CN105441075A - Titanium barium pyrophosphate phosphor and preparation method thereof - Google Patents
Titanium barium pyrophosphate phosphor and preparation method thereof Download PDFInfo
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- CN105441075A CN105441075A CN201510928899.8A CN201510928899A CN105441075A CN 105441075 A CN105441075 A CN 105441075A CN 201510928899 A CN201510928899 A CN 201510928899A CN 105441075 A CN105441075 A CN 105441075A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/71—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing alkaline earth metals
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Abstract
The invention discloses titanium barium pyrophosphate phosphor and a preparation method thereof. The titanium barium pyrophosphate phosphor has a chemical composition of Ba2P2O7: nTiO2. The invention also discloses a preparation method of the titanium barium pyrophosphate phosphor. The titanium barium pyrophosphate phosphor has a broadband emission spectrum comprising all lights with half width of 170nm near by blue lights with wavelength of 490nm and has high luminescence efficiency, wide half peak width and stable chemical performances. The titanium barium pyrophosphate phosphor has adjustable granularity. Through control of deposition conditions, precursor particle sizes are changed and the finished product has particle sizes of 4-30 microns. Through combination of the titanium barium pyrophosphate phosphor, tin magnesium strontium phosphate and other phosphor, a lamp prepared from the mixed powder realizes full spectrum display.
Description
Technical field
The present invention relates to rare earth luminescent material field, in particular to a kind of barium pyrophosphate titanium fluorescent material and preparation method thereof.
Background technology
After the 1950's, luminescent lamp mostly adopts calcium halophosphate activated by antimony andmanganese, is commonly called as halogen powder.Halogen powder low price, but luminous efficiency is not high enough, poor heat stability, and light decay is comparatively large, and lux maintenance is low, and therefore, it is not suitable in slim pipe diameter compact fluorescent lamp.
1974, first Holland succeeded in developing Philip and can send the red of human eye sensitivity, green, the fluorescent material yttrium oxide of blue three color light (glows, peak wavelength is 611nm), many magnesium aluminate (green light, peak wavelength is 541nm) and many magnesium aluminates barium (blue light-emitting, peak wavelength is 450nm) be mixed into three primary colors fluorescent powder (complete name is rare earth element three primary colors fluorescent powder) by a certain percentage, its luminous efficiency is high, and (average light efficiency is at more than 80lm/W, be about 5 times of incandescent light), colour temperature is 2500K-6500K, colour rendering index is about 85, the raw material making luminescent lamp with it can save the energy greatly, the cause of Here it is efficient energy-saving fluorescent lamp.Can say, the development & application of rare earth element three primary colors fluorescent powder is an important milestone in luminescent lamp development history.There is no three primary colors fluorescent powder, just can not have today of slim pipe diameter compact high efficiency energy saving luminescent lamp of new generation.But rare earth element three primary colors fluorescent powder also has its shortcoming, its disadvantage is exactly expensive.
Barium pyrophosphate titanium by ultraviolet short wavelength discharge excite, can use in luminescent lamp.The color sent in magnesium wolframate that what it sent be similar in color.Barium pyrophosphate titanium fluorescent material is apparent is white powder, excites and issues pearl opal fluorescence, peak wavelength about 490nm, half-width 170 ± 5nm, chromaticity coordinates x=0.260 ± 0.01, y=0.335 ± 0.005 at 253.7nm ultraviolet.Strontium phosphate magnesium tin of can arranging in pairs or groups uses, and is applied to high colour developing, high quality lighting field.
Summary of the invention
An object of the present invention is to provide a kind of blue emission, luminous efficiency be high, half-peak is wide, the barium pyrophosphate titanium fluorescent material of stable chemical performance.
The technical solution adopted in the present invention is as follows:
A kind of barium pyrophosphate titanium fluorescent material, it is characterized in that, its chemical general formula is: Ba
2p
2o
7: nTiO
2, wherein: 0.1≤n≤0.9.
