CN108893117A - A kind of the halogen-phosphate fluorescent powder and its preparation process of cerium activation - Google Patents
A kind of the halogen-phosphate fluorescent powder and its preparation process of cerium activation Download PDFInfo
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- CN108893117A CN108893117A CN201811117990.1A CN201811117990A CN108893117A CN 108893117 A CN108893117 A CN 108893117A CN 201811117990 A CN201811117990 A CN 201811117990A CN 108893117 A CN108893117 A CN 108893117A
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- fluorescent powder
- halogen
- phosphate
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- 239000000843 powder Substances 0.000 title claims abstract description 46
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 22
- 239000010452 phosphate Substances 0.000 title claims abstract description 16
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 14
- 230000004913 activation Effects 0.000 title claims abstract description 14
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000005284 excitation Effects 0.000 claims abstract description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 5
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 5
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 5
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 229910052788 barium Inorganic materials 0.000 claims abstract description 3
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 14
- 239000010431 corundum Substances 0.000 claims description 14
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 13
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 3
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910017665 NH4HF2 Inorganic materials 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 2
- KVBCYCWRDBDGBG-UHFFFAOYSA-N azane;dihydrofluoride Chemical compound [NH4+].F.[F-] KVBCYCWRDBDGBG-UHFFFAOYSA-N 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims 1
- 239000013589 supplement Substances 0.000 claims 1
- 229960000935 dehydrated alcohol Drugs 0.000 abstract description 13
- 238000001035 drying Methods 0.000 abstract description 13
- 239000003292 glue Substances 0.000 abstract description 4
- 208000017520 skin disease Diseases 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract 1
- 230000035800 maturation Effects 0.000 abstract 1
- 238000003836 solid-state method Methods 0.000 abstract 1
- 238000000295 emission spectrum Methods 0.000 description 18
- 238000000695 excitation spectrum Methods 0.000 description 13
- 238000001816 cooling Methods 0.000 description 12
- 229910052738 indium Inorganic materials 0.000 description 12
- 230000003595 spectral effect Effects 0.000 description 12
- 238000000034 method Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 150000003016 phosphoric acids Chemical class 0.000 description 2
- -1 rare earth fluoride Chemical class 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- IBIRZFNPWYRWOG-UHFFFAOYSA-N phosphane;phosphoric acid Chemical compound P.OP(O)(O)=O IBIRZFNPWYRWOG-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7777—Phosphates
- C09K11/7778—Phosphates with alkaline earth metals
- C09K11/7779—Phosphates with alkaline earth metals with halogens
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of halogen-phosphate fluorescent powders of cerium activation and its preparation process, the chemical general formula of the fluorescent powder to be：[A(1)3][A(2)1‑x][A(3)](PO4)3Z：xCe3+, wherein A (1) is at least one of Ca, Sr, Ba, and A (2) is at least one of Y, La, Gd, and A (3) is at least one of Na, Li, and at least one of Z F, Cl, x takes 0.005~0.10.It prepares the fluorescent powder and uses high temperature solid-state method, the specific steps are：According to each element stoichiometric ratio in fluorescent powder chemical formula, corresponding raw material is accurately weighed, dehydrated alcohol is added to mix, grinding uniformly, after drying, is sintered under reducing atmosphere in the agate mortar, obtains respective material through processing.Fluorescent powder of the invention has many advantages, such as wide in range optional excitation peak wavelength (250-314nm) and wide in range optional emission peak wavelength (310-365nm), and has that preparation is simple, technology maturation, prepares product efficient stable concurrently.According to different launch wavelength demands, which can be used for treating the occasions such as skin disease, UV glue curing, trap lamp and ore identification.
