CN108751991B - Preparation of Tb: Lu by laser sintering2O3Method for producing ceramic - Google Patents
Preparation of Tb: Lu by laser sintering2O3Method for producing ceramic Download PDFInfo
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Abstract
The invention discloses a method for preparing Tb: Lu by laser sintering2O3The method for preparing the ceramic comprises the following steps: according to the chemical structural formula (Lu)1‑ xTbx)2O3Respectively weighing reaction raw material powder according to the stoichiometric ratio of the elements, adding citric acid and glycol into the mixed raw materials, and uniformly stirring to obtain a precursor; then heating the precursor powder, grinding and calcining by stages; adding an adhesive polyvinyl alcohol solution into the calcined powder and preparing the powder into a wafer shape by adopting a dry pressing method to obtain a biscuit sheet; placing the biscuit in a Lu2O3On the gasket, double-sided sintering is carried out on the gasket by a laser; finally grinding and polishing to obtain Tb: Lu2O3A ceramic. The method provided by the invention can effectively inhibit Tb3+Ion direction Tb4+Ion transformation improves Tb in the ceramic3+The ion content can realize high-intensity green light emission under the excitation of 323nm ultraviolet light, the preparation process is simple, energy is saved, the environment is protected, the relative density of the prepared ceramic sample reaches 99.9 percent, the transmittance is high, and the compactness is good.
Description
Technical Field
The invention belongs to the technical field of ceramic material preparation, and particularly relates to a method for preparing Tb: Lu by laser sintering2O3A method of making a ceramic.
Background
Lutetium oxide (Lu)2O3) The material has high transmittance under visible light and infrared light, large emission section, low phonon energy, high density, and good mechanical and thermal properties. Therefore, the lutetium oxide is an excellent laser medium material and scintillator material, and has a wide application prospect. Lu (Lu)2O3The transparent ceramic has a cubic crystal structure, optical isotropy and directional-independent refractive index, and can be prepared by a nanocrystalline technology and a high-temperature sintering technology. At the same time, Lu2O3The transparent ceramics can be conveniently realizedThe doping of the rare earth ions with the same kind and different concentrations has wide optical application.
Among the rare earth ions, Tb3+Ionic radius of ion and Lu3+Ions have similar ionic radii, therefore Tb3+Ion incorporation of Lu2O3The lattice distortion generated after the lattice is small, and the doping with higher concentration can be realized. Under the excitation of ultraviolet light, Tb3+Ion can occur5D4Energy level direction7F5Transition of energy level to provide green light for white light synthesis, and Tb: Lu2O3The transparent ceramic has wide application in the field of white light LEDs. In addition, Tb: Lu2O3The transparent ceramic has high thermal conductivity, is beneficial to the dissipation of heat, and has wide application prospect in the field of plasma flat panel displays.
Vacuum sintering is widely applied to Tb: Lu as a sintering mode for effectively promoting densification2O3And (4) preparing transparent ceramics. During the vacuum sintering process, a large amount of oxygen vacancies are generated in the ceramic, and the oxygen vacancies need to be compensated by long-time high-temperature air annealing (1450 ℃ multiplied by 10 h). However, in the air annealing process, a large amount of Tb inevitably exists3+Ions with O2Formation of Tb by reaction4+Ion, and Tb4+Ion does not emit light, Tb3+The reduction of the ion content directly results in Tb: Lu2O3The luminous performance of the ceramic is reduced. In addition, in the conventional vacuum sintering technology, in order to effectively regulate and control the densification process of the ceramic, sintering aids such as MgO and TEOS are indispensable. But the introduction of sintering aids will lead to an imbalance in electrovalence. During sintering, Tb results from charge compensation3+Ion direction Tb4+The ions are transformed, thereby affecting the luminescent quality of the ceramic. Therefore, Tb is difficult to be sintered by vacuum sintering3+To Tb4+Is effectively controlled. In addition, the traditional vacuum sintering needs higher sintering temperature (1600-1800 ℃) and longer heat preservation time (8-20 hours), which causes the sintered ceramic grains to have generally larger size (10-30 mu m), poor mechanical properties and difficult satisfactionThe market demand for its mechanical properties.
