CN1766033A - Aluminate base long persistence phosphor powder preparation method - Google Patents
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 title claims description 21
- 150000004645 aluminates Chemical class 0.000 title claims description 12
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 230000002688 persistence Effects 0.000 title description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 31
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 20
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004327 boric acid Substances 0.000 claims abstract description 10
- 229910001940 europium oxide Inorganic materials 0.000 claims abstract description 10
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910003440 dysprosium oxide Inorganic materials 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 9
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 9
- 239000004571 lime Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims 1
- 230000005923 long-lasting effect Effects 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 13
- 239000000126 substance Substances 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000012190 activator Substances 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 238000000295 emission spectrum Methods 0.000 description 6
- 238000000695 excitation spectrum Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229910052984 zinc sulfide Inorganic materials 0.000 description 5
- 229910003668 SrAl Inorganic materials 0.000 description 4
- 239000005084 Strontium aluminate Substances 0.000 description 4
- 239000005083 Zinc sulfide Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 4
- 229910052693 Europium Inorganic materials 0.000 description 3
- IOGARICUVYSYGI-UHFFFAOYSA-K azanium (4-oxo-1,3,2-dioxalumetan-2-yl) carbonate Chemical compound [NH4+].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O IOGARICUVYSYGI-UHFFFAOYSA-K 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 2
- -1 strontium europium dysprosium aluminate Chemical class 0.000 description 2
- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004320 controlled atmosphere Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(III) nitrate Inorganic materials [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The preparation method for aluminate-base long-persistence phosphor comprises: weighting aluminum hydroxide, strontium nitrate, europium oxide, dysprosium oxide, and boric acid as stoichiometry to mix with alcohol; baking in reducing atmosphere; wherein, selecting aluminum hydroxide from activated clear industrial sodium aluminate liquid. This invention cuts and simplifies process, saves energy consumption.
Description
Technical Field
A preparation method of aluminate-based long-afterglow phosphor powder, relating to a preparation method of a photoluminescent material.
Background
The aluminate-based long-afterglow phosphor is a new photoluminescent material, and has the advantages of high luminous efficiency, long afterglow time, good chemical stability, no radioactive damage, good ageing resistance, high product added value and the like compared with sulfide materials because of the common attention on excellent long-afterglow characteristics. However, the requirements of the phosphor powder on the raw materials are very strict, and particularly, the aluminum oxide raw material for preparing the phosphor powder has a large influence on the performance of the phosphor powder. In general, analytically pure alumina is often used to produce aluminate-based phosphors, sometimes requiring further processing.
At present, some documents report about the preparation technology of aluminate-based long afterglow materials.
In SrAl2O4:Eu2+，Dy3+In the synthesis and characterization of long afterglow photoluminescent material by solid phase reaction (Zhang Xiyan, Bai dynasty, et al, rare metal materials and engineering, Vol.32, No. 5, 5 months 2003), a method is introduced, which uses SrCO as raw material3(99.2％)，Al2O3(99.99%) according to the formula, adding proper quantity of fluxing agent H3BO3And analytically pure Eu2O3、Dy2O3Mixing well, and adding Al to accelerate reaction2O3Ground to the appropriate particle size. And (3) sintering the mixture in a reducing atmosphere at 1300 ℃ for 2h, crushing the mixture, and sieving the crushed mixture with a sieve with the aperture of 76 mu m to obtain a luminescent material sample.
A high-temperature solid-phase reaction method is introduced in the research on strontium europium dysprosium aluminate long afterglow materials (Liuji, Shizheng, university of Hebei (Nature science edition), Vol 21, No. 4, 12 months 2001). The preparation method of the long afterglow material is characterized in that on one hand, oxides and salts of raw materials are required to react to generate a salt matrix, on the other hand, a rare earth activator is required to enter the matrix and be positioned in gaps of matrix lattices or replace lattice atoms, so that non-luminous materials are changed into luminous materials, the process needs higher temperature, and a high temperature solid phase reaction method is usually adopted, wherein the high temperature solid phase reaction method is a method for mixing solid raw materials according to the specific mass ratio, burning the mixed raw materials for preset time and temperature in a controlled atmosphere, crushing sintered substances and screening to obtain the long afterglow material. The purity requirement of raw materials is as follows: the harmful impurities can obviously reduce the luminescence property, so the matrix raw material of the fluorescent powder needs to be specially treated, SrCO3，Al2O3，H3BO3Required to achieve analytically pure, Eu2O3，Dy2O399.99-99.999%.