Description
Technical field
The present invention relates to a kind of halogen-phosphate fluorescent powders of cerium activation, and provide the preparation process of the fluorescent powder, institute
The fluorescent powder excitation wavelength of preparation is the intermediate waves ultraviolet light of 250-314nm, and launch wavelength is the middle long wave ultraviolet of 310-365nm
Light.Belong to solid luminescent material field
Background technique
With the continuous intensification that people recognize ultraviolet light, people are also more and more general for the application of different wave length ultraviolet light
Time.As short wave ultraviolet (UV-C) is often used to disinfection and sterilization；Ultraviolet B radiation (UV-B) is chiefly used in treating skin disease；Long wave is purple
Outside line (UV-A) can be used for making trap lamp, money-checking, ore identification and ink glue curing etc. then according to the difference of wavelength
Aspect.In at present in long wave ultraviolet light product, purple light fluorescent powder is coated mainly in low pressure mercury vapor lamp, is steamed using low-pressure mercury
The 253.7nm short wave ultraviolet light that gas lamp is launched excites purple light fluorescent powder, obtains the ultraviolet light of required wavelength.For a long time, purple
The research and utilization of outer fluorescent powder focus mostly in American-European western countries, and early in 1997, western countries began to study and utilize
Medium wave ultraviolet light (313nm) treats leucoderma.In recent years, the domestic research about ultraviolet fluorescence powder also increases year by year, studies
And have developed rare earth fluoride, RE borate, RE phosphate ultraviolet fluorescence powder.Traditional rare earth fluoride purple light fluorescence
Powder Ba5(PO4)3F：Pb, Gd, due to being limited its scope of application containing heavy metal lead.The research of RE borate purple light fluorescent powder
More mature, Commercial optical powder LaB3O6：Bi, Gd, launch wavelength 311nm are chiefly used in transdermal medical device, but cannot expire
The demand of sufficient other field.RE phosphate has many researchs in recent years, and relevant report includes the phosphoric acid salt for emitting visible light
Fluorescent powder and ultraviolet phosphate phosphor, phosphoric acid salt ultraviolet fluorescence powder is adaptable and few, at present with regard to Ultraluminescence
It to be also further improved in terms of powder physical property and luminous intensity.Therefore, in terms of ultraviolet fluorescence powder, it is green to develop environmental protection
The purple light fluorescent powder of color, launch wavelength multiplicity has a very important significance.
Summary of the invention
The object of the present invention is to provide the purple light transmitting fluorescent powders of launch wavelengths different (310-365nm) a series of, for not
The purple light fluorescent powder of wavelength needed for the work production of same domain provides.It also include some purple light fluorescent powders, transmitting in the present invention
Ultraviolet band there are no the fields of related application, but with the development of the subjects such as life, physics, chemistry, perhaps have and answer
Value.In addition, the present invention also provides the preparation processes of above-mentioned fluorescent powder.
The technical scheme is that：A kind of halogen-phosphate fluorescent powder of cerium activation, it is characterised in that the fluorescent powder
Chemical formula is：[A(1)3][A(2)1-x][A(3)](PO4)3Z：xCe3+, wherein A (1) is at least one of Ca, Sr, Ba, A (2)
For Y, La, Gd, at least one of, A (3) is at least one of Na, Li, at least one of Z F, Cl；X takes 0.005~
0.10。
The halogen-phosphate purple light transmitting fluorescent powder of cerium activation of the invention, excites peak wavelength between 250-314nm, hair
Spectrum peak wavelength is penetrated between 310-365nm.
In addition, the present invention provides a kind of preparation process of the halogen-phosphate purple light transmitting fluorescent powder of cerium activation, it is specific
Step is：
(1) according to chemical formula [A (1)3][A(2)1-x][A(3)](PO4)3Z：xCe3+Each element in (x takes 0.005~0.10)
Stoichiometric ratio, weighing raw material respectively is：Calcium, strontium, barium, sodium, lithium carbonate, yttrium, lanthanum, gadolinium, cerium oxide, phosphoric acid hydrogen two
Ammonium/ammonium dihydrogen phosphate, ammonium fluoride/ammonium acid fluoride and ammonium chloride；
(2) raw material is mixed, suitable alcohol is added, grinds 10min in the agate mortar, be uniformly mixed it, will grind
The raw material of milled in an oven, at 40-70 DEG C, dries 5-20h；
(3) uniformly mixed raw material is transferred in corundum crucible, crucible is placed in Muffle furnace, under reducing atmosphere, in
Calcination 2-5h at 900 DEG C -1300 DEG C；
(4) sample that sintering is obtained is ground up, sieved, and phosphor material powder can be obtained.
In the above method：Raw materials used NH4F/NH4HF2、NH4Excessive 10% (being calculated according to molar ratio) of Cl.To mend
Fill the F and Cl lost in reaction.
In the above method：The alcohol amount of addition is 1-1.5 times of total mass of raw material.