Disclosure of Invention
The invention aims to provide a method for preparing Tb: Lu by laser sintering2O3The method of the ceramic can effectively inhibit Tb3+Ion direction Tb4+Ion conversion, low sintering temperature and short sintering time.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: preparation of Tb: Lu by laser sintering2O3A method of making a ceramic, comprising the steps of:
(1) according to the chemical structural formula (Lu)1-xTbx)2O3The stoichiometric ratio of the elements in the solution is respectively called Lu containing lutetium ions3+And a compound containing terbium ion Tb3+The powder of the compound (2) is used as a reaction raw material, wherein x is Tb3+Doped Lu3+The mole percentage of the position, x is more than or equal to 0.001 and less than or equal to 0.02;
(2) adding citric acid and glycol solution into the mixed raw material powder, and uniformly stirring to obtain a precursor solution, wherein the molar ratio of metal ions to citric acid is 0.2-0.5, and the mass ratio of citric acid to glycol is 1-2;
(3) carrying out heat treatment on the precursor solution at 70-80 ℃, removing redundant water, cooling to room temperature, and grinding to obtain precursor powder; then placing the ground precursor powder at 500-800 ℃ for pre-calcining for 5-7 h, removing redundant organic matters, and placing the pre-calcined precursor powder at 800-1200 ℃ for calcining for 1-3 h;
(4) adding an adhesive polyvinyl alcohol solution into the calcined powder for plasticizing, and pressing the powder into a round sheet shape by adopting a dry pressing method to obtain a biscuit blank sheet, wherein the adding amount of the polyvinyl alcohol solution is 1.0-7.0% of the mass of the pressed powder;
(5) placing the biscuit in a Lu2O3On the gasket, sintering the two sides of the biscuit sheet simultaneously by using a laser to obtain a ceramic biscuit;
(6) grinding and polishing the sintered ceramic blank to 1-3 mm to obtain Tb: Lu2O3Is transparentA ceramic.
Preferably, in step (1), the Lu containing lutetium ions3+The compound of (A) is lutetium oxide or lutetium nitrate, and the compound contains terbium ions Tb3+The compound of (1) is one of terbium nitrate, terbium chloride and terbium oxide.
Preferably, in the step (4), the concentration of the polyvinyl alcohol solution is 0.05-0.2 g/ml.
Preferably, in the step (4), the polymerization degree of the polyvinyl alcohol is 1600 to 1900.
Preferably, in the step (4), the pressing pressure is 800-1200 Mpa, the diameter of the biscuit sheet is 2.0-6.0 mm, and the thickness is 0.5-3.0 mm.
Preferably, in the step (5), the laser output power density is 3.2-3.4W/mm2The beam diameter is 4.9-5.5 mm.
Preferably, in the step (5), the laser scanning speed is 2-12 mm/s.
Compared with the prior art, the invention has the following beneficial effects:
1. in the laser sintering process, oxygen vacancies are not generated in the ceramic, so that the sintered sample does not need air annealing, and Tb can be effectively inhibited3+Ion direction Tb4+Ion transformation; moreover, by adopting the laser sintering technology, as no sintering aid needs to be introduced, the phenomenon of unbalanced electrovalence in the ceramic can be avoided, thereby inhibiting Tb brought by charge compensation4+Ion generation, increased Tb in the ceramic3+The ion content can realize high-intensity green light emission under the excitation of 323nm ultraviolet light.
2. The method for preparing Tb: Lu2O3The required sintering time of the transparent ceramic is short, the laser sintering process only needs 3-15 min, the energy is saved, the environment is protected, and the batch production is easy; and the ceramic crystal grain prepared by laser sintering has small size (1-5 mu m) and good mechanical property, and meets the requirement of the current market on the mechanical property of the transparent ceramic.
3. The Tb: Lu prepared by the method provided by the invention2O3The relative density of the transparent ceramic sample reaches 99.9 percent, the compactness is good, the transmittance is high,laser output can be achieved.