In "rare earth doped xSrO. yAl2O3Long persistence luminescent materialsIn the preparation of (1) and the optical Properties of (Linyuanhua, Zhang Zhongtai, et al, functional materials 2001, 32(3)), xSrO. yAl is introduced2O3A method for preparing Eu, Dy series photoluminescent material. It is based on the chemical formula xSrO. yAl2O3Eu, Dy, and SrCO3，Eu(NO3)3And Dy (NO)3)3The raw materials (reagents are all analytically pure) are proportioned and doped with a small amount of alcohol. Ball milling for 10 hr in ball mill, taking out, drying at 100 deg.C for 5 hr, and subjecting the mixed powder to weak reducing atmosphere (1.5% H)2～98.5％N2) Roasting to obtain the productxSrO·yAl2O3Eu, Dy series luminescent material.
In the preparation and application of rare earth aluminate blue phosphor precursor (Yi Shen, Zhou Xue Zhen, China rare earth academic newspaper, volume 20, No. 6, 12 months 2002), it is pointed out that the precursor alumina used for preparing the phosphor should have fine and solid particles, uniform distribution, small surface area and good crystallinity. The aluminum oxide prepared by the aluminum ammonium sulfate pyrolysis method has fine particles, but has large specific surface, and the effect of directly firing the fluorescent powder is not ideal. Preparing fine particle precursor Al with good crystallinity by first preparing crystalline ammonium aluminum carbonate and then utilizing pyrolysis of the ammonium aluminum carbonate2O3. The method uses analytically pure NH4Al(SO4)2·24H2O and refined NH4HCO3Respectively preparing deionized water into solutions for later use. Slowly adding NH while heating in water bath at 50 deg.C and stirring4Al(SO4)2·24H2The O solution is added dropwise to NH to which the mixed surfactant is added in advance4HCO3In the solution, aging for 12h after reaction, filtering, repeatedly washing for 5 times by deionized water, drying in a drying oven to prepare precursor ammonium aluminum carbonate, and firing at a certain temperature to obtain Al2O3。
The prior art has the disadvantages of complicated process, long preparation time and difficult industrial popularization and application.
Disclosure of Invention
The invention aims to provide a method for preparing aluminate-based long-afterglow phosphor powder, which can overcome the defects of the prior art, effectively simplify the process, shorten the preparation time, and is easy to popularize and apply in industry, and the synthesized phosphor powder has high luminous brightness and long afterglow time.
The purpose of the invention is realized by the following technical scheme.
A process for preparing aluminate-base long-afterglow phosphorescent powder includes such steps as proportionally weighing the raw materials of aluminium hydroxide, strontium nitrate, europium oxide, dysprosium oxide and boric acid, mixing them with alcohol, and calcining in reducing atmosphere.
The preparation method of the aluminate-based long-afterglow phosphorescent powder is characterized in that the purification treatment of the industrial sodium aluminate solution is to add 10-30 g/l of lime into the solution, stir and react for 1-2 h at the temperature of 85-95 ℃, separate and filter to obtain the refined industrial sodium aluminate solution.
A process for preparing the long-afterglow phosphorescent powder based on aluminate features that the Na contained in sodium aluminate solution is used as the activating agent2And (3) adding nitric acid or hydrochloric acid into the purified sodium aluminate solution to obtain colloidal aluminum hydroxide according to the theoretical amount of acid required by all reactions, and filtering and drying to prepare high-activity aluminum hydroxide.
The method of the invention prepares the aluminum hydroxide for the phosphor powder by adopting the industrial sodium aluminate solution, and then synthesizes the phosphor powder, omits the process of roasting the aluminum hydroxide into the aluminum oxide, is linked with the production flow of the industrial aluminum oxide, effectively simplifies the process, saves energy, reduces consumption and is easy to popularize and apply in industry. Because the aluminum hydroxideproduced by the method has good activity, the synthesized phosphor powder has high luminous brightness and long afterglow time.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention.