In the above method：The reducing atmosphere is CO or N2/H2Mixed gas provides, wherein H2Volume account for N2/H2
The 5%-15% of mixed gas volume.
In the above method：The sieve specification of sieving is 200-300 mesh.
Fluorescent powder produced by the present invention is the fluorescent powder of ultraviolet light emission (310-365nm), is mainly used in treating skin
Skin disease, production trap lamp, money-checking, ore identification and ink glue curing etc..The ultraviolet light emission wavelength kind of fluorescent powder
Class washability is more, and luminescent properties are good.
Beneficial effect
1, preparation process of the present invention is simple, implementation easy to operate, is convenient for mass production.
2, purple light fluorescent powder of the invention can effectively be excited by the intermediate waves ultraviolet light of 250-314nm, emission spectrum peak
It is worth wavelength between 310-365nm, can satisfy the demand in different operating field.Therefore treatment skin disease, system be can be applied to
Make trap lamp, money-checking, ore identification and ink glue curing etc..
Detailed description of the invention
Fig. 1 is the excitation and emission spectra figure that different substrates form fluorescent powder.
Fig. 2 is emission spectrum of 2,7,12 products obtained therefrom of embodiment under 253nm ultraviolet excitation.
Specific embodiment
Here is the specific preferred embodiment of the present invention provided referring to attached drawing, belongs to explanation of the invention rather than protects model
The limitation enclosed.It is all to belong to the technology and equivalency range that above content of the present invention is covered, it is to be protected to be in institute of the invention
Within the scope of.
Embodiment 1：
4.3745gBaCO is weighed respectively3, 0.8301gY2O3, 0.2730gLi2CO3, 2.9273g (NH4)2HPO4,
0.3136gNH4F, 0.0064gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1100 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 270nm, and transmitting main peak is located at 331nm.
Embodiment 2：
3.8927gBaCO is weighed respectively3, 1.1858gGd2O3, 0.3485gNa2CO3, 2.6049g (NH4)2HPO4,
0.3888gNH4Cl, 0.0057gCeO2.It is put into agate mortar, the dehydrated alcohol of 10g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1100 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 313nm, and transmitting main peak is located at 365nm.253nm
The emission spectrum of ultraviolet excitation such as Fig. 2.
Embodiment 3：
4.0364gBaCO is weighed respectively3, 1.2296gGd2O3, 0.2519gLi2CO3, 2.7011g (NH4)2HPO4,
0.2894gNH4F, 0.0059gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 60 DEG C of baking oven, 8h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1100 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 274nm, and transmitting main peak is located at 310nm.
Embodiment 4：
4.1220gBaCO is weighed respectively3, 1.1286gLa2O3, 0.2572gLi2CO3, 2.7584g (NH4)2HPO4,
0.2955gNH4F, 0.0060gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1100 DEG C, it is sintered 3h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 273nm, and transmitting main peak is located at 333nm.
Embodiment 5：
3.8215gSrCO is weighed respectively3, 0.9693gY2O3, 0.4573gNa2CO3, 3.4183g (NH4)2HPO4,
0.5102gNH4Cl, 0.0074gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1000 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 273nm, and transmitting main peak is located at 349nm.
Embodiment 6：
3.4810gSrCO is weighed respectively3, 1.4175gGd2O3, 0.4165gNa2CO3, 3.1138g (NH4)2HPO4,
0.4648gNH4Cl, 0.0068gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1000 DEG C, it is sintered 5h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 274nm, and transmitting main peak is located at 310nm.
Embodiment 7：
3.6358gSrCO is weighed respectively3, 1.4805gGd2O3, 0.3033gLi2CO3, 3.2523g (NH4)2HPO4,
0.3484gNH4F, 0.0071gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1100 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 274nm, and transmitting main peak is located at 311nm.253nm
The emission spectrum of ultraviolet excitation such as Fig. 2.
Embodiment 8：
3.7290gSrCO is weighed respectively3, 1.3647gLa2O3, 0.3111gLi2CO3, 3.3356g (NH4)2HPO4,
0.3573gNH4F, 0.0072gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1150 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 273nm, and transmitting main peak is located at 316nm.
Embodiment 9：
3.3594gCaCO is weighed respectively3, 1.2568gY2O3, 0.5929gNa2CO3, 4.4322g (NH4)2HPO4,
0.4748gNH4F, 0.0096gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1200 DEG C, it is sintered 3h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 301nm, and transmitting main peak is located at 355nm.
