hollow structure orthophosphoric acid salt luminescent material Ba of the hollow structure that embodiment 2 obtains
2.94gd (PO
4)
3: Dy
0.06luminescent spectrum, curve 2 is contrast luminescent material Ba
2.94gd (PO
4)
3: Dy
0.06luminescent spectrum.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
The precipitator method prepare Ba
2.8gd (PO
4)
3: Dy
0.2
Take 4g glucose and be dissolved in the sorbitol solution that dehydrated alcohol obtains 40mL, this solution being proceeded to 50mL is with in teflon-lined reactor, add a cover after screwing, in 120 DEG C of reaction 36h, prepare the solution of carbon bead template, this solution of centrifugation obtains solid formation, washs 2 times respectively with deionized water and dehydrated alcohol, and dry at 60 DEG C, namely obtain carbon bead template.
According to Ba
2.8gd (PO
4)
3: Dy
0.2stoichiometry ratio measure 22.4mL0.5mol/LBa (CH
3cOO)
2, 4mL1mol/L Gd (CH
3cOO)
3with 1.6mL0.5mol/L Dy (CH
3cOO)
3solution mixes, and obtains mixing solutions, uses HNO
3the pH regulating mixing solutions is 1, then adds carbon bead template 480mg, stirs 0.5h.Separately get (NH
4)
2hPO
4under agitation it is slowly joined mixing solutions after being dissolved in deionized water the solution making 0.5mol/L, (NH
4)
2hPO
4the add-on of solution is 30mL, is precipitated, then stirring reaction 2h.Then suction filtration is also dry, obtains Ba
2.8gd (PO
4)
3: Dy
0.2@C presoma;
Presoma is ground, is put in atmosphere in 600 DEG C of pre-burnings 6 hours in high temperature box furnace, grinding after cooling, and then in 1100 DEG C of calcining 8h, obtain the Ba of hollow structure
2.8gd (PO
4)
3: Dy
0.2luminescent material.
Embodiment 2
The precipitator method prepare the Ba of hollow structure
2.94gd (PO
4)
3: Dy
0.06
Take 0.05g sucrose dissolved obtains 40mL sucrose alcohol solution in dehydrated alcohol, this solution being proceeded to 50mL is with in teflon-lined reactor, add a cover after screwing, in 160 DEG C of reaction 20h, prepare the solution of carbon bead template, this solution of centrifugation obtains solid formation, washs 3 times respectively with deionized water and dehydrated alcohol, and dry at 80 DEG C, namely obtain carbon bead template.
According to Ba
2.94gd (PO
4)
3: Dy
0.06stoichiometry ratio measure 11.76mL1mol/L Ba (NO
3)
2, 4mL1mol/L Gd (NO
3)
3with 4.8mL0.05mol/L Dy (NO
3)
3solution mixes, and obtains mixing solutions, uses HNO
3the pH regulating mixing solutions is 2, then adds carbon bead template 200mg, stirs 2h.Separately get (NH
4)
2hPO
4under agitation it is slowly joined mixing solutions after being dissolved in deionized water the solution making 1mol/L, (NH
4)
2hPO
4the add-on of solution is 15mL, is precipitated, then stirring reaction 4h.Then suction filtration is also dry, obtains Ba
2.94gd (PO
4)
3: Dy
0.06@C presoma;
Presoma is ground, is put in atmosphere in 800 DEG C of pre-burnings 2 hours in high temperature box furnace, grinding after cooling, and then in 1200 DEG C of calcining 4h, obtain the Ba of hollow structure
2.94gd (PO
4)
3: Dy
0.06luminescent material.
Fig. 1 is the embodiment 2 hollow structure orthophosphoric acid salt luminescent material prepared and the luminescent spectrum comparison diagram contrasted under the cathode-ray exciting of luminescent material under acceleration voltage is 1.5KV; Wherein, curve 1 is the hollow structure orthophosphoric acid salt luminescent material Ba of the hollow structure that embodiment 3 obtains
2.94gd (PO
4)
3: Dy
0.06luminescent spectrum, curve 2 is contrast luminescent material Ba
2.94gd (PO
4)
3: Dy
0.06luminescent spectrum.