FIG. 2 shows the excitation and emission spectra of yellow-green light of example 1;
(a) is SrAl2O4:Eu2+，RE3+The excitation spectrum of (1);
(b) is SrAl2O4:Eu2+，RE3+The emission spectrum of (a).
FIG. 3 shows Sr in example 24Al14O25:Eu2+，RE3+Excitation and emission spectra of (a);
(a) is Sr4Al14O25:Eu2+，RE3+The excitation spectrum of (1);
(b) is Sr4Ali4O25:Eu2+，RE3+The emission spectrum of (a).
FIG. 4 shows Sr in example 35Al2O7S:Eu2+Excitation and emission spectra of (a);
(a) is Sr5Al2O7S:Eu2+The excitation spectrum of (1);
(b) is Sr5Al2O7S:Eu2+The emission spectrum of (a).
Detailed Description
A preparation method of aluminate-based long afterglow phosphorescent powder comprises the steps of firstly adding 10-30 g/l of lime into an industrial sodium aluminate solution, controlling thestirring speed to be 30-60 r/min at the temperature of 85-95 ℃, stirring for reaction for 1-2 h, filtering and purifying; adding nitric acid or hydrochloric acid into the purified sodium aluminate solution to obtain active aluminum hydroxide colloidal substance, wherein the addition amount of nitric acid or hydrochloric acid is determined according to Na in the solution2The O concentration was calculated and added.
The amount of nitric acid or hydrochloric acid added is calculated based on the composition of the solution, due to Na in the solution2O is divided into two parts, one part is Al2O3Bound Na2O, the other part being free Na2O, when nitric acid or hydrochloric acid is added to the solution, the following reaction occurs.
Reaction with addition of hydrochloric acid:
therefore, the amount of nitric acid or hydrochloric acid added is determined according to Na in the solution2And (4) calculating the concentration of O.
Due to Al (OH)3Has an amphoteric nature, so that when a slight excess of acid is added, Al (OH)3Is easy to change into Al3+Go into solution, so calculate HNO3Or the amount of HCl added must be precise and must not be added in excess.
And finally, weighing the active aluminum hydroxide colloidal substance and raw materials such as strontium nitrate, europium oxide, dysprosium oxide, boric acid and the like according to a nominal component stoichiometric ratio, uniformly mixing the active aluminum hydroxide colloidal substance and the raw materials with alcohol, and roasting the mixture for 2-8 hours at the temperature of 1100-1400 ℃ in a reducing atmosphere to obtain the red, green and blue tricolor phosphor powder with good color purity and high luminous brightness.
Example 1
Adding 15g/l lime into industrial sodium aluminate solution, stirring and reacting for 1h at 85 ℃, filtering, and purifying to obtain sodium aluminate solution with the component of NT：150g/l、AO130g/l、Nk125g/l、SiO20.1 g/l; adding 254 g/l nitric acid into the refined sodium aluminate solution to obtain active aluminum hydroxide colloidal substance, filtering, and oven drying. Activated aluminium hydroxide, strontium nitrate, europium oxide, dysprosium oxide, boric acid and the like are used as raw materials, and a small amount of alcohol is added into the raw materials to be uniformly mixed. When the molar ratio of Sr to Al is 1: 2, the fluxing agent H3BO3The addition amount of the Eu activator is 9 percent of the total amount of the matrix2O3And sensitizer Dy2O3The addition amount is 3 percent (mol ratio) of the total amount of the matrix, the roasting temperature is 1300 ℃, the roasting time is 4 hours and the yellow-green SrAl can be obtained under the reducing atmosphere condition2O4:Eu2+，Dy3+The luminous intensity is high, the afterglow time is long, and the afterglow time is beyond the test range of the fluorescence spectrophotometer.
