CN111826156A - BaSi prepared by solution combustion method2O5Method for storing fluorescent powder by base light - Google Patents
BaSi prepared by solution combustion method2O5Method for storing fluorescent powder by base light Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 32
- 229910016066 BaSi Inorganic materials 0.000 title claims abstract description 10
- 238000002485 combustion reaction Methods 0.000 title description 2
- 238000003860 storage Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 17
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- 238000009841 combustion method Methods 0.000 claims abstract description 10
- 229910016064 BaSi2 Inorganic materials 0.000 claims abstract description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000446 fuel Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract 4
- 239000000243 solution Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 230000003287 optical effect Effects 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 229910052691 Erbium Inorganic materials 0.000 claims description 5
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 5
- 229910052689 Holmium Inorganic materials 0.000 claims description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 229910052772 Samarium Inorganic materials 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052775 Thulium Inorganic materials 0.000 claims description 5
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- 239000004471 Glycine Substances 0.000 claims description 3
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 3
- 235000004279 alanine Nutrition 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- XQBXQQNSKADUDV-UHFFFAOYSA-N lanthanum;nitric acid Chemical compound [La].O[N+]([O-])=O XQBXQQNSKADUDV-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 9
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 229910001960 metal nitrate Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 239000010453 quartz Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000009826 distribution Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 238000000904 thermoluminescence Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000005516 deep trap Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 230000000638 stimulation Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
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- 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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
Abstract
The invention discloses a method for preparing BaSi by a solution combustion method2O5A method for storing fluorescent powder based on light belongs to the field of inorganic material preparation; the invention utilizes a solution combustion method, takes metal nitrate and tetraethyl orthosilicate as raw materials, takes organic amine as fuel, controls the reaction temperature and the raw material ratio, and prepares a series of micro-nano rare earth doped and activated BaSi2O5Fluorescent powder; the rare earth doped BaSi synthesized by the method of the invention2O5The light storage fluorescent powder has the advantages of fluffy structure, simple post-treatment and uniform granularity, and the method is suitable for industrial production and market popularization and application.
Description
Technical Field
The invention relates to a method for preparing BaSi by a solution combustion method2O5A method for storing fluorescent powder based on light belongs to the field of inorganic material preparation.
Background
With the rapid development of internet technology, the amount of data generated and required to be stored is increasing. IDC corporation estimates that the total amount of data worldwide in 2025 will reach 163ZB, one hundred sixty three trillion GB. Therefore, there is an urgent need to develop new high-capacity storage media and technologies. The optical storage fluorescent material is a type of material which is excited by external energy (such as x-ray, high-energy particles, high-energy electrons, ultraviolet light, visible light, and the like), a part of electrons or holes excited in an excited state are stored in a crystal trap, and then are subjected to external stimulation (physical stimulation, pressure, low-energy photons, and the like), and the trapped electrons or holes are released and then emitted in the form of optical energy. Moreover, such materials have an ultra-high theoretical storage density. Therefore, the material has a huge application prospect in information storage, and attracts the attention of countless researchers.
However, in actual development, such materials still face many challenges. For example, despite many years of effort, researchers have developed a large number of light-storing phosphors based on improvements in different luminescent centers, multiple doping strategies, host types, and synthetic methods; however, the actual storage capacity of the material is still not ideal compared to the theoretical storage density. On the other hand, in a large amount of materials, only a few materials can be activated by natural sunlight to realize storage. This means that existing materials require higher writing energy or less light sources for efficient writing. In addition, there is a significant difficulty that hinders the development of light-storing fluorescent materials. For practical optical storage media, independent deep trap narrow-band distribution is required, because only deep trap narrow-band distribution can effectively prevent the stored information from losing at room temperature, thus achieving the purpose of storing information for a long time and permanently; the narrow-band distribution can efficiently respond to external re-stimulation, so that no residual information is output, and the accuracy of information output is ensured; independent refers to a distribution without shallow traps, because shallow traps are low-controlled-release at room temperature, and the generated afterglow signal seriously interferes with the resolution of the target addressing signal. In actual development, however, such a trap distribution is extremely difficult to obtain. Therefore, it is still far and hard to develop and put into practical use the light storage phosphor.
