CN110790571A - Preparation of Gd2Zr2O7Method for making transparent ceramics - Google Patents
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Abstract
The invention discloses a method for preparing Gd2Zr2O7The invention relates to a method for preparing transparent ceramics, which adopts a conventional muffle furnace, carries out sintering in air atmosphere, and then carries out hot isostatic pressing post-treatment to realize Gd2Zr2O7The transparent ceramic is prepared and has high optical transmittance. The method adopts the conventional muffle furnace to sinter in the air atmosphere and then carries out the hot isostatic pressing post-treatment, the operation flow is simple, the sintering cost of the conventional muffle furnace in the air atmosphere is low, the method is suitable for popularization and application, and the prepared Gd2Zr2O7The transparent ceramic has high transmittance.
Description
The technical field is as follows:
the invention relates to the field of ceramic materials, in particular to a method for preparing Gd2Zr2O7A method of making a transparent ceramic.
Background art:
Gd2Zr2O7the transparent ceramic is a cubic crystal material with isotropic optical properties, so that the powder particles can be densified by a ceramic sintering methodAnd (4) carrying out chemical arrangement and stacking to prepare a transparent polycrystalline structure. Transparent Gd2Zr2O7The ceramic has excellent optical performance and can be applied to aspects of high-energy physics, medical detection systems and the like.
At present Gd2Zr2O7The transparent ceramic is mainly prepared by methods such as vacuum hot pressing, vacuum sintering and the like. The high-temperature vacuum environment brings many process control problems to the preparation process, the operation process is often very complicated, and the repeatability of the process is inevitably influenced. The invention is to report that the Gd can be realized by adopting a conventional muffle furnace (low cost and strong operability), sintering in the air atmosphere and carrying out hot isostatic pressing post-treatment2Zr2O7The preparation of the transparent ceramic, which has not been reported before, can be Gd2Zr2O7The low-cost preparation of the transparent ceramic provides a new idea and a new breakthrough.
The invention content is as follows:
the invention aims to provide a method for preparing Gd2Zr2O7The method for preparing the transparent ceramic adopts a conventional muffle furnace, sintering is carried out in an air atmosphere, and then the method is subjected to hot isostatic pressing post-treatment, the operation flow is simple, the sintering cost of the conventional muffle furnace in the air atmosphere is low, the method is suitable for popularization and application, and the prepared Gd2Zr2O7The transparent ceramic has high transmittance.
In order to solve the problems, the technical scheme of the invention is as follows:
preparation of Gd2Zr2O7A method of making a transparent ceramic, comprising the steps of:
step one, Gd is used2O3、ZrO2Mixing the powders to obtain mixed powder, adding YF3The powder is a sintering aid, a dispersion medium is added into the mixed powder and the sintering aid, then, the mixture is subjected to ball milling and mixing to obtain slurry, and the slurry is molded to obtain a biscuit A; wherein Gd2O3And ZrO2Is 59.5: 40.5; YF3Mass of powder and Gd2O3、ZrO2The proportion of the total mass of the powder is 0.1-1%; gd (Gd)2O3、ZrO2The mass ratio of the mixed powder to the dispersion medium is 1: 1-4: 1;
step two, placing the biscuit A in a muffle furnace, heating to 1450-1600 ℃ in air atmosphere, preserving heat for 10-20 h, then cooling to 300 ℃, and taking out after natural cooling to obtain ceramic B;
step three, taking the ceramic B, and placing the ceramic B in a hot isostatic pressing furnace using argon as a pressure transmission medium for post-treatment, wherein the method specifically comprises the following steps: heating to 1600-1750 ℃, preserving the heat for 1-5 h, and then slowly cooling to 300 ℃ to obtain ceramic C; polishing the ceramic C to obtain Gd2Zr2O7A transparent ceramic.
In a further improvement, the dispersion medium is pure water or absolute ethyl alcohol.