Example 2
Adding 10g/l lime into industrial sodium aluminate solution, reacting at 90 deg.C for 2 hr, filtering, and purifying to obtain sodium aluminate solution with N as componentT：125(g/l)、AO109(g/l)、Nk106(g/l)、SiO20.12 (g/l); adding 215 g/l nitric acid into the refined sodium aluminate solution to prepare an active aluminum hydroxide colloidal substance, filtering and drying. Activated aluminium hydroxide, strontium nitrate, europium oxide, dysprosium oxide, boric acid and the like are used as raw materials, and a small amount of alcohol is added into the raw materials to be uniformly mixed. When the raw material ratio of Sr to Al (mol ratio) is 4: 14, the fluxing agent H3BO3The addition amount of the Eu activator is 9 percent of the total amount of the matrix2O3And sensitizer Dy2O3The addition amount is 3 percent (mol ratio) of the total amount of the matrix, the roasting temperature is 1300 ℃, the roasting time is 4 hours and the blue-green Sr can be obtained under the reducing atmosphere condition4Al14O25:Eu2+，Dy3+The luminous intensity is high, the afterglow time is long, and the afterglow time is beyond the test range of the fluorescence spectrophotometer.
Example 3
Adding 20g/l lime into industrial sodium aluminate solution, reacting at 85 deg.C for 2 hr, filtering, and purifying to obtain sodium aluminate solution with N as componentT：130(g/l)、AO105(g/l)、Nk107(g/l)、SiO20.03 (g/l); adding 217 g/l nitric acid into the refined sodium aluminate solution to obtain active aluminum hydroxide colloidal substance, filtering, and oven drying. Activated aluminum hydroxide, strontium nitrate, europium oxide, zinc sulfide, boric acid and the like are used as raw materials, and a small amount of alcohol is added to be mixed uniformly. When the raw material ratio of Sr to Al (mol ratio) is 1: 0.4, Sr to ZnS (mol ratio) is 1: 0.2, fluxing agent H3BO3The addition amount of the Eu activator is 9 percent of the total amount of the matrix2O3The red Sr can be obtained under the conditions that the addition amount is 6 percent (mol ratio) of the total amount of the matrix, the roasting temperature is 1200 ℃ and the roasting time is 8 hours5Al2O7S:Eu2+A luminous body with high luminous intensity and long afterglow.
Example 4
Adding 30g/l lime into industrial sodium aluminate solution, reacting at 95 deg.C for 1 hr, filtering, and purifying to obtain sodium aluminate solution with N as componentT：130(g/l)、AO105(g/l)、Nk110(g/l)、SiO20.03 (g/l); adding 129(g/l) hydrochloric acid into the refined sodium aluminate solution to prepare an active aluminum hydroxide colloidal substance, filtering and drying. Activated aluminum hydroxide, strontium nitrate, europium oxide, zinc sulfide, boric acid and the like are used as raw materials, and a small amount of alcohol is added to be mixed uniformly. When the raw materials are mixed in a molar ratio of Sr to Al1: 2, fluxing agent H3BO3The addition amount of the Eu activator is 9 percent of the total amount of the matrix2O3And sensitizer Dy2O3The addition amount is 3 percent (mol ratio) of the total amount of the matrix, the roasting temperature is 1300 ℃, the roasting time is 4 hours and the yellow-green SrAl can be obtained under the reducing atmosphere condition2O4:Eu2+，Dy3+The luminous intensity is high, the afterglow time is long, and the afterglow time is beyond the test range of the fluorescence spectrophotometer.
Example 5
Adding 25g/l lime into industrial sodium aluminate solution, reacting at 95 deg.C for 2 hr, filtering, and purifying to obtain sodium aluminate solution with N as componentT：130(g/l)、AO105(g/l)、Nk120(g/l)、SiO20.03 (g/l); adding 141 g/l hydrochloric acid into the refined sodium aluminate solution to obtain active aluminum hydroxide colloidal substance, filtering, and oven drying. Activated aluminum hydroxide, strontium nitrate, europium oxide, zinc sulfide, boric acid and the like are used as raw materials, and a small amount of alcohol is added to be mixed uniformly. When the raw material ratio of Sr to Al (molar ratio) is 1: 2, the fluxing agent H3BO3The addition amount of the Eu activator is 9 percent of the total amount of the matrix2O3And sensitizer Dy2O3The addition amount is 3 percent (mol ratio) of the total amount of the matrix, the roasting temperature is 1300 ℃, the roasting time is 4 hours and the yellow-green SrAl can be obtained under the reducing atmosphere condition2O4:Eu2+，Dy3+The luminous intensity is high, the afterglow time is long, and the afterglow time is beyond the test range of the fluorescence spectrophotometer.
