CN111253154A - Method for preparing rod-like transparent ceramic with YAG-based core-shell structure by gel casting - Google Patents
Method for preparing rod-like transparent ceramic with YAG-based core-shell structure by gel casting Download PDFInfo
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Abstract
The invention discloses a method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting, which comprises the steps of mixing a monomer, a cross-linking agent, a dispersing agent, a pH regulator and deionized water to prepare a premixed solution; adding Re YAG ceramic powder into the premixed liquid to prepare water-based ceramic slurry, and then carrying out ball milling; adding a catalyst into the ball-milled ceramic slurry, removing bubbles in vacuum, adding an initiator, and performing ultrasonic stirring; injecting the ceramic slurry into a cylindrical glass tube mold, curing the gel, and demolding; putting a Re: YAG biscuit serving as a core into a cylindrical glass mold, injecting pure YAG slurry around the core, and carrying out gel forming on YAG/Re: YAG; drying the demolded biscuit with the composite structure in a constant temperature and humidity box; calcining, and finally vacuum sintering to obtain the core-shell structure YAG/Re: YAG transparent ceramic. The YAG-based core-shell structure rod-shaped transparent ceramic prepared by the invention has the advantages of green and environment-friendly water-based slurry, simple process, high efficiency, good quality of formed biscuit, uniform and high density of the biscuit, and is very suitable for preparing large-size composite structure YAG transparent ceramic materials.
Description
Technical Field
The invention relates to the technical field of transparent ceramic preparation, in particular to a method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting.
Background
The high-performance laser gain material is the core and the foundation of the development and the application of the laser technology, and the transparent laser ceramic is widely concerned at home and abroad as a new-generation laser material after laser crystal and glass. The laser ceramic is used as a gain medium of a solid laser, has the advantages of high doping concentration, excellent optical property, high thermal conductivity, high damage threshold, high laser output efficiency, good thermal shock resistance, easy manufacture, low cost, large size, mass production, strong structure designability and the like, and plays an important role in the field of solid lasers. In 1995, Ikesue et al prepared Nd: YAG transparent ceramics by solid phase reaction and obtained laser output for the first time, and then, research on the application of YAG transparent ceramics doped with other rare earth ions such as Yb, Er, Ho, Tm, etc. to generation of various laser wavelengths and to solid laser has attracted much attention and research.
Although YAG ceramics and sesquioxide transparent ceramics have higher thermal conductivity, the thermal conductivity of ceramics decreases as the doping concentration increases. Therefore, for a transparent ceramic gain medium with a single structure, particularly a high-doped medium and a large-size medium, a serious thermal effect problem exists in the laser operation process, and the problems of optical distortion, limited output power, easy mechanical damage, light beam quality reduction caused by thermal lens effect and the like can occur in long-time work, so that the laser performance is reduced, and the laser output power and the efficiency of the solid laser are limited. Thermal management is effectively achieved by bonding pure YAG or other high thermal conductivity materials around the gain medium to form a composite structure transparent ceramic. The traditional dry pressing method can only prepare small-size and simple-shape ceramics and cannot meet the technological requirements of composite structure ceramic forming, and a series of problems of high preparation cost, poor optical quality, poor structural integrity, general heat effect control capability and the like exist in a thermal bonding method, a plasma spraying method, a heating die pressing method, a laser cladding method, a magnetron sputtering method and the like. In recent years, tape casting and slip casting have made great progress in preparing composite structure transparent ceramics, and the thermal management of laser ceramics is improved, but because the density of a biscuit needs further isostatic pressing treatment, additional process procedures are added, the requirement on equipment is high, and the production cost is increased.
Disclosure of Invention
The invention aims to provide a method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting, which has the advantages of low equipment cost, simple process, good forming effect, high biscuit strength and high density.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting.