In a further improvement, when the dispersion medium is absolute ethyl alcohol, in the first step, the biscuit a is formed by a dry method: pouring the slurry into a collecting bottle, vacuumizing to below 1000Pa, heating to 50-70 ℃, and allowing the time to be not less than 3h, so that the absolute ethyl alcohol in the slurry is fully volatilized, and obtaining dry powder; taking the dried powder, grinding the powder, and sieving the powder by a 200-mesh sieve; and taking the sieved powder, carrying out axial dry pressing to 10-30 MPa, and carrying out cold isostatic pressing treatment at 150-300 MPa to obtain a biscuit A.
In the further improvement, when the dispersion medium is pure water, an organic dispersant with the mass fraction of pure water of 0.5 to 2.0 percent is added into the pure water; the first step adopts a slip casting method: pouring the slurry into a porous gypsum mold, standing for 24-48 h at room temperature, taking out after the slurry is solidified, putting the slurry into a muffle furnace, heating to 500-700 ℃, calcining to remove organic matters, and carrying out cold isostatic pressing treatment at 150-300 MPa to obtain a biscuit A.
In a further improvement, the organic dispersant is an organic substance containing polyacrylate ions, preferably one of byk190, byk141 and byk9076 of Picko chemical.
In the third step, in the process of temperature rising and temperature lowering, the speed of temperature rising and temperature lowering is 1-5 ℃/min.
In the step one, slurry is obtained by ball milling and mixing through a planetary ball mill, the ball milling speed is controlled to be 100 r/m-300 r/m, and the ball milling time is 10 h-30 h.
In the third step, the hot isostatic pressing pressure during the heat preservation is 150 MPa-200 MPa.
The invention has the beneficial effects that:
at present Gd2Zr2O7The transparent ceramic is mainly prepared by methods such as vacuum hot pressing, vacuum sintering and the like. The high-temperature vacuum environment brings many process control problems to the preparation process, the operation process is often very complicated, and the repeatability of the process is inevitably influenced. The invention is to report that the Gd can be realized by adopting a conventional muffle furnace, sintering (low cost and strong operability) in an air atmosphere and then carrying out hot isostatic pressing post-treatment2Zr2O7The transparent ceramic is prepared and has high optical transmittance. The method has not been reported before, and can be Gd2Zr2O7A novel method for the low-cost preparation of transparent ceramics is provided.
Description of the drawings:
FIG. 1 is Gd obtained in example 12Zr2O7A transmittance map of the transparent ceramic;
FIG. 2 Gd obtained in example 22Zr2O7A transmittance map of the transparent ceramic;
FIG. 3 Gd obtained in example 32Zr2O7A transmittance map of the transparent ceramic;
FIG. 4 Gd obtained in example 42Zr2O7Transmittance of transparent ceramics.
The specific implementation mode is as follows:
in order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
Preparation of Gd2Zr2O7A method of making a transparent ceramic, comprising the steps of:
step one: weighing Gd2O3、ZrO250 g of YF serving as a raw material3The powder is used as sintering aid for standby. Wherein:
the Gd2O3、ZrO2The mass of the powder is 29.75 g and 20.25 g respectively;
the YF3The mass of the powder is Gd2O3、ZrO20.1 percent of the total mass of the powder (namely 0.05 g);
step two: mixing the three kinds of powder, pouring the mixture into a nylon tank, sequentially adding pure water and a dispersing agent, and performing ball milling and mixing to obtain slurry. Wherein:
the mass ratio of the pure water to the mixed powder is 1: 1 (i.e., 50 grams);
the dispersant was a commercially available byk190 g dispersant, added at 0.5% of the mass of the starting material (i.e., 0.25 g).
The ball milling and mixing refers to a method of planetary ball milling treatment, the ball milling rotating speed is controlled at 100r/m, and the ball milling time is 30 hours.