Drawings
FIG. 1 shows Tb: Lu prepared in example 2 of the present invention2O3XRD pattern of transparent ceramic.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Unless otherwise stated, the raw materials used in the following examples are all commercially available products, and the purity of the raw material powder is 99.9% or higher.
Example 1: (Lu)0.999Tb0.001)2O3Transparent ceramics
According to (Lu)0.999Tb0.001)2O3Respectively weighing Lu according to the stoichiometric ratio of each element2O3And Tb4O7The powder is used as a reaction raw material;
diluting citric acid with distilled water to a concentration of 0.05g/ml, adding citric acid and glycol solution (the molar ratio of metal ions to citric acid is 0.2, and the mass ratio of citric acid to glycol is 1) into the mixed raw materials, and uniformly stirring to obtain precursor solution;
heating the precursor solution to 70 ℃, preserving heat for 24h to remove redundant water, cooling to room temperature, and then placing the precursor solution in a mortar for grinding to obtain precursor powder; and then pre-calcining the ground precursor powder for 5 hours at 500 ℃ to remove redundant organic matters, and then placing the pre-calcined precursor powder in a muffle furnace to calcine for 1 hour at 800 ℃.
Adding 0.05g/ml of polyvinyl alcohol (with polymerization degree of 1600-1900) solution as an adhesive into the calcined powder for plasticizing, and pressing the powder into a wafer with the diameter of 2.0mm and the thickness of 0.5mm by a dry pressing method under the pressure of 80MPa to obtain the biscuit blank.
Placing the dry pressed vegetarian embryo pieces in Lu2O3On the spacer, the spacer was sintered with a laser beam having a diameter of 4.9mm at a laser power of 0.01W/mm2Linear power of 3.2W/mm2And is maintained at maximum power70s, the scanning speed is 2mm/s, and the time of full laser sintering is 5 min. In this process, the two sides of the biscuit sheet are sintered simultaneously. Finally, grinding and polishing the ceramic biscuit to 1mm to obtain Tb: Lu2O3A transparent ceramic.
The ceramic sample prepared in this example was Lu2O3The phase has no other impurity phase, and the ceramic has higher purity. The ceramic crystal grain size is 3.2 μm, the optical transmittance is 81.0% at 400nm, the optical quality is good, and the green light output of 550nm can be realized under the excitation of 323nm light.
Example 2: (Lu)0.995Tb0.005)2O3Transparent ceramics
According to (Lu)0.995Tb0.005)2O3Lu (NO) is weighed according to the stoichiometric ratio of each element3)3·6H2O and Tb (NO)3)3·5H2Taking O powder as a reaction raw material;
diluting citric acid with distilled water to a concentration of 0.1g/ml, adding citric acid and glycol solution (the molar ratio of metal ions to citric acid is 0.3, and the mass ratio of citric acid to glycol is 1.5) into the mixed raw materials, and uniformly stirring to obtain a precursor solution;
heating the precursor solution to 75 ℃, preserving heat for 24h to remove redundant water, cooling to room temperature, and then placing the precursor solution in a mortar for grinding to obtain precursor powder; and then pre-calcining the ground precursor powder for 5 hours at 700 ℃ to remove redundant organic matters, and then placing the pre-calcined precursor powder in a muffle furnace to calcine for 2 hours at 1000 ℃.
Adding 0.1g/ml of polyvinyl alcohol (with polymerization degree of 1600-1900) solution as an adhesive into the calcined powder for plasticizing, and pressing the powder into a wafer with the diameter of 4.0mm and the thickness of 1.5mm by a dry pressing method under the pressure of 120MPa to obtain the biscuit sheet.
Placing the dry pressed vegetarian embryo pieces in Lu2O3On the spacer, it was sintered with a laser beam having a diameter of 5.2mm at a power of 0.02W/mm2Linear power of 3.3W/mm2And the maximum power is kept for 85s, the scanning speed is 10mm/s, and the time of full laser sintering is 7 min. In this process, the two sides of the biscuit sheet are sintered simultaneously. Finally, grinding and polishing the ceramic biscuit to 2mm to obtain Tb: Lu2O3A transparent ceramic.