(1) Mixing monomer acrylamide, cross-linking agent N, N' -methylene bisacrylamide, dispersant ammonium citrate, pH regulator tetramethyl ammonium hydroxide and deionized water according to a certain proportion to prepare a premixed solution;
(2) adding the Re YAG ceramic powder into the premixed liquid to prepare water-based Re YAG ceramic slurry with the solid content of 48-50 vol%, and then carrying out ball milling for 4-6 h at the ball milling rotation speed of 150-180 r/min;
(3) adding a catalyst tetramethylethylenediamine solution into the ball-milled ceramic slurry, removing bubbles in vacuum for 5-10 min, adding an initiator ammonium persulfate solution, and ultrasonically stirring for 1-3 min;
(4) injecting the ceramic slurry obtained in the step (3) into a cylindrical glass tube mold, curing the gel for 12-20 h, and then demolding to obtain a Re: YAG biscuit;
(5) putting the demoulded Re: YAG biscuit serving as a core into a cylindrical glass mould, injecting pure YAG ceramic slurry with the solid content of 50-52 vol% around the core, wherein the pure YAG ceramic slurry is prepared in the same way as the Re: YAG ceramic slurry, the acrylamide monomer content in the pure YAG slurry is 2-3 wt%, and the gel forming YAG/Re: YAG is carried out;
(6) and (3) drying the demolded biscuit with the composite structure in a constant temperature and humidity box at 30-40 ℃ for 10-15 hours, and then heating to 50-60 ℃ for drying for 10-20 hours.
(7) And placing the dried biscuit with the composite structure in an air atmosphere, calcining for 6-8 h at 360-380 ℃, heating to 600-900 ℃, calcining for 4-6 h, and finally placing the biscuit in a vacuum furnace at 1700-1780 ℃ for sintering for 8-20 h to obtain the YAG/Re: YAG transparent ceramic with the core-shell structure.
Preferably, the chemical general formula of the Re: YAG ceramic powder is (Y)1-xRex)3Al5O12Re is one of rare earth elements of cerium, praseodymium, neodymium, samarium, europium, terbium, dysprosium, holmium, erbium, thulium or ytterbium, and x ranges from 0.001 to 0.15.
Preferably, in the step (1), the monomer content is 1.0-1.5 wt% of the ceramic powder, the cross-linking agent content is 0.1-0.15 wt% of the ceramic powder, the dispersing agent content is 0.2-0.6 wt% of the ceramic powder, and the pH regulator content is 1.0-2.0 wt% of the ceramic powder.
Preferably, in the step (3), the mass fraction of the tetramethylethylenediamine solution is 5 to 10%, the addition amount of the tetramethylethylenediamine solution is 0.2 to 0.5 vol%, the mass fraction of the ammonium persulfate solution is 20 to 30%, and the addition amount of the ammonium persulfate solution is 0.5 to 1.0 vol%.
Preferably, in the step (6), the humidity is 80-90% RH at the drying temperature of 30-40 ℃ and 30-40% RH at the drying temperature of 50-60 ℃.
Preferably, in the step (7), the temperature rise rate of calcination in air is 0.5-2 ℃/min to 360-380 ℃, and 5-10 ℃/min to 600-900 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. the YAG-based transparent ceramic with the core-shell structure is prepared by adopting a gel casting process, the process is simple, and the compact and deformation-free sintering can be realized without cold isostatic pressing treatment.
2. The drying is improved by controlling the solid contents of the two types of slurry of the core shell, the solid content of the slurry of the core shell is lower than that of the slurry of the shell, the diffusion of water in the shell towards the core is inhibited by the concentration difference of the water content, the biscuit is dry and has no deformation, the homogeneity of the biscuit with the composite structure is improved by regulating and controlling the microstructure of gel content, and meanwhile, the solid contents of the two types of slurry are very high, and the sintering is not required to be worried to.
Drawings
FIG. 1 is a schematic view of the core-shell structure of YAG-based transparent ceramics prepared by the present invention.
FIG. 2 is a microstructure of a core-shell structured biscuit in example 1: (a) YAG, (b) Yb: YAG.
