CN107117969B - Preparation method of yttrium oxide transparent ceramic - Google Patents
Preparation method of yttrium oxide transparent ceramic Download PDFInfo
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Abstract
A preparation method of yttrium oxide transparent ceramic comprises the following steps: (1) dissolving yttrium nitrate hexahydrate in deionized water, and carrying out magnetic stirring; (2) adding a surfactant into the mixed solution obtained in the step (1), and carrying out magnetic stirring to obtain an yttrium nitrate aqueous solution; (3) dissolving ammonium fluoride in deionized water, and magnetically stirring to obtain an ammonium fluoride aqueous solution; (4) dripping the ammonium fluoride aqueous solution obtained in the step (3) into the yttrium nitrate aqueous solution obtained in the step (2), and carrying out magnetic stirring; (5) heating the mixed solution obtained in the step (4) while magnetically stirring, and preserving heat; (6) centrifuging the mixed solution obtained in the step (5) to obtain a filter cake, washing, drying and annealing the filter cake to obtain yttrium fluoride nano powder; (7) and (4) carrying out dry pressing molding on the yttrium fluoride nano powder obtained in the step (6) to prepare a biscuit, and carrying out pressureless sintering in an air atmosphere to obtain the yttrium oxide transparent ceramic. The method has the characteristics of simplicity, easy operation and low cost.
Description
Technical Field
The invention relates to a preparation method of yttrium oxide transparent ceramic.
Background
Yttrium oxide (Y)2O3) Belongs to a cubic crystal system, and has a melting point of 2430 ℃. It is difficult to grow Y due to too high melting point and polycrystalline transformation at high temperature2O3And (3) single crystal. In recent years, with the development of powder sintering technology, low-temperature sintering of transparent ceramics has become possible. At present, a plurality of companies and subject groups at home and abroad successfully prepare Y with high optical quality2O3A transparent ceramic. Y is2O3The ceramic has the advantages of high melting point, good stability, wide light transmission range, high light transmittance, high thermal conductivity, high refractive index, corrosion resistance and the like, and has potential application value in the industries of high-temperature windows, infrared detection, luminescent media and semiconductors.
Y2O3The transparent ceramic was first made by the United states General Electric (GE) method, which uses 90mol% Y2O3And 10mol% ThO2As raw materials, sintering at high temperature (2000-2200 ℃) in a reducing atmosphereAnd (4) preparing the composition. U.S. Pat. No. 5, 3,545,9872 O 32 to 15mol% ThO is doped in the solution2，ZrO2Or HfO2Sintering at high temperature to obtain Y2O3A polycrystalline transparent ceramic. Because the tetravalent ion doped ceramic has negative ion defects, the ceramic is unstable at high temperature and low oxygen partial pressure and is easy to blacken. U.S. Pat. No. 4, 3,873,657,893,893 shows Y obtained by doping with BeO and sintering2O3Transparent polycrystalline ceramics, but BeO is highly toxic. At the end of the last century, Ikegami and Noriko, et al, synthesized Y by liquid phase method2O3Nano-powder and sintering under vacuum to obtain Y2O3Transparent ceramics, the sintering temperature of which is reduced to about 1700 ℃. Chinese patent 200510023376.5 by adding La2O3Preparing La-doped La with good transparency in a reducing atmosphere at a temperature of less than 1800 ℃ as a sintering aid3+Y of (A) is2O3Base transparent polycrystalline ceramics and laser ceramics; chinese patent 201610137851.X adopts YOF micro-nano powder as raw material, and is sintered at high temperature in air atmosphere to obtain semitransparent Y2O3A ceramic; chinese patent 200910195846.4 as commercial high purity Y2O3ZrO from powder2Adding polyacrylate after ball milling as sintering aid, slip casting in mold, and sintering under no pressure in hydrogen or vacuum atmosphere to obtain high optical quality Y2O3The light transmittance at 1100nm of the transparent ceramic reaches 81.3 percent. The traditional process method has the problems of complex process flow, complex operation and high production cost.
Disclosure of Invention
The invention aims to provide a preparation method of yttrium oxide transparent ceramic, which solves the problems of complex process flow, complex operation and high production cost of the traditional process method.
