CN109133922B - Double-doped rare earth ion garnet structure optical function ceramic powder and preparation method thereof - Google Patents
Double-doped rare earth ion garnet structure optical function ceramic powder and preparation method thereof Download PDFInfo
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- DFCYEXJMCFQPPA-UHFFFAOYSA-N scandium(III) nitrate Inorganic materials [Sc+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O DFCYEXJMCFQPPA-UHFFFAOYSA-N 0.000 description 1
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- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 1
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Abstract
A double-doped rare earth ion garnet structure optical functional ceramic powder and a preparation method thereof are disclosed, wherein the chemical general formula of the powder is as follows: (Y)1‑x‑yPrxCey)3(Al1‑nAn)5O12(ii) a A is Ga, Cr, Sc or Mn; the preparation method comprises the following steps: (1) preparing a metal cation mixed solution; (2) preparation of a solution containing NH4 +The precipitant solution of (a); (3) heating the metal cation mixed solution, and then titrating and mixing the heated metal cation mixed solution with a precipitant solution; (4) addition of NH4HCO3After adjusting the pH value of the solution, standing and aging; (5) filtering and washing to obtain a precursor; (6) and grinding and calcining. The powder particles prepared by the invention have good dispersibility; can be applied to the fields of LED fluorescent display, high-energy particle and ray detection and the like, and is a light functional material with wide application prospect.
Description
Technical Field
The invention belongs to the technical field of optical functional ceramic materials, and particularly relates to double-doped rare earth ion garnet structure optical functional ceramic powder and a preparation method thereof.
Background
The rare earth ion doped optical functional ceramic powder is a main basic material of fluorescent powder and high optical functional ceramic materials, and provides a multi-angle and multi-layer material foundation for realization and application of high-energy physics, safety inspection, nondestructive industrial flaw detection, X-CT and positron emission tomography PET technologies by utilizing the characteristic of effective interaction between a broadband light wave resource radiated by rich energy level transition of rare earth ions and high-energy particles or rays such as X rays, alpha, beta and gamma rays.
At present, in optical functional devices such as a solid laser, X-ray CT and the like which relate to the interaction of a dielectric material and high-energy particles or rays, the application of a single crystal material is still the most extensive, compared with the single crystal material obtained by using a pulling method, a traditional growth method and the like, a ceramic material has the characteristics of low preparation cost and energy consumption, easiness in realizing large-size, uniform high-concentration doping, and more ideal mechanical property and chemical thermal stability, and the preparation of a high-performance optical functional ceramic powder material provides an objective material basis and an effective way for the ceramic material to replace the single crystal material in the future.
In order to improve the quality and performance of the optical functional ceramic powder, how to perfect the preparation process of the powder material and further optimize the process parameters to realize the controllability of the microstructure and the performance shearing is the direction and content which needs to be further researched and discussed. The existing preparation methods of the optical functional ceramic powder material mainly comprise a solid phase method, a chemical method, a sol-gel method and the like, wherein the chemical coprecipitation method is easy to realize uniform doping on a molecular scale and is easy to further uniformly perform the substitution reaction of luminescent central ions and matrix ions; the preparation steps of the chemical coprecipitation process are mainly divided into two parts, namely precursor preparation and ceramic powder preparation, and the preparation steps mainly comprise: titration, aging, leaching and filtering, drying, grinding and calcining, wherein the process parameters related to each step have important influence on the performance of the finally obtained powder material sample. In the existing ceramic powder preparation technology, the agglomeration phenomenon is still one of the factors and problems influencing the microscopic morphology and the luminescence property of the optical functional ceramic powder; the YAG ceramic material is prepared by a wet chemical method in the intelligent forest, the agglomeration phenomenon is slowed down by a method of n-amyl alcohol-free and reduced pressure distillation aiming at the filtering and leaching process in the ceramic powder preparation process, and the obtained powder is calcined at 1100 ℃ for 2 hours to obtain YAG ceramic powder with improved dispersibility; sun Yan for Ce: the GAGG ceramic powder material is prepared by using an UACC (Ultra Assisted Chemical Co-precipitation) ultrasonic Assisted Chemical precipitation method in the process of a titration process, and introducing an external physical field to exert influence on the process of a precipitation reaction stage so as to improve the particle size and the spatial distribution state; zhou Hefeng and the like use a solid-phase reaction method to calcine for 9 hours at 1450 ℃ under the carbon reducing atmosphere to obtain the Ce, Pr and YAG ceramic powder.