FIG. 3 is a microscopic pore size distribution of the biscuit of example 1.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
A method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting comprises the following steps:
(1) mixing 1.2 wt% of monomer acrylamide, 0.12 wt% of cross-linking agent N, N' -methylene bisacrylamide, 0.4 wt% of dispersing agent ammonium citrate, 1.5 wt% of pH regulator tetramethylammonium hydroxide and deionized water to prepare a premixed solution;
(2) YAG powder with the concentration of 1 at% Yb is added into the premixed liquid to prepare ceramic slurry with the solid content of 49 vol%, and then ball milling is carried out for 5 hours at the ball milling rotating speed of 160 r/min;
(3) adding a tetramethylethylenediamine solution with the mass fraction of 8% and 0.5 vol% of a catalyst into the ball-milled ceramic slurry, then carrying out vacuum defoaming for 8min, adding an ammonium persulfate solution with the mass fraction of 15% and 0.5 vol% of an initiator, and carrying out ultrasonic stirring for 2 min;
(4) injecting the ceramic slurry obtained in the step (3) into a cylindrical glass tube mold with the inner diameter of 10mm, curing the gel for 15h, and then demolding to obtain a Re: YAG biscuit;
(5) placing the demoulded Re: YAG biscuit serving as a core into a cylindrical glass mould with the inner diameter of 20mm, and injecting pure YAG slurry with the solid content of 51 vol% around the core, wherein the pure YAG ceramic slurry is prepared in the same way as the Re: YAG ceramic slurry, the monomer content in the pure YAG slurry is 2.5 wt%, and the gel forming is carried out on YAG/Yb: YAG;
(6) drying the demolded biscuit with the composite structure in a constant-temperature constant-humidity box at 35 ℃ and 85% RH for 10-15 h, and then heating to 55 ℃ and drying at 35% RH for 15 h;
(7) and (2) placing the dried biscuit with the composite structure in an air atmosphere, heating to 370 ℃ at 1 ℃/min, calcining for 7h, heating to 720 ℃ at 7 ℃/min, calcining for 5h, and finally placing the biscuit in a vacuum furnace, sintering for 12h at 1750 ℃ to obtain the core-shell structure YAG/Re: YAG transparent ceramic, wherein the structural schematic diagram is shown in figure 1, the inner core part is Yb: YAG ceramic, and the outer shell part is YAG ceramic.
As shown in FIG. 2, FIG. 2(a) shows the microstructure of an external YAG biscuit after binder removal, FIG. 2(b) shows the microstructure of a core Yb: YAG biscuit after binder removal, and the microstructure of the external biscuit and the core biscuit is uniform and compact without obvious difference.
As shown in figure 3, the micro pore size of the core biscuit prepared by the invention is about 80nm, the micro pore size of the shell biscuit is about 70nm, the compactness is close, the pore sizes of the inner biscuit and the outer biscuit are both in unimodal distribution, and the structure is uniform.
