A zirconia ceramic plate which is not fully sintered and a method for manufacturing the same
By preparing incompletely sintered zirconia ceramic plates as gaskets for zirconia electrolyte sheets, the warping and cracking problems of zirconia electrolyte sheets during the sintering process were solved, improving the flatness and performance of the product and reducing costs.
Patent Information
- Application Number
- CN202311254817.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-27
- Publication Date
- 2025-11-28
- Estimated Expiration
- 2043-09-27
AI Technical Summary
In the prior art, during the preparation of alumina ceramic plates and zirconia electrolyte sheets, impurities are easily introduced, leading to cracking and warping, which affects product performance.
Incompletely sintered zirconia ceramic plates are used as gaskets for zirconia electrolyte sheets. By controlling the sintering and debinding parameters, incompletely sintered zirconia ceramic plates are prepared. These plates have loose grains and many pores, which facilitates the debinding of the electrolyte sheets and reduces warpage.
This improved the flatness of the zirconia electrolyte sheet, reduced the introduction of impurity elements, lowered costs, and improved the product's pass rate and performance.
Smart Images

Figure CN117263717B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of ceramic materials, in particular to a not fully sintered zirconia ceramic plate and a preparation method thereof. BACKGROUND
[0002] Solid oxide fuel cell (SOFC) belongs to the third generation fuel cell (the first generation fuel cell (phosphoric acid fuel cell, PAFC), the second generation fuel cell (molten carbonate fuel cell, MCFC), which is a full solid chemical power generation device that can efficiently and environmentally friendly convert chemical energy stored in fuel and oxidant into electric energy at medium-high temperature. It is considered to be widely used in the future as a fuel cell, and the demand for zirconia-based electrolyte sheets as solid oxide fuel cell electrolyte membranes is gradually expanding.
[0003] At present, the production method of zirconia electrolyte sheet is mainly through slurry preparation, then flow casting, and finally sintering to obtain the final zirconia ceramic electrolyte sheet. Because the thickness of the electrolyte sheet is relatively thin, generally about 0.1mm, how to keep it flat and not crack during the sintering process becomes a big problem. The solution to the bending and warping problem during sintering on the market is to cover the green body with a porcelain plate to smooth it. Because the price of aluminum oxide ceramic plate is cheap and the melting point is high, aluminum oxide ceramic plate is often used to smooth it. However, because the aluminum oxide porcelain cover plate presses the green body for sintering, it affects the shrinkage of the product green body, and is easy to crack, and also easy to introduce impurities, affecting the performance of the product.
[0004] In view of this, the present application is proposed. SUMMARY
[0005] The present application aims to overcome the shortcomings of the prior art and provide a not fully sintered zirconia ceramic plate and a preparation method thereof. The not fully sintered zirconia ceramic plate has loose crystal grains and more pores, which is beneficial to the degassing of the electrolyte sheet product and has low warping degree.
[0006] To achieve the above-mentioned purpose, the technical scheme adopted by the present application is as follows:
[0007] A preparation method of a not fully sintered zirconia ceramic plate, comprising the following steps:
[0008] (1) uniformly mix yttria-doped zirconia powder, solvent, dispersant, plasticizer and binder to obtain slurry;
[0009] (2) ball mill and defoam the slurry;
[0010] (3) the defoamed slurry is cast and isostatic pressed to obtain a green body;
[0011] (4) the green body is stacked and de-bindered to obtain a body;
[0012] (5) the body is sintered at 780-820 ℃ for 480-720 min, then sintered at the first temperature for 450-600 min, then sintered at the second temperature for 180-360 min, and finally sintered at 950-1050 ℃ for 180-240 min to obtain a zirconia ceramic plate;
[0013] The first temperature is 1200-1300 ℃, the second temperature is 1200-1300 ℃, and the first temperature is less than the second temperature.
[0014] The zirconia ceramic plate prepared by the method has not been completely sintered, the crystal grains are relatively loose, and there are many holes, which is beneficial to de-binder of the electrolyte sheet product, and the zirconia ceramic plate has good strength and hardness, is not easy to be damaged, is convenient for carrying and storing, and can be repeatedly used, thereby reducing the cost.