The work has certain limitation on the optical performance, namely luminous intensity and micro appearance, of the garnet-structured optical functional ceramic powder material, particularly on the improvement of the agglomeration phenomenon; the unicity of the introduction of the activator ions also limits the radiative transition luminescence of the material to some extent.
Disclosure of Invention
The invention aims to provide optical functional ceramic powder with a double-doped rare earth ion garnet structure and a preparation method thereof.
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
wherein A is Ga, Cr, Sc or Mn occupying lattice positions of Al atoms, x = 0.001-0.005, y = 0.001-0.005, and n = 0-0.05.
The grain size of the double-doped rare earth ion garnet structure optical functional ceramic powder is 30-80 nm.
The preparation method of the double-doped rare earth ion garnet structure optical functional ceramic powder comprises the following steps:
1. preparing Al according to the proportion of metal elements in the chemical general formula3+、Ce3+、Y3+And Pr3+Or a mixed solution of metal cations of (5), or containing Al3+、Ce3+、Y3+ 、Pr3+And a metal cation mixed solution of A ions; the A ion is Ga3+、Cr3+、Sc3+Or Mn2+(ii) a Al in metal cation mixed solution3+The concentration of (A) is 0.1-5 mol/L;
2. preparation of a solution containing NH4 +Solution of (2), NH4 +The concentration of (a) is 0.1-5 mol/L, and the solution is used as a precipitant solution;
3. heating the metal cation mixed solution to 30-60 ℃; by adopting a forward titration method, the precipitant solution is dripped into the heated metal cation mixed solution, and the mixture is stirred and mixed uniformlyMixing to form a mixed solution; or dripping the heated metal cation mixed solution into the precipitator solution by adopting a reverse titration method, and uniformly stirring and mixing to form a mixed solution; or titrating the heated metal cation mixed solution and the precipitant solution into a container simultaneously by adopting a co-titration method, and stirring and mixing uniformly to form a mixed solution; the dosage ratio of the metal cation mixed solution and the precipitant solution is that the total metal cation and NH4 +In a molar ratio of 1: 3;
4. adding NH into the mixed solution4HCO3Adjusting the pH value of the solution to 9-11, and then standing and aging for 6-24 hours to obtain a suspension;
5. filtering the suspension to obtain a filter cake, and washing to obtain a precursor;
6. grinding the precursor into powder, and calcining for 0.5-6 hours at 600-1200 ℃ to prepare the double-doped rare earth ion garnet structured light functional ceramic powder.
In the method, the raw material for preparing the metal cation mixed solution is metal inorganic salt with crystal water or metal inorganic salt solution prepared by dissolving the metal inorganic salt with crystal water in water; the metal inorganic salt with the crystal water is nitrate with the crystal water.
In the above method, the solution containing NH is prepared4 +The solution adopts ammonia water and/or NH as raw materials4HCO3。
In the above method, the solution containing NH is prepared4 +To a solution containing NH4 +Adding a high molecular active agent, oxalic acid and/or glycerol into the solution to prepare a mixed solution as a precipitator solution; the macromolecular active agent is PEG400, PEG600 or PEG 2000; when the high-molecular active agent is added, the mass concentration of the high-molecular active agent in the precipitator solution is 0.03-0.05%, and when the oxalic acid is added, the oxalic acid and NH in the precipitator solution4 +In a molar ratio of 1: 1; when the glycerol is added, the volume ratio of the glycerol to the precipitant solution is 1 (15-25).
In the method, the temperature of the precipitator solution is controlled to be 25-30 ℃ after the precipitator solution is prepared, and the control mode is an air cooling mode.
In the method, the washing is to wash with water to remove ionic impurities, then wash with absolute ethyl alcohol to remove organic impurities, and volatilize the residual absolute ethyl alcohol in the subsequent steps; wherein, when washing, the water is firstly heated to 30-90 ℃.