FIG. 1 is an XRD pattern of a ceramic sample, which can be seen as Lu2O3The phase has no other impurity phase, and the ceramic has higher purity. The ceramic crystal grain size is 2 μm, the optical transmittance is 80.7% at 400nm, the optical quality is good, and the green light output of 550nm can be realized under the excitation of 323nm light.
Example 3: (Lu)0.98Tb0.02)2O3Transparent ceramics
According to (Lu)0.98Tb0.02)2O3Lu (NO) is weighed according to the stoichiometric ratio of each element3)3·6H2O and TbCl3·6H2Taking O powder as a reaction raw material;
diluting citric acid with distilled water to a concentration of 0.2g/ml, adding citric acid and glycol solution (the molar ratio of metal ions to citric acid is 0.5, and the mass ratio of citric acid to glycol is 2) into the mixed raw materials, and uniformly stirring to obtain a precursor solution;
heating the precursor solution to 80 ℃, preserving heat for 24h to remove redundant water, cooling to room temperature, and then placing the precursor solution in a mortar for grinding to obtain precursor powder; and then pre-calcining the ground precursor powder at 800 ℃ for 7h to remove redundant organic matters, and then placing the pre-calcined precursor powder in a muffle furnace to calcine at 1200 ℃ for 3 h.
Adding 0.2g/ml of polyvinyl alcohol (with polymerization degree of 1600-1900) solution as an adhesive into the calcined powder for plasticizing, and pressing the powder into a wafer with the diameter of 6.0mm and the thickness of 3.0mm by a dry pressing method under the pressure of 150MPa to obtain the biscuit blank.
Placing the dry pressed vegetarian embryo pieces in Lu2O3On the spacer, the spacer was sintered with a laser beam having a diameter of 5.5mm at a laser power of 0.03W/mm2Linear power ofRise to 3.4W/mm2And the laser is maintained at the maximum power for 100s, the scanning speed is 12mm/s, and the time of full laser sintering is 8 min. In this process, the two sides of the biscuit sheet are sintered simultaneously. Finally, grinding and polishing the ceramic biscuit to 3mm to obtain Tb: Lu2O3A transparent ceramic.
The ceramic sample prepared in this example was Lu2O3The phase has no other impurity phase, and the ceramic has higher purity. The ceramic crystal grain size is 2.8 μm, the optical transmittance is 80.6% at 400nm, the optical quality is good, and the green light output of 550nm can be realized under the excitation of 323nm light.
Claims (7)
1. Preparation of Tb: Lu by laser sintering2O3Method for producing a ceramic, characterized in that it comprises the following steps
(1) According to the chemical structural formula (Lu)1-xTbx)2O3The stoichiometric ratio of the elements in the solution is respectively called Lu containing lutetium ions3+And a compound containing terbium ion Tb3+The powder of the compound (2) is used as a reaction raw material, wherein x is Tb3+Doped Lu3+The mole percentage of the position, x is more than or equal to 0.001 and less than or equal to 0.02;
(2) adding citric acid and glycol solution into the mixed raw material powder, and uniformly stirring to obtain a precursor solution, wherein the molar ratio of metal ions to citric acid is 0.2-0.5, and the mass ratio of citric acid to glycol is 1-2;
(3) carrying out heat treatment on the precursor solution at 70-80 ℃, removing redundant water, cooling to room temperature, and grinding to obtain precursor powder; then placing the ground precursor powder at 500-800 ℃ for pre-calcining for 5-7 h, removing redundant organic matters, and placing the pre-calcined precursor powder at 800-1200 ℃ for calcining for 1-3 h;
(4) adding an adhesive polyvinyl alcohol solution into the calcined powder for plasticizing, and pressing the powder into a round sheet shape by adopting a dry pressing method to obtain a biscuit sheet, wherein the adding amount of the polyvinyl alcohol solution is 1.0-7.0% of the mass of the sheet-pressing powder;
(5) placing the biscuit in a Lu2O3On the gasket, sintering two surfaces of the biscuit sheet simultaneously by using a laser to obtain a ceramic biscuit;
(6) grinding and polishing the sintered ceramic biscuit to 1-3 mm to obtain Tb: Lu2O3A transparent ceramic.