Step three: and (4) forming by a wet method to prepare a biscuit A. Pouring the slurry into a porous gypsum mold, standing for 48h at room temperature, taking out after the slurry is solidified, putting the slurry into a muffle furnace, heating to 700 ℃, keeping the temperature for 10h, calcining to remove residual organic matters, and carrying out cold isostatic pressing treatment at 150MPa to obtain a biscuit A.
Step four: and (3) placing the biscuit A in a muffle furnace, heating to 1600 ℃ in the air atmosphere, preserving the heat for 10 hours, slowly cooling to 300 ℃, and taking out after natural cooling to obtain the ceramic B.
In the process of temperature rising and reducing, the speed is 5 ℃/min.
Step five: placing the ceramic B in a hot isostatic pressing furnace using argon as a pressure transmission medium, heating to 1750 ℃, preserving heat for 1h for post-treatment, slowly cooling to 300 ℃ to obtain ceramic C, and polishing to 1mm thick to obtain Gd2Zr2O7A transparent ceramic.
In the process of temperature rising and reducing, the speed is 15 ℃/min.
The hot isostatic pressure during the heat preservation period is 150 MPa.
Example 2:
preparation of Gd2Zr2O7A method of making a transparent ceramic, comprising the steps of:
the method comprises the following steps: weighing Gd2O3、ZrO250 g of YF serving as a raw material3The powder is used as sintering aid for standby. Wherein:
the Gd2O3、ZrO2The mass of the powder is 29.75 g and 20.25 g respectively;
the YF3The mass of the powder is Gd2O3、ZrO20.2 percent (namely 0.10 g) of the total mass of the powder;
step two: mixing the three kinds of powder, pouring the mixture into a nylon tank, sequentially adding pure water and a dispersing agent, and performing ball milling and mixing to obtain slurry. Wherein:
the mass ratio of the pure water to the mixed powder is 2: 1 (i.e., 100 grams);
the dispersant was a commercially available byk190 g dispersant, added at 0.5% of the mass of the starting material (i.e., 0.25 g).
The ball milling and mixing refers to a method of planetary ball milling treatment, the ball milling rotating speed is controlled to be 300r/m, and the ball milling time is 10 hours.
Step three: and (4) forming by a wet method to prepare a biscuit A. Pouring the slurry into a porous gypsum mold, standing for 24h at room temperature, taking out after the slurry is solidified, putting the slurry into a muffle furnace, heating to 500 ℃, keeping the temperature for 15h, calcining to remove residual organic matters, and carrying out cold isostatic pressing treatment at 300MPa to obtain a biscuit A.
Step four: and (3) placing the biscuit A in a muffle furnace, heating to 1450 ℃ in the air atmosphere, preserving the heat for 10 hours, slowly cooling to 300 ℃, naturally cooling, and taking out to obtain the ceramic B.
In the process of temperature rising and reducing, the speed is 1 ℃/min.
Step five: placing the ceramic B in a hot isostatic pressing furnace using argon as a pressure transmission medium, heating to 1600 ℃, preserving heat for 5h for post-treatment, slowly cooling to 300 ℃ to obtain ceramic C, and polishing to 1mm thick to obtain Gd2Zr2O7A transparent ceramic.
In the process of temperature rising and reducing, the speed is 5 ℃/min.
The hot isostatic pressure during the holding period is 170 MPa.
Example 3:
preparation of Gd2Zr2O7A method of making a transparent ceramic, comprising the steps of:
the method comprises the following steps: weighing Gd2O3、ZrO250 g of YF serving as a raw material3The powder is used as sintering aid for standby. Wherein:
the Gd2O3、ZrO2The mass of the powder is 29.75 g and 20.25 g respectively;
the YF3The mass of the powder is Gd2O3、ZrO20.5 percent (namely 0.25 g) of the total mass of the powder;
step two: mixing the three kinds of powder, pouring the mixture into a nylon tank, adding absolute ethyl alcohol, and performing ball milling and mixing to obtain slurry. Wherein:
the mass ratio of the absolute ethyl alcohol to the mixed powder is 2: 1 (i.e., 100 grams);
the ball milling and mixing refers to a method of planetary ball milling treatment, the ball milling rotating speed is controlled at 100r/m, and the ball milling time is 30 hours.