NH in the above step 44HCO3The concentration of the solution is 10-15%.
The invention uses the improved chemical coprecipitation method to obtain the nano ceramic powder with excellent optical performance and good powder particle dispersibility; the chemical precipitation method has the advantages of low production cost, low energy consumption and the like, the precipitation reaction is uniformly carried out on a molecular scale, the rare earth ion double-doped ceramic powder with a good microstructure and good luminous performance can avoid the agglomeration phenomenon of the product and improve the crystal form integrity (when the product is not added, the product is added if the agglomeration phenomenon exists), and the method can be applied to the fields of LED fluorescent display, high-energy particle, ray detection and the like and is a light functional material with a wide application prospect.
Drawings
FIG. 1 is a graph of the infrared spectrum of the precursor of example 1;
FIG. 2 is a Field Emission Scanning Electron Microscope (FESEM) surface topography of the precursor of example 1;
FIG. 3 is an X-ray diffraction (XRD) spectrum of a dual doped rare earth ion garnet structure optical functional ceramic powder in example 1;
FIG. 4 is a surface morphology of a field emission electron scanning microscope (FESEM) of a dual-doped rare earth ion garnet structure optical functional ceramic powder in example 1;
FIG. 5 is a field emission electron scanning microscope (FESEM) surface topography plot of a product prepared in a comparative experiment in example 1 without the addition of a polymeric active agent;
FIG. 6 is a graph of the excitation emission spectrum (520 nm) of the double-doped rare earth ion garnet structural optical functional ceramic powder in example 1;
FIG. 7 is a graph of the excitation emission spectrum (360 nm) of the double-doped rare earth ion garnet structure optical functional ceramic powder in example 1.
Detailed Description
To further illustrate the invention, the following specific examples are given; the examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention.
Al (NO) used in examples of the present invention3)3∙9H2O、Y(NO3)3∙6H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O、Ga (NO3)3∙6H2O、Cr(NO3)3∙9H2O、Sc(NO3)3∙6H2O or Mn (NO)3)2∙6H2O is a commercial product with the purity of more than 99.99 percent.
The water used in the examples of the present invention is deionized water.
The absolute ethyl alcohol adopted in the embodiment of the invention is a commercially available analytical pure reagent.
NH used in the examples of the present invention4HCO3Is a commercially available analytical pure reagent.
The ammonia water (with the mass concentration of 28-30%) adopted in the embodiment of the invention is a commercially available analytical pure reagent.
The PEG400, PEG600 and PEG2000 used in the examples of the present invention are commercially available products.
The oxalic acid and the glycerol adopted in the embodiment of the invention are commercially available analytical pure reagents.
The drying mode in the embodiment of the invention is electric oven drying, vacuum drying or microwave drying.
NH in examples of the invention4HCO3The concentration of the solution is 10-15%.
Example 1
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3Al5O12；
wherein x =0.001, y =0.005, and the grain size is 30-80 nm;
the preparation method comprises the following steps:
mixing Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O and Pr (NO)3)3∙6H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+And Pr3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 0.5 mol/L;
with ammonia and NH4HCO3Preparation of NH4 +Adding PEG600 with the concentration of 0.05 percent of the total mass of the solution to form a mixed solution as a precipitator solution;
heating the cation mixed solution to 30 ℃; dripping the heated metal cation mixed solution into a precipitator solution by adopting a reverse titration method, and uniformly stirring and mixing to form a mixed solution; the dosage ratio of the metal cation mixed solution and the precipitant solution is that the total metal cation and NH4 +In a molar ratio of 1: 3;
adding NH into the mixed solution4HCO3Adjusting the pH value of the solution to 9.3, and then standing and aging for 6h to obtain a suspension;
filtering the suspension to obtain a filter cake, washing with water to remove ionic impurities, and then washing with anhydrous ethanol to remove organic impurities (the residual anhydrous ethanol is volatilized in the subsequent steps) to obtain a precursor, wherein the infrared spectrum curve of the precursor is shown in figure 1, and the scanning surface morphology of an electron microscope is shown in figure 2; wherein, when washing, the water is firstly heated to 30 ℃;
grinding the precursor into powder, calcining at 900 deg.C for 3 hr to obtain double-doped rare earth ion garnet structure optical functional ceramic powder, with X-ray diffraction as shown in FIG. 3 and electron microscope scanning surface morphology as shown in FIG. 4 (from figure, its particle diameter D can be seen)50= 30-80 nm), the excitation emission spectrum curves are respectively shown in FIG. 6 (detection emission wavelength: 520nm, gate width 5nm, photomultiplier voltage 550V) and FIG. 7 (detection excitation wavelength 360nm, gate width 5nm, photomultiplier voltage 550V)Tube voltage 500V);
the raw materials are adopted for comparison tests, PEG600 is not added when the precipitator solution is prepared, other conditions are the same, the electron microscope scanning surface appearance of the prepared ceramic powder is shown in figure 5, and the agglomeration phenomenon is serious as can be seen from the figure.