Another object of the present invention, is to provide a kind of preparation method of barium pyrophosphate titanium fluorescent material, comprises the following steps:
1) by chemical general formula BaHPO
4stoichiometric ratio take Ba (NO
3)
2, (NH
4)
2hPO
4, wherein (NH
4)
2hPO
4excessive 5 ~ 20%, by Ba (NO
3)
2be dissolved in pure water, controlled concentration is at 0.2 ~ 0.5mol/L, and temperature is between 35 ~ 60 DEG C; By (NH4)
2hPO
4be dissolved in pure water, controlled concentration is at 2.5 ~ 4mol/L, and temperature is between 35 ~ 60 DEG C;
2) Ba (NO will configured
3)
2solution remains on 35 ~ 60 DEG C and under being in rapid stirring state, at the uniform velocity adds step 1) in (NH of configuration
4)
2hPO
4solution, feed time is 5 ~ 60min; Keep temperature 35 ~ 60 DEG C to continue stirring 0.5 ~ 2h afterwards, after stopping stirring, keep temperature 35 ~ 60 DEG C, leave standstill 0.5 ~ 6h, be precipitated;
3) by step 2) precipitation that obtains poured out 80 ~ 250 eye mesh screens, then used pure water, will be deposited in 120 ~ 180 DEG C of drying and dewaterings, the precipitation of oven dry 80 ~ 250 eye mesh screens, obtain Ba
2p
2o
7: nTiO
2precursor B aHPO
4;
4) according to chemical formula Ba
2p
2o
7: nTiO
2stoichiometric ratio take step 3) obtained precursor B aHPO
4and TiO
2, then adding fusing assistant, obtained mixture, is placed in mixture in mixing tank, adds batch mixing ball, mix;
5) by step 4) in through mixing mixture be placed in air atmosphere, in 1000 ~ 1040 DEG C insulation 4 ~ 8h; Take out after being cooled to 25 ~ 30 DEG C, cross 20 ~ 80 eye mesh screens, add water and stir form slurry and cross 400 eye mesh screens, be washed to conductance≤50 μ s/cm;
6) toward step 5) slurry in add pure water and nano aluminium oxide coating, 5% ammoniacal liquor and 5% hydrochloric acid is used to regulate PH to 9.0 ~ 9.3, stir 0.5 ~ 3h, stir disposed slurry and cross 250 eye mesh screens, washing conductance≤50 μ s/cm, at 120 ~ 180 DEG C of drying and dewaterings, cross 160 eye mesh screens and namely obtain a kind of barium pyrophosphate titanium fluorescent material.
Further, described precursor B aHPO
4final washing conductance≤100 μ s/cm.
Further, step 2) described in fusing assistant be BaF
2, weight percent is 0.5 ~ 2.5%.
Further, step 2) described in the granularity of TiO2 be 20 ~ 100nm.
Further, step 6) described in nano aluminium oxide coating be the nano-alumina solution of 1 ~ 2%wt.
Further, step 6) described in nano aluminium oxide coating and the weight ratio of powder be 1 ~ 6:20.
Nano aluminium oxide coating refers to the nano-alumina solution adding certain concentration a certain amount of in the fluorescent powder paste material stirred; the particle diameter of fluorescent material is in micron level; the particle diameter of nano aluminium oxide at Nano grade very solution absorbs at fluorescent powder grain on the surface; form layer protective layer; also protective membrane is; this technique is also coating process; employ nano aluminium oxide and carry out coating; just be nano aluminium oxide coating process, other material such as nano yttrium oxide or nano silicon can be selected as required to carry out coating during coating also passable.Coating is large to some light decays, the fluorescent material of poor chemical stability, the effect of stability property can be played, improve the agglomeration of fluorescent material simultaneously, the dispersiveness of fluorescent material is improved, improve the loose density of fluorescent material, also be improved the coating property of fluorescent material when being coated with pipe, but the add-on of nano aluminium oxide can not be too many, no person can reduce the brightness of fluorescent material.For improving the covered effect of nano aluminium oxide, generally can regulate PH when coating, regulating the object of PH to be current potential in order to regulator solution, make the band of the phosphor surface nuclear energy that powers on enough better adsorb nano aluminium oxide.Coating takes the fluorescent material finished product furnishing slurry that again adds water to carry out coating, also can wash qualified preparations of conductance at fluorescent material and dry and put in storage, but the furnishing slurry that directly adds water when also not drying carries out coating, can save one stoving process like this.The coating agent that " nano aluminium oxide coating " technique uses is certain mass percentage concentration " nano-alumina solution ".