Example 6
In industrial sodium aluminate solutionAdding 18g/l lime, reacting at 90 deg.C for 1 hr, filtering, and purifying to obtain sodium aluminate solution containing NT：130(g/l)、AO105(g/l)、Nk115(g/l)、SiO20.03 (g/l); adding 135 g/l hydrochloric acid into the refined sodium aluminate solution to prepare an active aluminum hydroxide colloidal substance, filtering and drying. Activated aluminum hydroxide, strontium nitrate, europium oxide, zinc sulfide, boric acid and the like are used as raw materials, and a small amount of alcohol is added to be mixed uniformly. When the raw material ratio of Sr to Al (molar ratio) is 1: 2, the fluxing agent H3BO3The addition amount of the Eu activator is 9 percent of the total amount of the matrix2O3And sensitizer Dy2O3The addition amount is 3 percent (mol ratio) of the total amount of the matrix, the roasting temperature is 1300 ℃, the roasting time is 4 hours and the yellow-green SrAl can be obtained under the reducing atmosphere condition2O4:Eu2+，Dy3+The luminous intensity is high, the afterglow time is long, and the afterglow time is beyond the test range of the fluorescence spectrophotometer.
Claims (3)
1. A process for preparing aluminate-base long-afterglow phosphorescent powder includes such steps as proportionally weighing the raw materials of aluminium hydroxide, strontium nitrate, europium oxide, dysprosium oxide and boric acid, mixing them with alcohol, and calcining in reducing atmosphere.
2. The method for preparing aluminate-based long-afterglow phosphorescent powder according to claim 1, wherein the purification treatment of the industrial sodium aluminate solution is to add 10-30 g/l lime into the solution, stir and react for 1-2 h at 85-95 ℃, separate and filter to obtain the refined industrial sodium aluminate solution.
3. The method for preparing aluminate-based long-lasting phosphor powder according to claim 1, wherein the activation treatment of the sodium aluminate solution is carried out according to Na in the sodium aluminate solution2Adding nitric acid into the purified sodium aluminate solution according to the theoretical amount of acid required by the complete reaction of OOr preparing colloidal aluminum hydroxide from hydrochloric acid, and preparing the high-activity aluminum hydroxide by filtering and drying.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038778A (en) * | 2009-03-20 | 2015-11-11 | 贝科斯基公司 | Alumina, luminophores and mixed compounds, and associated production methods |
| CN111635757A (en) * | 2020-06-03 | 2020-09-08 | 重庆交通大学 | Preparation method of yellow-green long-afterglow fluorescent material and application of ammonium bicarbonate |
| CN112430359A (en) * | 2020-10-27 | 2021-03-02 | 南京弘毅伯泰数字技术有限公司 | Formulation of phosphor sheet for medicine bottle and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5770111A (en) * | 1995-04-14 | 1998-06-23 | Kabushiki Kaisha Tokyo Kagaku Kenkyusho | Phosphor with afterglow characteristic |
| CN1206314C (en) * | 2003-04-11 | 2005-06-15 | 唐敏 | Acumulating self-luminescence material with long afterglow and its preparing method |
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2005
- 2005-09-09 CN CNB2005101024108A patent/CN100338174C/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038778A (en) * | 2009-03-20 | 2015-11-11 | 贝科斯基公司 | Alumina, luminophores and mixed compounds, and associated production methods |
| CN105038778B (en) * | 2009-03-20 | 2018-07-17 | 贝科斯基公司 | Aluminium oxide, illuminator and mixing blend and relative manufacturing process |
| CN111635757A (en) * | 2020-06-03 | 2020-09-08 | 重庆交通大学 | Preparation method of yellow-green long-afterglow fluorescent material and application of ammonium bicarbonate |
| CN111635757B (en) * | 2020-06-03 | 2022-11-01 | 重庆交通大学 | Preparation method of yellow-green long afterglow fluorescent material and application of ammonium bicarbonate |
| CN112430359A (en) * | 2020-10-27 | 2021-03-02 | 南京弘毅伯泰数字技术有限公司 | Formulation of phosphor sheet for medicine bottle and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100338174C (en) | 2007-09-19 |
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