[0015] The zirconia ceramic plate is applied to preparation of a SOFC electrolyte sheet, and specifically, the zirconia ceramic plate is used as a gasket for sintering of the SOFC electrolyte sheet (such as the zirconia gasket in CN116573933), so as to solve the problems of warping, bending and cracking of the zirconia electrolyte sheet in the sintering process, improve the qualified rate, save the cost, reduce the introduction of impurity elements, ensure the product performance, and have a wide application prospect.
[0016] The inventor of the present application finds that if the zirconia ceramic plate has been completely sintered in advance, the performance of the zirconia electrolyte sheet is easily affected in the sintering process for preparation of the zirconia electrolyte sheet, and therefore, the zirconia ceramic plate needs to be incompletely sintered.
[0017] The inventor of the present application creatively controls the parameters of sintering and de-binder, effectively controls the warping degree of the zirconia ceramic plate, and enables the zirconia electrolyte sheet to effectively improve the flatness of the zirconia electrolyte sheet when the zirconia electrolyte sheet is prepared, without the need of extremely controlling the number and size of the sintered sheet.
[0018] As a preferred embodiment of the present application, the yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is (2-4):(96-98).
[0019] As a preferred embodiment of the present application, the average particle size of the yttria-doped zirconia powder is 0.5-1 μm.
[0020] As a preferred embodiment of the present application, the solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene and isopropyl alcohol is (2-4):1;
[0021] The dispersant is methyl pentanol;
[0022] The plasticizer is phthalate ester;
[0023] The binder is PVB.
[0024] As a preferred embodiment of the present application, the mass ratio of the yttria-doped zirconia powder, the solvent, the dispersant, the plasticizer, and the binder is 100:(70-90):(2-4):(5-8):(7-12).
[0025] As a preferred embodiment of the present application, the ball milling is specifically performed in a ball milling tank, the ball milling speed is 200-400 rpm, the ball milling time is 18-28 h, the mass ratio of the zirconium ball to the slurry is 1:(1-2) during the ball milling, the zirconium ball comprises zirconium balls with a diameter of 10 mm and zirconium balls with a diameter of 15 mm, and the mass ratio of the zirconium balls with a diameter of 10 mm to the zirconium balls with a diameter of 15 mm is (1-2):1.
[0026] As a preferred embodiment of the present application, the defoaming is performed at a vacuum degree of less than -0.05 MPa, and the defoaming time is 1-3 h.
[0027] As a preferred embodiment of the present application, the casting is performed in a casting machine, and during the casting, the temperature of the oven of the casting machine is divided into two sections, the temperature of the first half section is 30-40℃, and the temperature of the second half section is 50-75℃.
[0028] As a preferred embodiment of the present application, the isostatic pressing pressure is 50-100 MPa, and the time is 30-120 min.
[0029] As a preferred embodiment of the present application, the glue discharging is specifically performed by first discharging glue from the stacked green body at a first temperature of 250-300℃ for 200-400 min, then discharging glue at a third temperature for 180-240 min, and finally discharging glue at a fourth temperature for 180-360 min.
[0030] The third temperature is 350-400℃, the fourth temperature is 350-400℃, and the third temperature is less than the fourth temperature.
[0031] The present application also provides an incompletely sintered zirconia ceramic plate prepared by the above preparation method.
[0032] The beneficial effects of the present application are that (1) the zirconia ceramic plate prepared by the present application is not completely sintered, the crystal grains are relatively loose, there are more pores, which is beneficial to the glue removal of the electrolyte sheet product, and at the same time has good strength and hardness, is not easy to damage, is beneficial to transportation and storage, and can be reused, thereby reducing the cost. (2) The zirconia ceramic plate is applied to prepare SOFC electrolyte sheet, specifically, the zirconia ceramic plate is used as a gasket for sintering of the SOFC electrolyte sheet, to solve the problems of warping, bending, cracking and the like in the sintering process of the zirconia electrolyte sheet, improve the qualified rate, save the cost, at the same time reduce the introduction of impurity elements, ensure the product performance, and have a wide application prospect. BRIEF DESCRIPTION OF DRAWINGS
[0033] Figure 1 The end face electron microscope graph of the zirconia ceramic plate prepared for example 1.