The present invention has following beneficial effect:
(1) emmission spectrum of fluorescent material of the present invention is broadband emission, and scope contains all light of half-breadth 170nm near 490nm wavelength blue light;
(2) phosphor emission blue light of the present invention, luminous efficiency is high, half-peak is wide, stable chemical performance;
(3) MODEL OF THE PHOSPHOR PARTICLE SIZE of the present invention is adjustable, changes the size of presoma by controlling deposition condition, and the particle diameter of final finished can 4 μm ~ 30 μm interval adjustment;
(4) fluorescent material of the present invention coordinates strontium phosphate magnesium tin and other fluorescent material to use, and can reach the display of full spectrum after the powder mix lamp made.
Accompanying drawing explanation
Fig. 1 is fluorescent material product embodiments 1 (Ba of the present invention
2p
2o
7: 0.8TiO
2) utilizing emitted light spectrogram;
Fig. 2 is scanning electronic microscope (SEM) photo of the embodiment of the present invention 1.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment 1
1) by chemical general formula BaHPO
4stoichiometric ratio take Ba (NO
3)
2, (NH
4)
2hPO
4, wherein (NH
4)
2hPO
4excessive 5%.Ba (NO
3)
2be dissolved in pure water, controlled concentration is at 0.25mol/L, and temperature is at 40 DEG C.(NH4)
2hPO
4be dissolved in pure water, controlled concentration is at 3.5mol/L, and temperature is at 40 DEG C.0.25mol/LBa (NO
3)
2solution keeps temperature 40 DEG C and under rapid stirring state, adds temperature at the (NH of 40 DEG C of concentration at 3.5mol/L
4)
2hPO
4solution, at the uniform velocity adds solution, feed time 10 minutes.Add (NH
4)
2hPO
4solution, keeps temperature 40 DEG C to continue to stir 1h, after stopping stirring, keeps temperature 40 DEG C that precipitation is left standstill 4h.Precipitation was poured out 160 eye mesh screens, with pure water to conductance≤100 μ s/cm, by precipitation dehydration 180 DEG C of oven dry, the precipitation of oven dry 250 eye mesh screens, obtain Ba
2p
2o
7: 0.8TiO
2precursor B aHPO
4;
2) according to chemical formula Ba
2p
2o
7: 0.8TiO
2stoichiometric ratio take step 1) the precursor B aHPO for preparing
4and TiO
2, TiO
2particle diameter is 20nm; Add the BaF of 0.5% parts by weight again
2, obtained mixture, is placed in mixture in mixing tank, adds batch mixing ball, mix;
3) by step 2) in through mixing mixture be placed in air atmosphere, in 1010 DEG C insulation 9h; Take out after being cooled to 28 DEG C, cross 60 eye mesh screens, add water and stir form slurry and cross 400 eye mesh screens, be washed to conductance≤50 μ s/cm.In the ratio of 1% nano-alumina solution of 1000g powder (after dry weight), 6L pure water, 50ml, pure water and 1% nano-alumina solution is added in the slurry of washing conductance≤50 μ s/cm, 5% ammoniacal liquor and 5% hydrochloric acid is used to regulate PH=9.2, stir 3h, stir disposed slurry and cross 250 eye mesh screens, washing conductance≤50 μ s/cm, dewaters 120 DEG C of oven dry, crosses 160 eye mesh screens and namely obtains barium pyrophosphate titanium fluorescent material.