The literature reports rare earth-activated Ba of lanthanide series1-x-ySi2O5:xEu2+,yRe3+(Re = Dy, Pr, Ce, Nd, Tm, Sm, Yb, Gd, Er, Tb, Ho) exhibits high photon storage capacity and variable trap depth with application number 201711212687.5 as a silicateThe fluorescent powder has excellent water stability and physical and chemical stability, and is a potentially practical light storage fluorescent powder. However, the preparation method of the high-temperature solid-phase method results in large and non-uniform (μm-grade) particles in final molding, ceramic products and difficult post-treatment. This will lead to a serious reduction in the use value, because the non-uniformity of the particles will cause the deviation of the reading and writing optical path to cause the information error; on the other hand, the ultra-high capacity optical read-write technology requires that the phosphor particles need to reach the nanometer level.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a solution combustion method for preparing BaSi2O5The method for preparing the basic light storage fluorescent powder overcomes the defect of preparing Ba by a high-temperature solid phase method1-x-ySi2O5:xEu2+,yRe3+(Re is one or more of Dy, Pr, Ce, Nd, Tm, Sm, Yb, Gd, Er, Tb and Ho) or Ba1-xSi2O5:xEu2+The method obtains Ba with fluffy structure, simple post-treatment, uniform and small granularity (micro-nano grade) and high storage capacity by a solution combustion method1-x-ySi2O5:xEu2+,yRe3+(Re is one or more of Dy, Pr, Ce, Nd, Tm, Sm, Yb, Gd, Er, Tb and Ho) or Ba1-xSi2O5:xEu2+An optical storage phosphor.
The method comprises the steps of taking barium nitrate as a barium source, tetraethyl orthosilicate as a silicon source, taking organic amine as a fuel, mixing the barium source, the silicon source, europium nitrate and the organic amine according to a required proportion, adding the mixture into an ethanol aqueous solution, stirring and uniformly mixing, heating the mixture to 200-500 ℃, fully evaporating until the mixture burns, and generating a powder precursor after the mixture burns; calcining the precursor for 3-6 h at 1000-1300 ℃ in a reducing atmosphere, and cooling to room temperature to obtain BaSi2O5A base light storing phosphor; the BaSi2O5The general chemical formula of the basic optical storage fluorescent powder is Ba1-xSi2O5:xEu2+Wherein x is more than or equal to 0.001 and less than or equal to 0.03.
The method comprises the steps of taking barium nitrate as a barium source, tetraethyl orthosilicate as a silicon source, taking organic amine as a fuel, mixing the barium source, the silicon source, europium nitrate, lanthanide nitrate and the organic amine according to a required proportion, adding the mixture into an ethanol water solution, stirring and uniformly mixing, heating the mixture to 200-500 ℃, fully evaporating until the mixture is combusted, and generating a powder precursor after the mixture is combusted; calcining the precursor for 3-6 h at 1000-1300 ℃ in a reducing atmosphere, and cooling to room temperature to obtain BaSi2O5A base light storing phosphor; the BaSi2O5The chemical general formula of the basic optical storage fluorescent powder is Ba1-x-ySi2O5:xEu2+,yRe3+(ii) a Wherein x is more than or equal to 0.001 and less than or equal to 0.03, y is more than or equal to 0.001 and less than or equal to 0.12, and Re is one or more of Dy, Pr, Ce, Nd, Tm, Sm, Yb, Gd, Er, Tb and Ho.
According to the method, a cosolvent boric acid or ammonium chloride can be added during preparation of the precursor, wherein the addition amount of the cosolvent is 3-5% of the total mass of barium nitrate and tetraethyl orthosilicate.
The organic amine is one or more of urea, alanine and glycine, and the molar ratio of ammonium radicals in the organic amine to nitrate radicals in the mixture is 3-4: 6.
The reducing gas is H with the volume concentration of 5 percent2And 95% nitrogen.
The volume concentration of ethanol in the ethanol water solution is 50-80%.