[0034] Figure 2 The plane electron microscope graph of the zirconia ceramic plate prepared for example 1. DETAILED DESCRIPTION
[0035] In order to make the purpose, technical scheme and advantages of the embodiments of the present application more clear, the technical scheme in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.
[0036] In the present application, the technical features described in an open manner include both the closed technical scheme consisting of the listed features and the open technical scheme containing the listed features.
[0037] In the present application, if no special description is provided, the numerical range is regarded as continuous and includes the minimum value and the maximum value of the range and each value between the minimum value and the maximum value. Further, when the range refers to an integer, each integer between the minimum value and the maximum value of the range is included. In addition, when multiple ranges are provided to describe a feature or a characteristic, the ranges can be combined. In other words, unless otherwise indicated, all ranges disclosed herein should be understood to include any and all sub-ranges subsumed therein.
[0038] In the present application, the specific dispersion and stirring treatment method is not particularly limited.
[0039] The reagents or instruments used in the present application are not marked with the manufacturer, and are all conventional products that can be obtained by market purchase, and the same kind is used in parallel experiments.
[0040] Example 1
[0041] A preparation method of a not fully sintered zirconia ceramic plate, comprising the following steps:
[0042] (1) uniformly mixing yttria-doped zirconia powder, solvent, methyl amyl alcohol, phthalate, PVB to obtain a slurry;
[0043] The yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is 3:97;
[0044] The solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene to the isopropyl alcohol is 3:1;
[0045] The mass ratio of the yttria-doped zirconia powder, the solvent, the methyl amyl alcohol, the phthalate and the PVB is 100:75:2.5:6:9.
[0046] (2) ball milling the slurry in a nylon jar, the ball milling speed is 250 rpm, the ball milling time is 24 h, the mass ratio of zirconium balls to the slurry is 1:2 during the ball milling, the zirconium balls comprise zirconium balls with a diameter of 10 mm and zirconium balls with a diameter of 15 mm, and the mass ratio of the zirconium balls with a diameter of 10 mm to the zirconium balls with a diameter of 15 mm is 2:1;
[0047] (3) transferring the ball-milled slurry to a vacuum tank for defoaming, defoaming for 1 h under a vacuum degree of -0.08 MPa, and the discharge viscosity is 5000 mPa·s;
[0048] (4) using a casting machine to cast the defoamed slurry, controlling the casting speed to be 0.3 m / min, the front oven temperature to be 35℃, the rear oven temperature to be 70℃, and controlling the discharge green body thickness to be 1.5 mm;
[0049] (5) cutting the green body into a square block with a size of 150*150 mm, vacuum packaging the green body and glass with a size of 150*150*5 mm together, and isostatic pressing for 60 min under the conditions of 80 MPa and 60℃;
[0050] (6) stacking the isostatic pressed green body in 5 layers, first de-binding the stacked green body at 280℃ for 300 min, then de-binding the green body at 350℃ for 200 min, and finally de-binding the green body at 380℃ for 240 min to obtain a body;
[0051] (7) sintering the body at 800℃ for 600 min, then sintering the body at 1220℃ for 540 min, then sintering the body at 1250℃ for 300 min, and finally sintering the body at 1000℃ for 200 min to obtain a zirconia ceramic plate.
[0052] The zirconia prepared in Example 1 is taken out for detection, and the SEM image is shown in the figure, Figure 1For cross-section electron microscope, Figure 2 For planar electron microscope, it can be seen that the ceramic sheet is not completely sintered, the crystal grains are relatively loose, and the pores are relatively many, which is beneficial to the glue removal of the electrolyte sheet product, and meanwhile has good strength and hardness, is not easy to be damaged, is beneficial to transportation and storage, and can be repeatedly used, thereby reducing the cost.