As can be seen from Figure 1, at the emission peak at 581nm place, the luminous intensity of luminescent material prepared by the present embodiment enhances 21%.
Embodiment 3
The precipitator method prepare the Ba of hollow structure
2.98gd (PO
4)
3: Dy
0.02
Take 0.003g glucose and be dissolved in the sorbitol solution that dehydrated alcohol obtains 40mL, this solution being proceeded to 50mL is with in teflon-lined reactor, add a cover after screwing, in 150 DEG C of reaction 10h, prepare the solution of carbon bead template, this solution of centrifugation obtains solid formation, washs 2 times respectively with deionized water and dehydrated alcohol, and dry at 70 DEG C, namely obtain carbon bead template.
The BaO taking 30.6658g is dissolved in the Ba (NO that nitric acid obtains 100mL2mol/L
3)
2solution, takes 9.0623g Gd
2o
3be dissolved in the Gd (NO that nitric acid obtains 100mL0.5mol/L
3)
3solution and take 3.7300gDy
2o
3be dissolved in the Dy (NO that nitric acid obtains 100mL0.2mol/L
3)
3solution.
According to Ba
2.98gd (PO
4)
3: Dy
0.02stoichiometry ratio measure 5.96mL2mol/L Ba (NO
3)
2, 8mL0.5mol/L Gd (NO
3)
3with 0.4mL0.2mol/L Dy (NO
3)
3solution mixes, and obtains mixing solutions, uses HNO
3the pH regulating mixing solutions is 3, then adds carbon bead template 4.8mg, stirs 6h.Separately get (NH
4)
2hPO
4under agitation it is slowly joined mixing solutions after being dissolved in deionized water the solution making 0.5mol/L, (NH
4)
2hPO
4the add-on of solution is 30mL, is precipitated, then stirring reaction 8h.Then suction filtration is also dry, obtains Ba
2.98gd (PO
4)
3: Dy
0.02@C presoma;
Presoma is ground, is put in high temperature box furnace calcining at constant temperature 1h at 1000 DEG C, grinding after cooling, and then in 1150 DEG C of calcining 3h, obtain the Ba of hollow structure
2.98gd (PO
4)
3: Dy
0.02luminescent material.
Embodiment 4
The precipitator method prepare the Ba of hollow structure
2.9gd (PO
4)
3: Dy
0.1
Take 5g glucose and be dissolved in the sorbitol solution that dehydrated alcohol obtains 40mL, this solution being proceeded to 50mL is with in teflon-lined reactor, add a cover after screwing, in 180 DEG C of reaction 24h, prepare the solution of carbon bead template, this solution of centrifugation obtains solid formation, washs 2 times respectively with deionized water and dehydrated alcohol, and dry at 60 DEG C, namely obtain carbon bead template.
Take the BaCO of 98.6700g
3be dissolved in the Ba (NO that nitric acid obtains 100mL5mol/L
3)
2solution, takes 4.9452g Gd
2(CO
3)
3be dissolved in the Gd (NO that nitric acid obtains 100mL0.2mol/L mol/L
3)
3solution and take 2.5251g Dy
2(CO
3)
3be dissolved in the Dy (NO that nitric acid obtains 100mL0.1
3)
3solution.
According to Ba
2.9gd (PO
4)
3: Dy
0.1stoichiometry ratio measure 2.32mL5mol/L Ba (NO
3)
2, 20mL0.2mol/L Gd (NO
3)
3with 4mL0.1mol/L Dy (NO
3)
3solution mixes, and obtains mixing solutions, uses HNO
3the pH regulating mixing solutions is 1, then adds carbon bead template 1.2mg, stirs 5h.Separately get (NH
4)
2hPO
4under agitation it is slowly joined mixing solutions after being dissolved in deionized water the solution making 1mol/L, (NH
4)
2hPO
4the add-on of solution is 15mL, is precipitated, then stirring reaction 6h.Then suction filtration is also dry, obtains Ba
2.9gd (PO
4)
3: Dy
0.1@C presoma;
Presoma is ground, is put in high temperature box furnace calcining at constant temperature 1h at 800 DEG C, grinding after cooling, and then in 1200 DEG C of calcining 5h, obtain the Ba of hollow structure
2.9gd (PO
4)
3: Dy
0.1luminescent material.