Example 2
A method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting comprises the following steps:
(1) mixing 1.0 wt% of monomer acrylamide, 0.1 wt% of cross-linking agent N, N' -methylene bisacrylamide, 0.2 wt% of dispersing agent ammonium citrate, 1.0 wt% of pH regulator tetramethylammonium hydroxide and deionized water to prepare a premixed solution;
(2) adding 0.1 at% of Ce: YAG powder into the premixed liquid to prepare ceramic slurry with the solid content of 48 vol%, and then carrying out ball milling for 4h at the ball milling rotating speed of 150 r/min;
(3) adding a tetramethylethylenediamine solution with the mass fraction of 5% and 0.3 vol% of a catalyst into the ball-milled ceramic slurry, then carrying out vacuum defoaming for 5min, adding an ammonium persulfate solution with the mass fraction of 20% and 0.7 vol% of an initiator, and carrying out ultrasonic stirring for 1 min;
(4) injecting the ceramic slurry obtained in the step (3) into a cylindrical glass tube mold with the inner diameter of 10mm, curing the gel for 12 hours, and then demolding to obtain a Ce: YAG biscuit;
(5) placing the demolded Ce: YAG biscuit serving as a core into a cylindrical glass mold with the inner diameter of 20mm, injecting pure YAG slurry with the solid content of 50 vol% around the core, wherein the pure YAG ceramic slurry is prepared in the same way as the Ce: YAG ceramic slurry, the monomer content in the pure YAG slurry is 2 wt%, and performing gel molding on YAG/Ce: YAG;
(6) drying the demolded biscuit with the composite structure in a constant temperature and humidity box at 30 ℃ and at the humidity of 80% RH for 10h, and then heating to 50 ℃ and at the humidity of 30% RH for 10 h;
(7) and placing the dried biscuit with the composite structure in an air atmosphere, heating to 360 ℃ at a speed of 0.5 ℃/min, calcining for 6h, heating to 600 ℃ at a speed of 5 ℃/min, calcining for 4h, and finally placing the biscuit in a vacuum furnace, sintering for 20h at a temperature of 1700 ℃ to obtain the YAG/Ce: YAG transparent ceramic with the core-shell structure.
Example 3
A method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting comprises the following steps:
(1) mixing 1.5 wt% of monomer acrylamide, 0.15 wt% of cross-linking agent N, N' -methylene bisacrylamide, 0.6 wt% of dispersing agent ammonium citrate, 2.0 wt% of pH regulator tetramethylammonium hydroxide and deionized water to prepare a premixed solution;
(2) adding 15 at% Yb: YAG powder into the premixed liquid to prepare ceramic slurry with the solid content of 50 vol%, and then carrying out ball milling for 6 hours at the ball milling rotating speed of 180 r/min;
(3) adding a tetramethylethylenediamine solution with the mass fraction of 10% and 0.2 vol% of a catalyst into the ball-milled ceramic slurry, then carrying out vacuum defoaming for 10min, adding an ammonium persulfate solution with the mass fraction of 30% and 1.0 vol% of an initiator, and carrying out ultrasonic stirring for 3 min;
(4) pouring the ceramic slurry obtained in the step (3) into a cylindrical glass tube mold with the inner diameter of 10mm, curing the gel for 20 hours, and then demolding to obtain a Yb: YAG biscuit;
(5) placing the demolded Yb: YAG biscuit serving as a core into a cylindrical glass mold with the inner diameter of 20mm, and injecting pure YAG slurry with the solid content of 52 vol% around the core, wherein the pure YAG ceramic slurry is prepared in the same way as the Re: YAG ceramic slurry, the monomer content of the pure YAG slurry is 3 wt%, and the YAG/Yb: YAG is formed by gel molding;
(6) drying the demolded biscuit with the composite structure in a constant temperature and humidity box at 40 ℃ and the humidity of 90% RH for 15h, and then heating to 60 ℃ and drying at the humidity of 40% RH for 20 h;
(7) and placing the dried biscuit with the composite structure in an air atmosphere, heating to 380 ℃ at a speed of 2 ℃/min, calcining for 8h, heating to 900 ℃ at a speed of 10 ℃/min, calcining for 6h, and finally placing the biscuit in a vacuum furnace, sintering for 8h at a temperature of 1780 ℃ to obtain the YAG/Yb: YAG transparent ceramic with the core-shell structure.