[0053] Example 2
[0054] A preparation method of a zirconia ceramic plate which is not completely sintered, comprising the following steps:
[0055] (1) uniformly mixing yttria-doped zirconia powder, solvent, methyl amyl alcohol, phthalate, and PVB to obtain a slurry;
[0056] The yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is 2:98;
[0057] The solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene to the isopropyl alcohol is 3:1;
[0058] The mass ratio of the yttria-doped zirconia powder, the solvent, the methyl amyl alcohol, the phthalate, and the PVB is 100:80:3:7:8.
[0059] (2) ball milling the slurry in a nylon tank, the ball milling speed is 250 rpm, the ball milling time is 24 h, the mass ratio of zirconium balls to the slurry during ball milling is 1:2, the zirconium balls comprise zirconium balls with a diameter of 10 mm and zirconium balls with a diameter of 15 mm, and the mass ratio of the zirconium balls with a diameter of 10 mm to the zirconium balls with a diameter of 15 mm is 2:1;
[0060] (3) transferring the ball-milled slurry to a vacuum tank for defoaming, and defoaming for 1 h under a vacuum degree of -0.08 MPa;
[0061] (4) using a casting machine to cast the defoamed slurry, controlling the casting speed to be 0.3 m / min, controlling the front oven temperature to be 35℃, controlling the rear oven temperature to be 70℃, and controlling the green body thickness to be 1.5 mm;
[0062] (5) cutting the green body into a square block with a size of 150*150 mm, vacuum packaging the square block and a glass with a size of 150*150*5 mm together, and isostatic pressing for 60 min under the conditions of 80 MPa and 60℃;
[0063] (6) stacking the isostatic pressed green body in 5 layers, first removing glue from the stacked green body at 250℃ for 400 min, then removing glue from the stacked green body at 350℃ for 240 min, and finally removing glue from the stacked green body at 330℃ for 300 min, to obtain a body;
[0064] (7) sintering the green body at 780 ℃ for 720 min, then at 1200 ℃ for 600 min, then at 1220 ℃ for 360 min, and finally at 1050 ℃ for 240 min to obtain the zirconia ceramic plate.
[0065] Example 3
[0066] A method for preparing an incompletely sintered zirconia ceramic plate comprises the following steps:
[0067] (1) uniformly mixing yttria-doped zirconia powder, a solvent, methyl amyl alcohol, phthalate, and PVB to obtain a slurry;
[0068] The yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is 4:96;
[0069] The solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene to the isopropyl alcohol is 3:1;
[0070] The mass ratio of the yttria-doped zirconia powder, the solvent, the methyl amyl alcohol, the phthalate, and the PVB is 100:90:4:8:11.5.
[0071] (2) ball-milling the slurry in a nylon jar at a speed of 250 rpm for 24 h, and the mass ratio of zirconium balls to the slurry is 1:2, wherein the zirconium balls comprise zirconium balls with a diameter of 10 mm and zirconium balls with a diameter of 15 mm, and the mass ratio of the zirconium balls with a diameter of 10 mm to the zirconium balls with a diameter of 15 mm is 2:1;
[0072] (3) transferring the ball-milled slurry to a vacuum tank for defoaming at a vacuum degree of -0.08 MPa for 1 h;
[0073] (4) using a casting machine to cast the defoamed slurry, controlling the casting speed to be 0.3 m / min, the front oven temperature to be 35 ℃, and the rear oven temperature to be 70 ℃, and controlling the thickness of the green body to be 1.5 mm;
[0074] (5) cutting the green body into a square block with a size of 150*150 mm, vacuum-packaging the square block together with a glass with a size of 150*150*5 mm, and isostatic pressing the vacuum-packaged square block and the glass at 80 MPa and 60 ℃ for 60 min;
[0075] (6) stacking the isostatic pressed green body in 5 layers, first de-binding the stacked green body at 300 ℃ for 200 min, then de-binding the green body at 360 ℃ for 200 min, and finally de-binding the green body at 350 ℃ for 180 min to obtain a green body;
[0076] (7) sintering the green body at 820 ℃ for 480 min, then at 1280 ℃ for 450 min, then at 1300 ℃ for 180 min, and finally at 950 ℃ for 180 min to obtain the zirconia ceramic plate.