Embodiment 5
The precipitator method prepare the Ba of hollow structure
2.97gd (PO
4)
3: Dy
0.03
Take 6g sucrose dissolved obtains 40mL sucrose alcohol solution in dehydrated alcohol, this solution being proceeded to 50mL is with in teflon-lined reactor, add a cover after screwing, in 200 DEG C of reaction 5h, prepare the solution of carbon bead template, this solution of centrifugation obtains solid formation, washs 2 times respectively with deionized water and dehydrated alcohol, and dry at 75 DEG C, namely obtain carbon bead template.
According to Ba
2.97gd (PO
4)
3: Dy
0.03stoichiometry ratio measure 11.88mL1mol/L Ba (NO
3)
2, 4mL1mol/L Gd (NO
3)
3with 6mL0.02mol/L Dy (NO
3)
3solution mixes, and obtains mixing solutions, uses HNO
3the pH regulating mixing solutions is 2, then adds carbon bead template 100mg, stirs 4h.Separately get (NH
4)
2hPO
4under agitation it is slowly joined mixing solutions after being dissolved in deionized water the solution making 0.5mol/L, (NH
4)
2hPO
4the add-on of solution is 30mL, is precipitated, then stirring reaction 5h.Then suction filtration is also dry, obtains Ba
2.97gd (PO
4)
3: Dy
0.03@C presoma;
Presoma is ground, is put in high temperature box furnace calcining at constant temperature 3h at 900 DEG C, grinding after cooling, and then in 1300 DEG C of calcining 1h, obtain the Ba of hollow structure
2.97gd (PO
4)
3: Dy
0.03luminescent material.
Embodiment 6
The precipitator method prepare the Ba of hollow structure
2.995gd (PO
4)
3: Dy
0.005
Take 5.705g sucrose dissolved obtains 40mL sucrose alcohol solution in dehydrated alcohol, this solution being proceeded to 50mL is with in teflon-lined reactor, add a cover after screwing, in 140 DEG C of reaction 15h, prepare the solution of carbon bead template, this solution of centrifugation obtains solid formation, washs 2 times respectively with deionized water and dehydrated alcohol, and dry at 80 DEG C, namely obtain carbon bead template.
According to Ba
2.995gd (PO
4)
3: Dy
0.005stoichiometry ratio measure 11.98mL1mol/L Ba (NO
3)
2, 2mL2mol/L Gd (NO
3)
3with 2mL0.01mol/L Dy (NO
3)
3solution mixes, and obtains mixing solutions, uses HNO
3the pH regulating mixing solutions is 1, then adds carbon bead template 150mg, stirs 3h.Separately get (NH
4)
2hPO
4under agitation it is slowly joined mixing solutions after being dissolved in deionized water the solution making 1mol/L, (NH
4)
2hPO
4the add-on of solution is 15mL, is precipitated, then stirring reaction 3h.Then suction filtration is also dry, obtains Ba
2.995gd (PO
4)
3: Dy
0.005@C presoma;
Presoma is ground, is put in high temperature box furnace calcining at constant temperature 2h at 750 DEG C, grinding after cooling, and then in 1200 DEG C of calcining 4h, obtain the Ba of hollow structure
2.995gd (PO
4)
3: Dy
0.005luminescent material.
Should be understood that, the above-mentioned statement for present pre-ferred embodiments is comparatively detailed, and therefore can not think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.