The invention has the following advantages and technical effects:
1. the preparation method is simple and easy to operate, and is suitable for industrial production and market popularization and application;
2. the micro-nano level uniform particles prepared by the method have the advantages of fluffy fluorescent powder structure, simple post-treatment and smaller fluorescent powder particles, and are beneficial to later application.
Drawings
FIG. 1 shows Ba in example 10.97Si2O5:0.03Eu2+Storing a XRD diffraction pattern of the fluorescent powder by light;
FIG. 2 shows Ba in example 10.97Si2O5:0.03Eu2+Storing the SEM atlas of the fluorescent powder by light;
FIG. 3 shows Ba in example 20.9275Si2O5:0.0025Eu2+,0.07Er3+A thermoluminescent curve graph of the optical storage fluorescent powder;
FIG. 4 shows Ba in example 30.965Si2O5:0.005Eu2+,0.03Dy3+A thermoluminescent curve graph of the optical storage fluorescent powder;
FIG. 5 shows Ba in example 40.92Si2O5:0.01Eu2+,0.02Pr3+,0.05Nd3+Thermoluminescence curve diagram of the optical storage fluorescent powder.
Detailed description of the invention
The invention is explained in more detail below with reference to the figures and examples, without limiting the scope of the invention.
Example 1: ba0.97Si2O5:0.03Eu2+The preparation method of the optical storage fluorescent powder comprises the following steps:
0.2535g Ba (NO)3)20.1137g Glycine (C)2H5NO2)、0.0232g H3BO3、0.4208g C8H20O4Si, 30. mu.L of 1mmol/mL Eu (NO)3)3Putting the ethanol solution into a 100mL quartz beaker, adding 50mL ethanol water solution with volume concentration of 50%, adding a magnetic stirrer, putting the quartz beaker on a heating magnetic stirrer, heating to 200 ℃, and fully evaporating the solution until the solution is combusted to generate a precursor; the precursor is placed in a tube furnace again, heated to 1200 ℃, and reduction gas (5% H) is flowed through2、95%N2) Preserving the temperature for 4 hours in the environment, and cooling to room temperature; by X-ray diffraction, it was found that Ba could be obtained0.97Si2O5:0.03Eu2+Pure phase phosphor (fig. 1); in addition, the particles were found to be uniform and to have a particle size of the order of micro-nanometers by scanning electron microscope testing (fig. 2).
Example 2: ba0.9275Si2O5:0.0025Eu2+,0.07Er3+The preparation method of the optical storage fluorescent powder comprises the following steps:
0.4848g Ba (NO)3)2、0.1137g C2H5NO20.0455g of urea (CH)4N2O)、0.02717g NH4Cl、0.8416g C8H20O4Si, 70. mu.l of 1mmol/mL Eu (NO)3)3Ethanol solution, 140. mu.l of 1mmol/mL Er (NO)3)3Putting the ethanol solution into a 100mL quartz beaker, adding 50mL ethanol water solution with volume concentration of 50%, adding a magnetic stirrer, putting the quartz beaker on a heating magnetic stirrer, heating to 300 ℃, and fully evaporating the solution until the solution is combusted to generate a precursor; the precursor is placed in a tube furnace again, heated to 1300 ℃, and reduction gas (5% H) is flowed through2、95%N2) Preserving the heat for 3 hours in the environment, and cooling to room temperature; through the thermoluminescence curve test, the sample was found to possess abundant traps, storing photons (fig. 3).
Example 3: ba0.965Si2O5:0.005Eu2+,0.03Dy3+The preparation of the light storage fluorescent powder is as follows:
0.2522g Ba (NO)3)20.1542g alanine (C)3H7O2N)、0.0185g H3BO3、0.4208g C8H20O4Si, 5. mu.L of 1mmol/mL Eu (NO)3)3Ethanol solution, 30 μ L of 1mmol/mL Dy (NO)3)3Putting the ethanol solution into a 100mL quartz beaker, adding 50mL ethanol aqueous solution with volume concentration of 50%, adding a magnetic stirrer, putting the quartz beaker on a heating magnetic stirrer, heating to 500 ℃, fully evaporating the solution, and then combusting to generate a precursor; the precursor is placed in a tube furnace again, heated to 1000 ℃, and reduction gas (5% H) is flowed through2、95%N2) Preserving the temperature for 6 hours in the environment, and cooling to room temperature; through the thermoluminescence curve test, the sample was found to possess abundant traps, storing photons (fig. 4).