The technical scheme adopted for realizing the aim is that the preparation method of the yttrium oxide transparent ceramic comprises the following steps:
(1) dissolving yttrium nitrate hexahydrate in deionized water, and carrying out magnetic stirring for 10-30 min;
(2) adding a surfactant into the mixed solution obtained in the step (1), and carrying out magnetic stirring for 10-30 min to obtain an yttrium nitrate aqueous solution;
(3) dissolving ammonium fluoride in deionized water, and performing magnetic stirring for 10-30 min to obtain an ammonium fluoride aqueous solution;
(4) dripping the ammonium fluoride aqueous solution obtained in the step (3) into the yttrium nitrate aqueous solution obtained in the step (2), and carrying out magnetic stirring for 10-30 min;
(5) heating the mixed solution obtained in the step (4) while magnetically stirring, and preserving heat, wherein the heating temperature is 50-90 ℃, and the preserving heat time is 1-3 h;
(6) centrifuging the mixed solution obtained in the step (5) to obtain a filter cake, washing, drying and annealing the filter cake to obtain yttrium fluoride nano powder, wherein the drying temperature is 80-120 ℃, the drying time is 5-24 hours, the annealing temperature is 500-700 ℃, and the annealing time is 1-3 hours;
(7) and (3) carrying out dry pressing molding on the yttrium fluoride nano powder obtained in the step (6) for 5-30 min at the pressure of 50-80 MPa to prepare a biscuit, and carrying out pressureless sintering at 900 ℃, 1100 ℃ and 1650 ℃ in an air atmosphere for 5h, 5h and 20h respectively to obtain the yttrium oxide transparent ceramic.
Advantageous effects
Compared with the prior art, the invention has the following advantages.
The method for preparing the transparent yttria ceramic comprises the steps of reacting yttrium nitrate hexahydrate and ammonium fluoride serving as raw materials to obtain yttrium fluoride nano powder, and then carrying out dry pressing on the yttrium fluoride nano powder to form a biscuit, wherein a step-by-step pressureless sintering process is adopted during sintering, the yttrium fluoride reacts with oxygen in the air during low-temperature sintering to generate yttrium oxyfluoride firstly, and then the yttrium oxide is generated; the ceramic blank is further densified through high-temperature sintering, the transmittance is further improved, and the obtained yttrium oxide transparent ceramic has high density and good transmittance; the preparation method of the transparent yttria ceramic provided by the invention has the advantages of simple process flow, low cost and easiness in operation, and is suitable for industrial production.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings.
FIG. 1 is a view of a transparent yttria ceramic obtained in example 1 of the present invention.
FIG. 2 is a view of the transparent yttria ceramic obtained in example 2 of the present invention.
Detailed Description
A preparation method of yttrium oxide transparent ceramic comprises the following steps:
(1) dissolving yttrium nitrate hexahydrate in deionized water, and carrying out magnetic stirring for 10-30 min;
(2) adding a surfactant into the mixed solution obtained in the step (1), and carrying out magnetic stirring for 10-30 min to obtain an yttrium nitrate aqueous solution;
(3) dissolving ammonium fluoride in deionized water, and performing magnetic stirring for 10-30 min to obtain an ammonium fluoride aqueous solution;
(4) dripping the ammonium fluoride aqueous solution obtained in the step (3) into the yttrium nitrate aqueous solution obtained in the step (2), and carrying out magnetic stirring for 10-30 min;
(5) heating the mixed solution obtained in the step (4) while magnetically stirring, and preserving heat, wherein the heating temperature is 50-90 ℃, and the preserving heat time is 1-3 h;
(6) centrifuging the mixed solution obtained in the step (5) to obtain a filter cake, washing, drying and annealing the filter cake to obtain yttrium fluoride nano powder, wherein the drying temperature is 80-120 ℃, the drying time is 5-24 hours, the annealing temperature is 500-700 ℃, and the annealing time is 1-3 hours;
(7) and (3) carrying out dry pressing molding on the yttrium fluoride nano powder obtained in the step (6) for 5-30 min at the pressure of 50-80 MPa to prepare a biscuit, and carrying out pressureless sintering at 900 ℃, 1100 ℃ and 1650 ℃ in an air atmosphere for 5h, 5h and 20h respectively to obtain the yttrium oxide transparent ceramic.
Example 1
A preparation method of yttria transparent ceramics comprises the following steps:
(1) putting 3.83g of yttrium nitrate hexahydrate in 80mL of deionized water, magnetically stirring, after completely dissolving, adding 1.80g of polyvinylpyrrolidone into the solution, and magnetically stirring for 30min to obtain an yttrium nitrate mixed aqueous solution;
(2) dissolving 1.48g of ammonium fluoride in 20mL of deionized water, and magnetically stirring for 30min to obtain an ammonium fluoride aqueous solution;
(3) dripping the ammonium fluoride aqueous solution obtained in the step (2) into the yttrium nitrate aqueous solution obtained in the step (1), and carrying out magnetic stirring for 10 min;
(4) heating the mixed solution obtained in the step (3) to 80 ℃ while magnetically stirring, and preserving heat for 2 hours;
(5) centrifuging the mixed solution obtained in the step (4) to obtain a filter cake, washing the filter cake with water and absolute ethyl alcohol for 2 times respectively, then placing the filter cake in an electrothermal drying oven at 100 ℃ for drying for 12 hours, and then annealing the filter cake in a muffle furnace at 600 ℃ for 3 hours to obtain yttrium fluoride nano powder;
(6) performing dry pressing molding on the yttrium fluoride nano powder obtained in the step (5) at 60MPa, and maintaining the pressure for 5min to prepare a ceramic biscuit;
(7) and (4) respectively sintering the ceramic biscuit obtained in the step (6) for 5h, 5h and 20h at 900 ℃, 1100 ℃ and 1650 ℃ in an air atmosphere to obtain the yttrium oxide transparent ceramic.