Step three: and (4) forming by a dry method to prepare a biscuit A. In particular, this is the case:
pouring the slurry into a collecting bottle, vacuumizing to 500Pa, heating to 50 ℃, and keeping the temperature for 5 hours to obtain dry powder; taking the dried powder, grinding the powder, and sieving the powder by a 200-mesh sieve; and (3) taking the sieved powder, carrying out axial dry pressing to 10MPa, and then carrying out cold isostatic pressing treatment at 300MPa to obtain a biscuit A.
Step four: and (3) placing the biscuit A in a muffle furnace, heating to 1600 ℃ in the air atmosphere, preserving the heat for 10 hours, slowly cooling to 300 ℃, and taking out after natural cooling to obtain the ceramic B.
In the process of temperature rising and reducing, the speed is 5 ℃/min.
Step five: taking ceramic B, placing the ceramic B in a hot isostatic pressing furnace with argon as a pressure transmission mediumHeating to 1750 deg.C, maintaining for 1h, performing post-treatment, slowly cooling to 300 deg.C to obtain ceramic C, polishing to 1mm thickness to obtain Gd2Zr2O7A transparent ceramic.
In the process of temperature rising and reducing, the speed is 15 ℃/min.
The hot isostatic pressure during the heat preservation period is 180 MPa.
Example 4:
preparation of Gd2Zr2O7A method of making a transparent ceramic, comprising the steps of:
the method comprises the following steps: weighing Gd2O3、ZrO250 g of YF serving as a raw material3The powder is used as sintering aid for standby. Wherein:
the Gd2O3、ZrO2The mass of the powder is 29.75 g and 20.25 g respectively;
the YF3The mass of the powder is Gd2O3、ZrO21.0 percent (namely 0.5 g) of the total mass of the powder;
step two: mixing the three kinds of powder, pouring the mixture into a nylon tank, adding absolute ethyl alcohol, and performing ball milling and mixing to obtain slurry. Wherein:
the mass ratio of the absolute ethyl alcohol to the mixed powder is 4: 1 (i.e., 200 grams);
the ball milling and mixing refers to a method of planetary ball milling treatment, the ball milling rotating speed is controlled at 200r/m, and the ball milling time is 20 hours.
Step three: and (4) forming by a dry method to prepare a biscuit A. In particular, this is the case:
pouring the slurry into a collecting bottle, vacuumizing to 800Pa, heating to 65 ℃, and keeping the temperature for 3 hours to obtain dry powder; taking the dried powder, grinding the powder, and sieving the powder by a 200-mesh sieve; and (3) taking the sieved powder, carrying out axial dry pressing to 30MPa, and carrying out cold isostatic pressing treatment at 200MPa to obtain a biscuit A.
Step four: and (3) placing the biscuit A in a muffle furnace, heating to 1700 ℃ in the air atmosphere, preserving the heat for 18h, slowly cooling to 300 ℃, naturally cooling, and taking out to obtain the ceramic B.
In the process of temperature rising and reducing, the speed is 2 ℃/min.
Step five: placing the ceramic B in a hot isostatic pressing furnace using argon as a pressure transmission medium, heating to 1730 ℃, preserving heat for 2h for post-treatment, slowly cooling to 300 ℃ to obtain ceramic C, and polishing to 1mm thick to obtain Gd2Zr2O7A transparent ceramic.
In the process of temperature rising and reducing, the speed is 7 ℃/min.
The hot isostatic pressure during the heat preservation period is 200 MPa.