Embodiment 10：
2.9793gCaCO is weighed respectively3, 1.7894gGd2O3, 0.3666gLi2CO3, 3.9308g (NH4)2HPO4,
0.5867gNH4Cl, 0.0085gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1100 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 274nm, and transmitting main peak is located at 312nm.
Embodiment 11：
3.0742gCaCO is weighed respectively3, 1.6595gLa2O3, 0.5426gNa2CO3, 4.0560g (NH4)2HPO4,
0.4345gNH4F, 0.0088gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 900 DEG C, it is sintered 5h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 274nm, and transmitting main peak is located at 336nm.
Embodiment 12：
3.1608gCaCO is weighed respectively3, 1.7062gLa2O3, 0.3889gLi2CO3, 4.1702g (NH4)2HPO4,
0.4468gNH4F, 0.0091gCeO2.It is put into agate mortar, the dehydrated alcohol of 8g is added, is fully ground in the agate mortar
10min.At a temperature of 50 DEG C of baking oven, 10h is dried.The raw material of drying is ground and is sieved, the corundum crucible of 50ml is then transferred into
In, in CO reducing atmosphere, at 1100 DEG C, it is sintered 4h.After natural cooling, sieve is smashed and ground and crossed, final products can be obtained.It is right
It carries out spectral scan, excitation and emission spectra such as Fig. 1.Excitation main peak is located at 273nm, and transmitting main peak is located at 318nm.253nm
The emission spectrum of ultraviolet excitation such as Fig. 2.
Claims (7)
1. a kind of halogen-phosphate fluorescent powder of cerium activation, it is characterised in that：The chemical general formula of the fluorescent powder is：[A(1)3][A
(2)1-x][A(3)](PO4)3Z：xCe3+, wherein：A (1) is at least one of Ca, Sr, Ba, A (2) be in Y, La, Gd extremely
Few one kind, A (3) are at least one of Na, Li, and at least one of Z F, Cl, x takes 0.005~0.10.
2. a kind of halogen-phosphate fluorescent powder of cerium activation as described in claim 1, it is characterised in that：The fluorescent powder excitation
Wavelength peak is between 250-314nm, and emission peak is between 310-365nm.
3. a kind of halogen-phosphate fluorescent powder of cerium activation as described in claim 1, specific step is as follows by preparation process：
(1) according to chemical formula [A (1)3][A(2)1-x][A(3)](PO4)3Y：xCe3+Each element chemistry in (x takes 0.005~0.10)
Ratio is measured, weighing raw material respectively is：Calcium, strontium, barium, sodium, lithium carbonate, yttrium, lanthanum, gadolinium, cerium oxide, diammonium hydrogen phosphate/
Ammonium dihydrogen phosphate, ammonium fluoride/ammonium acid fluoride and ammonium chloride；
(2) raw material is mixed, suitable alcohol is added, grinds 10min in the agate mortar, be uniformly mixed it, it will be ground
Raw material in an oven, at 40-70 DEG C, dry 5-20h；
(3) uniformly mixed raw material is transferred in corundum crucible, crucible is placed in Muffle furnace, under reducing atmosphere, in 900
Calcination 2-5h at DEG C -1300 DEG C；
(4) sample that sintering is obtained is ground, sieve is sieved, and phosphor material powder can be obtained.
4. a kind of preparation process of the halogen-phosphate fluorescent powder of cerium activation as claimed in claim 3, it is characterised in that：Original used
Expect NH4F/NH4HF2、NH4Excessive 10% (being calculated according to molar ratio) of Cl.To supplement the F and Cl that lose in reaction.
5. a kind of preparation process of the halogen-phosphate fluorescent powder of cerium activation as claimed in claim 3, it is characterised in that：It is added
Alcohol amount is 1-1.5 times of total mass of raw material.
6. a kind of preparation process of the halogen-phosphate fluorescent powder of cerium activation as claimed in claim 3, it is characterised in that：Described
Reducing atmosphere is CO or N2/H2Mixed gas provides, wherein H2Volume account for N2/H2The 5%-15% of mixed gas volume.
7. a kind of preparation process of the halogen-phosphate fluorescent powder of cerium activation as claimed in claim 3, it is characterised in that：Sieving is used
Sieve specification be 200-300 mesh.
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