Example 2
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3Al5O12；
wherein x =0.002, y =0.004, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) al in metal cation mixed solution3+The concentration of (A) is 0.1 mol/L;
(2) preparation of NH from ammonia4 +The solution with the concentration of 1mol/L is used as a precipitant solution;
(3) heating the cation mixed solution to 50 ℃; dropwise adding the precipitant solution into the heated metal cation mixed solution by adopting a forward titration method, and uniformly stirring and mixing to form a mixed solution;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 9.5, and then standing and aging for 8 hours;
(5) when washing, firstly heating water to 40 ℃;
(6) the precursor was ground to a powder and then calcined at 600 ℃ for 6 hours.
Example 3
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3Al5O12；
wherein x =0.003, y =0.003, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) al in metal cation mixed solution3+The concentration of (A) is 1 mol/L;
(2) by NH4HCO3Preparation of NH4 +The solution with the concentration of 1.5mol/L is used as a precipitant solution;
(3) heating the cation mixed solution to 60 ℃; titrating the heated metal cation mixed solution and the precipitant solution into a container simultaneously by adopting a co-titration method, and stirring and mixing uniformly to form a mixed solution;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 9.8, and then standing and aging for 12 h;
(5) when washing, firstly heating water to 50 ℃;
(6) the precursor was ground to a powder and then calcined at 1200 ℃ for 0.5 hours.
Example 4
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
wherein A is Ga element, x =0.001, y =0.005, n =0.01, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) mixing Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O and Ga (NO)3)3∙6H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+、Pr3+And Ga3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 2 mol/L;
(2) with ammonia and NH4HCO3Preparation of NH4 +Adding PEG40 as high molecular active agent into the solution with the concentration of 5mol/L0, as precipitant solution; the mass concentration of the high molecular active agent in the precipitant solution is 0.03%; controlling the temperature to be 25-30 ℃ by adopting an air cooling mode;
(3) heating the cation mixed solution to 35 ℃; dropwise adding the precipitant solution into the heated metal cation mixed solution by adopting a forward titration method, and uniformly stirring and mixing to form a mixed solution;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 10, and then standing and aging for 16 h;
(5) when washing, firstly heating water to 60 ℃;
(6) the precursor was ground to a powder and then calcined at 1100 ℃ for 1 hour.
Example 5
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
in the formula, A is Cr element, x =0.002, y =0.004, n =0.02, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) to Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O and Cr (NO)3)3∙9H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+、Pr3+And Cr3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 3 mol/L;
(2) adopts the raw material of ammonia water to prepare NH4 +Adding a macromolecular active agent PEG600 as a precipitant solution into the solution with the concentration of 3 mol/L; the mass concentration of the high molecular active agent in the precipitant solution is 0.04 percent; by air coolingThe temperature is controlled to be 25-30 ℃;
(3) heating the cation mixed solution to 45 ℃;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 10.4, and then standing and aging for 18 h;
(5) when washing, firstly heating water to 70 ℃;
(6) the precursor was ground to a powder and then calcined at 1000 ℃ for 1.5 hours.