As can be seen from fig. 1, the character "Y2O3" after the ceramic sheet is seen through the transparent yttria ceramic sheet indicates that the ceramic sheet has high transmittance and high density.
Example 2
A preparation method of yttria transparent ceramics comprises the following steps:
(1) putting 3.83g of yttrium nitrate hexahydrate in 80mL of deionized water, magnetically stirring, after completely dissolving, adding 1.80g of polyvinylpyrrolidone into the solution, and magnetically stirring for 30min to obtain an yttrium nitrate mixed aqueous solution;
(2) dissolving 1.48g of ammonium fluoride in 20mL of deionized water, and magnetically stirring for 30min to obtain an ammonium fluoride aqueous solution;
(3) dripping the ammonium fluoride aqueous solution obtained in the step (2) into the yttrium nitrate aqueous solution obtained in the step (1), and carrying out magnetic stirring for 10 min;
(4) heating the mixed solution obtained in the step (3) to 80 ℃ while magnetically stirring, and preserving heat for 2 hours;
(5) centrifuging the mixed solution obtained in the step (4) to obtain a filter cake, washing the filter cake with water and absolute ethyl alcohol for 2 times respectively, then placing the filter cake in an electrothermal drying oven at 100 ℃ for drying for 12 hours, and then annealing the filter cake in a muffle furnace at 600 ℃ for 3 hours to obtain yttrium fluoride nano powder;
(6) performing dry pressing molding on the yttrium fluoride nano powder obtained in the step (5) at 60MPa, and maintaining the pressure for 30min to prepare a ceramic biscuit;
(7) and (4) respectively sintering the ceramic biscuit obtained in the step (6) for 5h, 5h and 20h at 900 ℃, 1100 ℃ and 1650 ℃ in an air atmosphere to obtain the yttrium oxide transparent ceramic.
As can be seen from fig. 2, the character "Y2O3" after the ceramic sheet was seen through the transparent ceramic yttria sheet and was more clearly seen than the ceramic sheet obtained in example 1, indicating that the ceramic sheet obtained in example 2 had better light transmittance.
Claims (1)
1. A preparation method of transparent yttria ceramics is characterized by comprising the following steps:
(1) dissolving yttrium nitrate hexahydrate in deionized water, and carrying out magnetic stirring for 10-30 min;
(2) adding a surfactant into the mixed solution obtained in the step (1), and carrying out magnetic stirring for 10-30 min to obtain an yttrium nitrate aqueous solution;
(3) dissolving ammonium fluoride in deionized water, and performing magnetic stirring for 10-30 min to obtain an ammonium fluoride aqueous solution;
(4) dripping the ammonium fluoride aqueous solution obtained in the step (3) into the yttrium nitrate aqueous solution obtained in the step (2), and carrying out magnetic stirring for 10-30 min;
(5) heating the mixed solution obtained in the step (4) while magnetically stirring, and preserving heat, wherein the heating temperature is 50-90 ℃, and the preserving heat time is 1-3 h;
(6) centrifuging the mixed solution obtained in the step (5) to obtain a filter cake, washing, drying and annealing the filter cake to obtain yttrium fluoride nano powder, wherein the drying temperature is 80-120 ℃, the drying time is 5-24 hours, the annealing temperature is 500-700 ℃, and the annealing time is 1-3 hours;
(7) and (3) carrying out dry pressing molding on the yttrium fluoride nano powder obtained in the step (6) for 5-30 min at the pressure of 50-80 MPa to prepare a biscuit, and carrying out pressureless sintering at 900 ℃, 1100 ℃ and 1650 ℃ in an air atmosphere for 5h, 5h and 20h respectively to obtain the yttrium oxide transparent ceramic.
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| CN108163882A (en) * | 2018-01-09 | 2018-06-15 | 江苏师范大学 | A kind of method that yttrium oxide powder and crystalline ceramics are prepared using composite dispersing agent |
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