Embodiment 2
1) by chemical general formula BaHPO
4stoichiometric ratio take Ba (NO
3)
2, (NH
4)
2hPO
4, wherein (NH
4)
2hPO
4excessive 5%.Ba (NO
3)
2be dissolved in pure water, controlled concentration is at 0.25mol/L, and temperature is at 45 DEG C.(NH
4)
2hPO
4be dissolved in pure water, controlled concentration is at 3.5mol/L, and temperature is at 42 DEG C.0.25mol/LBa (NO
3)
2solution keeps temperature 40 DEG C and under rapid stirring state, adds temperature at the (NH of 40 DEG C of concentration at 3.5mol/L
4)
2hPO
4solution, at the uniform velocity adds solution, feed time 8 minutes.Add (NH
4)
2hPO
4solution, keeps temperature 40 DEG C to continue to stir 1h, after stopping stirring, keeps temperature 40 DEG C that precipitation is left standstill 5h.Precipitation was poured out 160 eye mesh screens, with pure water to conductance≤50 μ s/cm, by precipitation dehydration 170 DEG C of oven dry, the precipitation of oven dry 250 eye mesh screens, obtain Ba
2p
2o
7: 0.8TiO
2precursor B aHPO
4;
2) according to chemical formula Ba
2p
2o
7: 0.8TiO
2stoichiometric ratio take step 1) the precursor B aHPO for preparing
4and TiO
2, TiO
2particle diameter is 20nm; Add the BaF of 0.5% parts by weight again
2, obtained mixture, is placed in mixture in mixing tank, adds batch mixing ball, mix;
3) by step 2) in through mixing mixture be placed in air atmosphere, in 1010 DEG C insulation 9h; Take out after being cooled to 26 DEG C, cross 60 eye mesh screens, add water and stir form slurry and cross 400 eye mesh screens, be washed to conductance≤50 μ s/cm.In the ratio of 1% nano-alumina solution of 1000g powder (after dry weight), 6L pure water, 50ml, pure water and 1% nano-alumina solution is added in the slurry of washing conductance≤50 μ s/cm, 5% ammoniacal liquor and 5% hydrochloric acid is used to regulate PH=9.2, stir 3h, stir disposed slurry and cross 250 eye mesh screens, washing conductance≤50 μ s/cm, dewaters 120 DEG C of oven dry, crosses 160 eye mesh screens and namely obtains barium pyrophosphate titanium fluorescent material.
Claims (7)
1. a barium pyrophosphate titanium fluorescent material, is characterized in that, its chemical general formula is: Ba
2p
2o
7: nTiO
2, wherein: 0.1≤n≤0.9.
2. a preparation method for barium pyrophosphate titanium fluorescent material according to claim 1, is characterized in that, comprise the following steps:
1) by chemical general formula BaHPO
4stoichiometric ratio take Ba (NO
3)
2, (NH
4)
2hPO
4, wherein (NH
4)
2hPO
4excessive 5 ~ 20%, by Ba (NO
3)
2be dissolved in pure water, controlled concentration is at 0.2 ~ 0.5mol/L, and temperature is between 35 ~ 60 DEG C; By (NH
4)
2hPO
4be dissolved in pure water, controlled concentration is at 2.5 ~ 4mol/L, and temperature is between 35 ~ 60 DEG C;
2) Ba (NO will configured
3)
2solution remains on 35 ~ 60 DEG C and under being in rapid stirring state, at the uniform velocity adds step 1) in (NH of configuration
4)
2hPO
4solution, feed time is 5 ~ 60min; Keep temperature 35 ~ 60 DEG C to continue stirring 0.5 ~ 2h afterwards, after stopping stirring, keep temperature 35 ~ 60 DEG C, leave standstill 0.5 ~ 6h, be precipitated;
3) by step 2) precipitation that obtains poured out 80 ~ 250 eye mesh screens, then used pure water, will be deposited in 120 ~ 180 DEG C of drying and dewaterings, the precipitation of oven dry 80 ~ 250 eye mesh screens, obtain Ba
2p
2o
7: nTiO
2precursor B aHPO
4;
4) according to chemical formula Ba
2p
2o
7: nTiO
2stoichiometric ratio take step 3) obtained precursor B aHPO
4and TiO
2, then adding fusing assistant, obtained mixture, is placed in mixture in mixing tank, adds batch mixing ball, mix;
5) by step 4) in through mixing mixture be placed in air atmosphere, after being warming up to 1000 ~ 1040 DEG C be incubated 4 ~ 8h; Take out after being cooled to 25 ~ 30 DEG C, cross 20 ~ 80 eye mesh screens, add water and stir form slurry and cross 400 eye mesh screens, be washed to conductance≤50 μ s/cm;
6) toward step 5) slurry in add pure water and nano aluminium oxide coating, 5% ammoniacal liquor and 5% hydrochloric acid is used to regulate PH to 9.0 ~ 9.3, stir 0.5 ~ 3h, stir disposed slurry and cross 250 eye mesh screens, washing conductance≤50 μ s/cm, at 120 ~ 180 DEG C of drying and dewaterings, cross 160 eye mesh screens and namely obtain a kind of barium pyrophosphate titanium fluorescent material.