Example 6
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
wherein A is Sc element, x =0.003, y =0.003, n =0.03, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) mixing Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O and Sc (NO)3)3∙6H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+、Pr3+And Sc of3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 4 mol/L;
(2) by NH4HCO3Preparation of NH4 +Adding a macromolecular active agent PEG2000 as a precipitant solution into the solution with the concentration of 0.1 mol/L; the mass concentration of the high molecular active agent in the precipitant solution is 0.05 percent; controlling the temperature to be 25-30 ℃ by adopting an air cooling mode;
(3) heating the cation mixed solution to 55 ℃; titrating the heated metal cation mixed solution and the precipitant solution into a container simultaneously by adopting a co-titration method, and stirring and mixing uniformly to form a mixed solution;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 10.6, and then standing and aging for 20 h;
(5) when washing, firstly heating water to 80 ℃;
(6) the precursor was ground to a powder and then calcined at 800 ℃ for 2.5 hours.
Example 7
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
in the formula, A is Mn element, x =0.004, y =0.003, n =0.04, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) mixing Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O and Mn (NO)3)3∙6H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+、Pr3+And Mn3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 5 mol/L;
(2) preparation of NH from ammonia4 +The solution with the concentration of 2mol/L is added with oxalic acid to be used as a precipitator solution; oxalic acid and NH in precipitant solution4 +In a molar ratio of 1: 1; controlling the temperature to be 25-30 ℃ by adopting an air cooling mode;
(3) dropwise adding the precipitant solution into the heated metal cation mixed solution by adopting a forward titration method, and uniformly stirring and mixing to form a mixed solution;
(4) adding NH into the mixed solution4HCO3Adjusting the pH valueIs 11, then stands and ages for 24 hours;
(5) when washing, firstly heating water to 90 ℃;
(6) the precursor was ground to a powder and then calcined at 700 ℃ for 4 hours.
Example 8
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
wherein A is Ga element, x =0.005, y =0.001, n =0.05, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) mixing Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O and Ga (NO)3)3∙6H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+、Pr3+And Ga3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 0.8 mol/L;
(2) by NH4HCO3Preparation of NH4 +The concentration of the solution is 2.5mol/L, and the solution is used as a precipitator solution after glycerol is added; wherein the volume ratio of the glycerol to the precipitant solution is 1: 20; controlling the temperature to be 25-30 ℃ by adopting an air cooling mode;
(3) heating the cation mixed solution to 40 ℃;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 9.6, and then standing and aging for 13 h;
(5) when washing, firstly heating water to 55 ℃;
(6) the precursor was ground to a powder and then calcined at 1150 ℃ for 1 hour.
Example 9
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
in the formula, A is Cr element, x =0.002, y =0.002, n =0.02, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) mixing Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O and Cr (NO)3)3∙9H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+、Pr3+And Cr3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 1.5 mol/L;
(2) with ammonia and NH4HCO3Preparation of NH4 +Adding a high molecular active agent, oxalic acid and glycerol into the solution with the concentration of 0.8mol/L to prepare a precipitator solution; the macromolecular active agent is PEG 600; the mass concentration of the macromolecular active agent in the precipitant solution is 0.04%, and oxalic acid and NH4 +In a molar ratio of 1: 1; the volume ratio of the glycerol to the precipitant solution is 1: 15; controlling the temperature to be 25-30 ℃ by adopting an air cooling mode;
(3) heating the cation mixed solution to 50 ℃; titrating the heated metal cation mixed solution and the precipitant solution into a container simultaneously by adopting a co-titration method, and stirring and mixing uniformly to form a mixed solution;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 10.1, and then standing and aging for 15 h;
(5) when washing, firstly heating water to 65 ℃;
(6) the precursor was ground to a powder and then calcined at 1050 ℃ for 1.5 hours.