Claims (6)
1. A method for preparing a rod-shaped transparent ceramic with a YAG-based core-shell structure by gel casting is characterized by comprising the following steps:
(1) mixing monomer acrylamide, cross-linking agent N, N' -methylene bisacrylamide, dispersant ammonium citrate, pH regulator tetramethyl ammonium hydroxide and deionized water according to a certain proportion to prepare a premixed solution;
(2) adding the Re YAG ceramic powder into the premixed liquid to prepare water-based Re YAG ceramic slurry with the solid content of 48-50 vol%, and then carrying out ball milling for 4-6 h at the ball milling rotation speed of 150-180 r/min;
(3) adding a catalyst tetramethylethylenediamine solution into the ball-milled ceramic slurry, removing bubbles in vacuum for 5-10 min, adding an initiator ammonium persulfate solution, and ultrasonically stirring for 1-3 min;
(4) injecting the ceramic slurry obtained in the step (3) into a cylindrical glass tube mold, curing the gel for 12-20 h, and then demolding to obtain a Re: YAG biscuit;
(5) putting the demoulded Re: YAG biscuit serving as a core into a cylindrical glass mould, injecting pure YAG ceramic slurry with the solid content of 50-52 vol% around the core, wherein the pure YAG ceramic slurry is prepared in the same way as the Re: YAG ceramic slurry, the acrylamide monomer content in the pure YAG slurry is 2-3 wt%, and the gel forming YAG/Re: YAG is carried out;
(6) and (3) drying the demolded biscuit with the composite structure in a constant temperature and humidity box at 30-40 ℃ for 10-15 hours, and then heating to 50-60 ℃ for drying for 10-20 hours.
(7) And placing the dried biscuit with the composite structure in an air atmosphere, calcining for 6-8 h at 360-380 ℃, heating to 600-900 ℃, calcining for 4-6 h, and finally placing the biscuit in a vacuum furnace at 1700-1780 ℃ for sintering for 8-20 h to obtain the YAG/Re: YAG transparent ceramic with the core-shell structure.
2. The method for preparing the rod-shaped transparent ceramic with the YAG-based core-shell structure by the gel casting as claimed in claim 1, wherein the chemical formula of the Re: YAG ceramic powder is (Y)1-xRex)3Al5O12Re is one of rare earth elements of cerium, praseodymium, neodymium, samarium, europium, terbium, dysprosium, holmium, erbium, thulium or ytterbium, and x ranges from 0.001 to 0.15.
3. The method for preparing the YAG-based core-shell structure rod-shaped transparent ceramic by gel casting according to claim 1, wherein in the step (1), the monomer content is 1.0-1.5 wt% of the ceramic powder, the cross-linking agent content is 0.1-0.15 wt% of the ceramic powder, the dispersing agent content is 0.2-0.6 wt% of the ceramic powder, and the pH regulator content is 1.0-2.0 wt% of the ceramic powder.
4. The method for preparing the YAG-based core-shell structure rod-shaped transparent ceramic by gel injection molding according to claim 1, wherein in the step (3), the mass fraction of the tetramethylethylenediamine solution is 5-10%, the addition amount of the tetramethylethylenediamine solution is 0.2-0.5 vol%, the mass fraction of the ammonium persulfate solution is 20-30%, and the addition amount of the ammonium persulfate solution is 0.5-1.0 vol%.
5. The method for preparing the rod-shaped transparent ceramic with the YAG-based core-shell structure by gel casting according to claim 1, wherein in the step (6), the humidity is 80-90% RH at the temperature of 30-40 ℃ and 30-40% RH at the temperature of 50-60 ℃ in drying.
6. The method for preparing the rod-shaped transparent ceramic with the YAG-based core-shell structure by the gel casting as claimed in claim 1, wherein in the step (7), the temperature rise rate of calcination in air is 0.5-2 ℃/min to 360-380 ℃ and 5-10 ℃/min to 600-900 ℃.
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| CN112299828A (en) * | 2020-11-09 | 2021-02-02 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of transparent ceramic back plate applied to 5G solar mobile phone |
| CN112341184A (en) * | 2020-11-09 | 2021-02-09 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of waveguide structure laser transparent ceramic optical fiber based on Isobam gel state dip-coating technology |
| CN112851331A (en) * | 2021-02-08 | 2021-05-28 | 新沂市锡沂高新材料产业技术研究院有限公司 | Industrial production method of YAG-based transparent ceramic |
| CN113149631A (en) * | 2021-01-20 | 2021-07-23 | 江苏师范大学 | Method for preparing YAG transparent ceramic by colloidal state curing molding |
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