3. the preparation method of barium pyrophosphate titanium fluorescent material according to claim 2, is characterized in that, step 3) described in precursor B aHPO
4final washing conductance≤100 μ s/cm.
4. the preparation method of barium pyrophosphate titanium fluorescent material according to claim 2, is characterized in that, step 2) described in fusing assistant be BaF
2, weight percent is 0.5 ~ 2.5%.
5. the preparation method of barium pyrophosphate titanium fluorescent material according to claim 2, is characterized in that, step 2) described in the granularity of TiO2 be 20 ~ 100nm.
6. the preparation method of barium pyrophosphate titanium fluorescent material according to claim 2, is characterized in that, step 6) described in nano aluminium oxide coating be the nano-alumina solution of 1 ~ 2%wt.
7. the preparation method of barium pyrophosphate titanium fluorescent material according to claim 2, is characterized in that, step 6) described in nano aluminium oxide coating and the weight ratio of powder be 1 ~ 6:20.
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Citations (7)
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|---|---|---|---|---|
| US2596509A (en) * | 1950-07-17 | 1952-05-13 | Thorn Electrical Ind Ltd | Titanium activated barium pyrophosphate phosphor |
| US3067145A (en) * | 1960-10-25 | 1962-12-04 | Sylvania Electric Prod | Process for preparation of titanium activated barium pyrophosphate phosphor |
| JPS54144082A (en) * | 1978-04-28 | 1979-11-09 | Toshiba Corp | Fluorescent lamp |
| JPH02173182A (en) * | 1988-12-27 | 1990-07-04 | Nichia Chem Ind Ltd | Fluorescent lamp emitting light of pink color |
| CN101440284A (en) * | 2008-12-18 | 2009-05-27 | 江门市科恒实业股份有限公司 | Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof |
| CN102327784A (en) * | 2011-07-29 | 2012-01-25 | 中国科学院宁波材料技术与工程研究所 | Phosphate material for efficiently and selectively removing lead ions and application thereof |
| CN104818018A (en) * | 2015-03-18 | 2015-08-05 | 江门市科恒实业股份有限公司 | Coprecipitation preparation method for pyrophosphate phosphor containing alkali earth metal, and phosphor and application thereof |
-
2015
- 2015-12-14 CN CN201510928899.8A patent/CN105441075B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2596509A (en) * | 1950-07-17 | 1952-05-13 | Thorn Electrical Ind Ltd | Titanium activated barium pyrophosphate phosphor |
| US3067145A (en) * | 1960-10-25 | 1962-12-04 | Sylvania Electric Prod | Process for preparation of titanium activated barium pyrophosphate phosphor |
| JPS54144082A (en) * | 1978-04-28 | 1979-11-09 | Toshiba Corp | Fluorescent lamp |
| JPH02173182A (en) * | 1988-12-27 | 1990-07-04 | Nichia Chem Ind Ltd | Fluorescent lamp emitting light of pink color |
| CN101440284A (en) * | 2008-12-18 | 2009-05-27 | 江门市科恒实业股份有限公司 | Europium activated phosphates purple light transmitting fluorescent powder and preparation thereof |
| CN102327784A (en) * | 2011-07-29 | 2012-01-25 | 中国科学院宁波材料技术与工程研究所 | Phosphate material for efficiently and selectively removing lead ions and application thereof |
| CN104818018A (en) * | 2015-03-18 | 2015-08-05 | 江门市科恒实业股份有限公司 | Coprecipitation preparation method for pyrophosphate phosphor containing alkali earth metal, and phosphor and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| D. E. HARRISON: "The System BaO-TiO2-P2O5: Phase Relations, Fluorescence, and Phosphor Preparation", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 * |
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Inventor after: Ding Xuemei Inventor after: Chen Wei Inventor after: Shi Rongrui Inventor after: Wan Guojiang Inventor before: Zhong Hua Inventor before: Lin Jiale Inventor before: Liu Zongmiao Inventor before: Ding Xuemei Inventor before: Wan Guojiang Inventor before: Shi Rongrui |
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