FIGS. 1 to 4 show Gd prepared in examples 1 to 4, respectively2Zr2O7Transmittance of transparent ceramics.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. Preparation of Gd2Zr2O7A method of making a transparent ceramic, comprising the steps of:
step one, Gd is used2O3、ZrO2Mixing the powders to obtain mixed powder, adding YF3The powder is a sintering aid, a dispersion medium is added into the mixed powder and the sintering aid, and the mixture is ball-milled and mixed to obtain slurry, and then a biscuit A is obtained after molding; wherein, the Gd2O3And ZrO2Is 59.5: 40.5; the YF3Mass of powder and Gd2O3、ZrO2The proportion of the total mass of the powder is 0.1-1%; gd (Gd)2O3、ZrO2The mass ratio of the mixed powder to the dispersion medium is 1: 1-4: 1;
step two, placing the biscuit A in a muffle furnace, heating to 1450-1600 ℃ in air atmosphere, preserving heat for 10-20 h, then cooling to 300 ℃, and taking out after natural cooling to obtain ceramic B;
step three, taking the ceramic B, and placing the ceramic B in argon as a pressure transmission mediumThe post-treatment is carried out in the hot isostatic pressing furnace, and specifically: heating to 1600-1750 ℃, preserving the heat for 1-5 h, and then slowly cooling to 300 ℃ to obtain ceramic C; polishing the ceramic C to obtain Gd2Zr2O7A transparent ceramic.
2. Preparation of Gd according to claim 12Zr2O7The method for preparing the transparent ceramic is characterized in that the dispersion medium is pure water or absolute ethyl alcohol.
3. Preparation of Gd according to claim 22Zr2O7The method for preparing the transparent ceramic is characterized in that when the dispersion medium is absolute ethyl alcohol, in the first step, the biscuit A is formed by a dry method: pouring the slurry into a collecting bottle, vacuumizing to below 1000Pa, heating to 50-70 ℃, and allowing the time to be not less than 3h, so that the absolute ethyl alcohol in the slurry is fully volatilized, and obtaining dry powder; taking the dried powder, grinding the powder, and sieving the powder by a 200-mesh sieve; and taking the sieved powder, carrying out axial dry pressing to 10-30 MPa, and carrying out cold isostatic pressing treatment at 150-300 MPa to obtain a biscuit A.
4. Preparation of Gd according to claim 22Zr2O7The method for preparing the transparent ceramic is characterized in that when the dispersion medium is pure water, an organic dispersant with the mass fraction of pure water of 0.5-2.0 percent is added into the pure water; the first step adopts a slip casting method: pouring the slurry into a porous gypsum mold, standing for 24-48 h at room temperature, taking out after the slurry is solidified, putting the slurry into a muffle furnace, heating to 500-700 ℃, calcining to remove organic matters, and carrying out cold isostatic pressing treatment at 150-300 MPa to obtain a biscuit A.
5. Preparation of Gd according to claim 42Zr2O7The method for preparing the transparent ceramic is characterized in that the organic dispersing agent is organic substance containing polyacrylate ions.
6. The method of claim 5Preparation of Gd2Zr2O7The method for preparing transparent ceramics is characterized in that the organic dispersant is one of byk190, byk141 and byk9076 in Pico chemical.
7. Preparation of Gd according to claim 12Zr2O7The method for preparing the transparent ceramic is characterized in that in the third step, in the process of temperature rising and temperature reduction, the temperature rising and temperature reduction rates are both 1-5 ℃/min.
8. Preparation of Gd according to claim 12Zr2O7The method for preparing the transparent ceramic is characterized in that in the step one, slurry is obtained by ball milling and mixing through a star ball mill, the ball milling rotating speed is controlled to be 100 r/m-300 r/m, and the ball milling time is 10 h-30 h.
9. Preparation of Gd according to claim 12Zr2O7The method for preparing the transparent ceramic is characterized in that in the third step, the hot isostatic pressure during the heat preservation period is 150 MPa-200 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911261178.0A CN110790571A (en) | 2019-12-10 | 2019-12-10 | Preparation of Gd2Zr2O7Method for making transparent ceramics |
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| CN115010503A (en) * | 2022-06-13 | 2022-09-06 | 闽都创新实验室 | Use method of sintering aid for transparent oxide ceramic material |
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