Example 10
The chemical general formula of the double-doped rare earth ion garnet structure optical functional ceramic powder is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
in the formula, A is Sc element, x =0.004, y =0.004, n =0.04, and the grain size is 30-80 nm;
the method is the same as example 1, except that:
(1) mixing Al (NO)3)3∙9H2O、Ce(NO3)3∙6H2O、Pr(NO3)3∙6H2O and Sc (NO)3)3∙6H2O is prepared into aqueous solution respectively to prepare Y (NO)3)3∙6H2O; mixing the aqueous solution with Y (NO)3)3∙6H2Dissolving O in water to obtain Al-containing solution3+、Ce3+、Y3+、Pr3+And Sc of3+The metal cation mixed solution of (1); al in metal cation mixed solution3+The concentration of (A) is 2.2 mol/L;
(2) by NH4HCO3Preparation of NH4 +Adding oxalic acid and glycerol into the solution with the concentration of 4mol/L to prepare a precipitator solution; oxalic acid and NH in precipitant solution4 +The molar ratio of the glycerol to the precipitant solution is 1:1, and the volume ratio of the glycerol to the precipitant solution is 1: 25; controlling the temperature to be 25-30 ℃ by adopting an air cooling mode;
(3) heating the cation mixed solution to 60 ℃; dropwise adding the precipitant solution into the heated metal cation mixed solution by adopting a forward titration method, and uniformly stirring and mixing to form a mixed solution;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value to 10.7, and then standing and aging for 19 h;
(5) when washing, firstly heating water to 45 ℃;
(6) the precursor was ground to a powder and then calcined at 950 ℃ for 3.5 hours.
Claims (1)
1. A preparation method of double-doped rare earth ion garnet structure optical functional ceramic powder is characterized by comprising the following steps:
(1) according to the proportion of metal elements in the chemical general formula of the double-doped rare earth ion garnet structure optical function ceramic powder body3+、Ce3+、Y3+ 、Pr3+And a metal cation mixed solution of A ions; the A ion is Ga3+、Cr3+、Sc3+Or Mn2+(ii) a Al in metal cation mixed solution3+The concentration of (A) is 0.1-5 mol/L; the chemical general formula is as follows:
(Y1-x-yPrxCey)3(Al1-nAn)5O12；
wherein A is Ga, Cr, Sc or Mn occupying Al atomic lattice positions, x = 0.002-0.004, y = 0.002-0.004, and n = 0.02-0.05; the raw material for preparing the metal cation mixed solution is metal inorganic salt with crystal water or metal inorganic salt solution prepared by dissolving the metal inorganic salt with crystal water in water; the metal inorganic salt with the crystal water is nitrate with the crystal water;
(2) preparation of a solution containing NH4 +Solution of (2), NH4 +The concentration of the sodium hydroxide is 0.8-5 mol/L, and the sodium hydroxide is used as a precipitant solution; preparation of a solution containing NH4 +The solution adopts ammonia water and/or NH as raw materials4HCO3(ii) a Preparation of a solution containing NH4 +To a solution containing NH4 +Adding oxalic acid and/or glycerol into the solution to prepare a mixed solution as a precipitant solution; when oxalic acid is added, the oxalic acid and NH in the precipitant solution4 +In a molar ratio of 1: 1; when the glycerol is added, the volume ratio of the glycerol to the precipitator solution is 1 (15-25); after the precipitator solution is prepared, controlling the temperature to be 25-30 ℃, and selecting an air cooling mode as a control mode;
(3) heating the metal cation mixed solution to 30-60 ℃; by means of forward titrationDropwise adding a precipitant solution into the heated metal cation mixed solution, and uniformly stirring and mixing to form a mixed solution; or dripping the heated metal cation mixed solution into the precipitator solution by adopting a reverse titration method, and uniformly stirring and mixing to form a mixed solution; or titrating the heated metal cation mixed solution and the precipitant solution into a container simultaneously by adopting a co-titration method, and stirring and mixing uniformly to form a mixed solution; the dosage ratio of the metal cation mixed solution and the precipitant solution is that the total metal cation and NH4 +In a molar ratio of 1: 3;
(4) adding NH into the mixed solution4HCO3Adjusting the pH value of the solution to 9.6-11, and then standing and aging for 13-24 hours to obtain a suspension; NH (NH)4HCO3The concentration of the solution is 10-15%;
(5) filtering the suspension to obtain a filter cake, and washing to obtain a precursor;
(6) grinding the precursor into powder, and calcining at 700-1150 ℃ for 1-4 hours to prepare the double-doped rare earth ion garnet structure optical function ceramic powder with the grain size of 30-80 nm.
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