Claims (8)
1. a preparation method for hollow structure orthophosphoric acid salt luminescent material, is characterized in that, comprises the steps:
Be that the sucrose of 0.00075 ~ 0.15g/ml or the ethanolic soln of glucose are placed in reactor by concentration, at 120 ~ 200 DEG C, 5 ~ 36h is reacted after sealed reactor, be cooled to centrifugation after room temperature, and the solid phase obtained is washed, obtain carbon bead template after drying;
Be Ba according to general structure
3-xgd (PO
4)
3: Dy
xin each element chemistry metering ratio, provide the salts solution of Ba, Gd and Dy to mix respectively, obtain mixing solutions; The pH value of mixing solutions is regulated to be 1 ~ 3 subsequently; Then add carbon bead template again, stir 0.5-6h, more then slowly add (NH when stirring
4)
2hPO
4sinking agent, produces precipitation, then stirring reaction 2-8h, and then suction filtration is also dry, obtains Ba
3-xgd (PO
4)
3: Dy
x@C presoma; Wherein, described carbon bead template and Ba
3-xgd (PO
4)
3: Dy
xmol ratio be 0.025:1 ~ 10:1;
Described presoma is ground, and powder pre-burning 1 ~ 6 hour at 600 ~ 1000 DEG C will be ground, grinding after cooling, and then in 1100 ~ 1300 DEG C of calcining 1 ~ 6h, obtain Ba
3-xgd (PO
4)
3: Dy
xluminescent material;
In above-mentioned steps, the span of x is 0 < x≤0.2.
2. the preparation method of hollow structure orthophosphoric acid salt luminescent material according to claim 1, is characterized in that, the reactor in described carbon bead template preparation process is teflon-lined reactor.
3. the preparation method of hollow structure orthophosphoric acid salt luminescent material according to claim 1, is characterized in that, is use deionized water and dehydrated alcohol repetitive scrubbing successively repeatedly to the washing of the solid phase that described centrifugation obtains.
4. the preparation method of hollow structure orthophosphoric acid salt luminescent material according to claim 1, is characterized in that, carries out at 60 ~ 80 DEG C the drying of the solid phase after described washing.
5. the preparation method of hollow structure orthophosphoric acid salt luminescent material according to claim 1, is characterized in that, the salts solution of described Ba is respectively barium acetate or nitrate of baryta that concentration is 0.5 ~ 5mol/L; The salts solution of described Gd is respectively gadolinium acetate or Gadolinium trinitrate that concentration is 0.2 ~ 2mol/L; The salts solution of described Dy is respectively acetic acid dysprosium or Dysprosium trinitrate that concentration is 0.01 ~ 0.5mol/L.
6. the preparation method of hollow structure orthophosphoric acid salt luminescent material according to claim 1, is characterized in that, the relative Ba of mole dosage of described sinking agent
2+and Gd
3+mole dosage excessive 25%.
7. the preparation method of hollow structure orthophosphoric acid salt luminescent material according to claim 1, is characterized in that, pre-burning and the calcining of described grinding powder are carried out all in air atmosphere, in high temperature box furnace.
8. the preparation method of hollow structure orthophosphoric acid salt luminescent material according to claim 1, is characterized in that, the span of x is 0.02≤x≤0.1.
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| CN113024244B (en) * | 2021-03-24 | 2022-05-06 | 山东大学 | Orthophosphate thermal barrier coating material with high thermal expansion coefficient and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN102337136A (en) * | 2010-07-21 | 2012-02-01 | 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 |
| CN102477294A (en) * | 2010-11-25 | 2012-05-30 | 海洋王照明科技股份有限公司 | Calcium titanate luminescent material and preparation method thereof |
-
2013
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337136A (en) * | 2010-07-21 | 2012-02-01 | 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 |
| CN102477294A (en) * | 2010-11-25 | 2012-05-30 | 海洋王照明科技股份有限公司 | Calcium titanate luminescent material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Luminescent materials and spectroscopic properties of Dy3+ ion;Qiang Su et al;《JOURNAL OF LUMINESCENCE》;20060314;第122－123卷;第927-930页 * |
| Luminescent materials and spectroscopic properties of Dy3+ ion;Qiang Su et al;《JOURNAL OF LUMINESCENCE》;20060314;第122－123卷;第928页右栏第1-5行 * |
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