2. Lu Tb prepared by laser sintering according to claim 12O3The method for producing ceramics, wherein in the step (1), the Lu containing lutetium ions3+The compound of (A) is lutetium oxide or lutetium nitrate, and the compound contains terbium ions Tb3+The compound of (1) is one of terbium nitrate, terbium chloride and terbium oxide.
3. Lu Tb prepared by laser sintering according to claim 1 or 22O3The method for preparing the ceramic is characterized in that in the step (4), the concentration of the polyvinyl alcohol solution is 0.05-0.2 g/ml.
4. Lu Tb prepared by laser sintering according to claim 1 or 22O3The method for producing the ceramic is characterized in that in the step (4), the polymerization degree of the polyvinyl alcohol is 1600-1900.
5. Lu Tb prepared by laser sintering according to claim 1 or 22O3The method for preparing the ceramic is characterized in that in the step (4), the pressing pressure is 800-1200 MPa, the diameter of the biscuit sheet is 2.0-6.0 mm, and the thickness of the biscuit sheet is 0.5-3.0 mm.
6. Lu Tb prepared by laser sintering according to claim 1 or 22O3The method for preparing the ceramic is characterized in that in the step (5), the laser output power density is 3.2-3.4W/mm2The beam diameter is 4.9-5.5 mm.
7. Lu Tb prepared by laser sintering according to claim 1 or 22O3The ceramic preparation method is characterized in that in the step (5), the laser scanning speed is 2-12 mm/s.
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| CN111233471A (en) * | 2020-01-29 | 2020-06-05 | 桂林理工大学 | Square tungsten bronze structure Mo3Nb2O14Method for producing materials and use thereof |
| CN112209710A (en) * | 2020-10-17 | 2021-01-12 | 江苏师范大学 | Method for preparing Ce: YAG fluorescent ceramic by laser sintering |
| EP4304857A1 (en) * | 2021-03-12 | 2024-01-17 | Technische Universität Darmstadt | Method and device for producing ceramics and ceramic product |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760157A (en) * | 2005-06-28 | 2006-04-19 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of lutecia based transparent ceramics |
| CN102093054A (en) * | 2010-12-01 | 2011-06-15 | 中国科学院上海光学精密机械研究所 | Faraday magnetic rotation transparent ceramic and preparation method thereof |
| CN104529449A (en) * | 2014-12-18 | 2015-04-22 | 徐州市江苏师范大学激光科技有限公司 | Method for preparing yttrium oxide-based transparent ceramic employing two-step sintering method |
| CN104557012A (en) * | 2014-12-18 | 2015-04-29 | 徐州市江苏师范大学激光科技有限公司 | Preparation method of Pr:LuAG ceramic scintillator |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20110150735A1 (en) * | 2006-11-01 | 2011-06-23 | Lawrence Livermore National Security, Llc. | Fabrication of Transparent Ceramics Using Nanoparticles Synthesized Via Flame Spray Pyrolysis |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760157A (en) * | 2005-06-28 | 2006-04-19 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of lutecia based transparent ceramics |
| CN102093054A (en) * | 2010-12-01 | 2011-06-15 | 中国科学院上海光学精密机械研究所 | Faraday magnetic rotation transparent ceramic and preparation method thereof |
| CN104529449A (en) * | 2014-12-18 | 2015-04-22 | 徐州市江苏师范大学激光科技有限公司 | Method for preparing yttrium oxide-based transparent ceramic employing two-step sintering method |
| CN104557012A (en) * | 2014-12-18 | 2015-04-29 | 徐州市江苏师范大学激光科技有限公司 | Preparation method of Pr:LuAG ceramic scintillator |
Non-Patent Citations (1)
| Title |
|---|
| Lu2O3:Tb,Hf storage phosphor;Dagmara Kulesza et al.;《Radiation Measurements》;20101231;第45卷;第490-492页 * |
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