Example 4: ba0.92Si2O5:0.01Eu2+,0.02Pr3+,0.05Nd3+The preparation of the light storage fluorescent powder is as follows
0.2405g Ba (NO)3)2、0.0606g CH4N2O、0.0096g H3BO3、0.0096g NH4Cl、0.4208gC8H20O4Si, 10. mu.L of 1mmol/mL Eu (NO)3)3Ethanol solution, 20. mu.L of 1mmol/mL Pr (NO)3)3Ethanol solution, 50. mu.L of 1mmol/mL Nd (NO)3)3Putting the ethanol solution into a 100mL quartz beaker, adding 50mL ethanol water solution with volume concentration of 50%, adding a magnetic stirrer, putting the quartz beaker on a heating magnetic stirrer, heating to 450 ℃, and fully evaporating the solution until the solution is combusted to generate a precursor; the precursor is placed in a tube furnace again, heated to 1230 ℃, and reduction gas (5% H) is flowed2、95%N2) Preserving the temperature for 5h under the environment, and cooling to room temperature. Through the thermoluminescence curve test, the sample was found to possess abundant traps, storing photons (fig. 5).
Claims (5)
1. BaSi prepared by solution combustion method2O5The method for storing the fluorescent powder by the base light is characterized by comprising the following steps: mixing barium nitrate serving as a barium source, tetraethyl orthosilicate serving as a silicon source and organic amine serving as a fuel, adding the mixture of the barium source, the silicon source, europium nitrate and the organic amine into an ethanol aqueous solution, stirring and uniformly mixing, heating the mixture to 200-500 ℃, fully evaporating until the mixture burns, and generating a powder precursor after the mixture burns; calcining the precursor for 3-6 h at 1000-1300 ℃ in a reducing atmosphere, and cooling to room temperature to obtain BaSi2O5A base light storing phosphor; the BaSi2O5The general chemical formula of the basic optical storage fluorescent powder is Ba1-xSi2O5:xEu2+Wherein x is more than or equal to 0.001 and less than or equal to 0.03.
2. The solution combustion method for preparing BaSi according to claim 12O5The method for storing the fluorescent powder by the base light is characterized by comprising the following steps: the raw material also comprises lanthanide nitrate, and the prepared BaSi2O5The general chemical formula of the basic optical storage fluorescent powder is Ba1-x-ySi2O5:xEu2+,yRe3+(ii) a Wherein x is more than or equal to 0.001 and less than or equal to 0.03, and y is more than or equal to 0.001 and less than or equal to 0.12Re is one or more of Dy, Pr, Ce, Nd, Tm, Sm, Yb, Gd, Er, Tb and Ho.
3. The solution combustion method for preparing BaSi according to claim 1 or 22O5The method for storing the fluorescent powder by the base light is characterized by comprising the following steps: the raw materials also comprise a cosolvent boric acid or ammonium chloride, and the addition amount of the cosolvent is 3-5% of the total mass of the barium nitrate and the tetraethyl orthosilicate.
4. The solution combustion method for preparing BaSi according to claim 32O5The method for storing the fluorescent powder by the base light is characterized by comprising the following steps: the organic amine is one or more of urea, alanine and glycine, and the molar ratio of ammonium radicals in the organic amine to nitrate radicals in the mixture is 3-4: 6.
5. The solution combustion method for preparing BaSi according to claim 32O5The method for storing the fluorescent powder by the base light is characterized by comprising the following steps: the volume concentration of ethanol in the ethanol water solution is 50-80%.
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V.B. BHATKAR ET AL.: "Combustion synthesis of silicate phosphors", 《OPTICAL MATERIALS》 * |
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