[0077] Comparative Example 1
[0078] A preparation method of an incompletely sintered zirconia ceramic plate, comprising the following steps:
[0079] (1) uniformly mixing yttria-doped zirconia powder, a solvent, methyl amyl alcohol, phthalate, and PVB to obtain a slurry;
[0080] The yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is 3:97;
[0081] The solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene to the isopropyl alcohol is 3:1;
[0082] The mass ratio of the yttria-doped zirconia powder, the solvent, the methyl amyl alcohol, the phthalate, and the PVB is 100:75:2.5:6:9.
[0083] (2) ball milling the slurry in a nylon tank, the ball milling speed is 250 rpm, the ball milling time is 24 h, the mass ratio of zirconium balls to the slurry is 1:2 during the ball milling, the zirconium balls comprise zirconium balls with a diameter of 10 mm and zirconium balls with a diameter of 15 mm, and the mass ratio of the zirconium balls with a diameter of 10 mm to the zirconium balls with a diameter of 15 mm is 2:1;
[0084] (3) transferring the ball-milled slurry to a vacuum tank for defoaming, defoaming at a vacuum degree of -0.08 MPa for 1 h, and the discharge viscosity is 5000 mPa·s;
[0085] (4) casting the defoamed slurry using a casting machine, controlling the casting speed to be 0.3 m / min, the front oven temperature to be 35 ℃, and the rear oven temperature to be 70 ℃, and controlling the discharge green body thickness to be 1.5 mm;
[0086] (5) cutting the green body into a square block with a size of 150*150 mm, vacuum packaging the green body and glass with a size of 150*150*5 mm together, and isostatic pressing at 80 MPa and 60 ℃ for 60 min;
[0087] (6) stacking the isostatic pressed green body in 5 layers, first discharging glue from the stacked green body at 500 ℃ for 300 min to obtain a green body;
[0088] (7) sintering the green body at 1280 ℃ for 300 min to obtain a zirconia ceramic plate.
[0089] Comparative Example 2
[0090] The degumming of the present comparative example is different from that of Example 1, and the others are the same.
[0091] A preparation method of a zirconia ceramic plate which is not completely sintered, comprising the following steps:
[0092] (1) uniformly mixing yttria-doped zirconia powder, solvent, methyl amyl alcohol, phthalate ester and PVB to obtain a slurry;
[0093] The yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is 3:97;
[0094] The solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene to the isopropyl alcohol is 3:1;
[0095] The mass ratio of the yttria-doped zirconia powder, the solvent, the methyl amyl alcohol, the phthalate ester and the PVB is 100:75:2.5:6:9.
[0096] (2) ball-milling the slurry in a nylon jar, the ball-milling speed is 250 rpm, the ball-milling time is 24 h, the mass ratio of zirconium balls to the slurry is 1:2 during the ball-milling, the zirconium balls comprise zirconium balls with a diameter of 10 mm and zirconium balls with a diameter of 15 mm, and the mass ratio of the zirconium balls with a diameter of 10 mm to the zirconium balls with a diameter of 15 mm is 2:1;
[0097] (3) transferring the ball-milled slurry to a vacuum tank for defoaming, defoaming for 1 h under a vacuum degree of -0.08 MPa, and the discharge viscosity is 5000 mPa·s;
[0098] (4) using a casting machine to cast the defoamed slurry, controlling the casting speed to be 0.3 m / min, the front oven temperature to be 35℃, the rear oven temperature to be 70℃, and controlling the discharge green body thickness to be 1.5 mm;
[0099] (5) cutting the green body into a square block with a size of 150*150 mm, vacuum packaging the square block together with glass with a size of 150*150*5 mm, and isostatic pressing for 60 min under the conditions of 80 MPa and 60℃;
[0100] (6) stacking the isostatic pressed green body in 5 layers, first degumming the stacked green body at 280℃ for 300 min, then degumming the green body at 380℃ for 240 min, and finally degumming the green body at 350℃ for 200 min to obtain a body;
[0101] (7) sintering the body at 800℃ for 600 min, then sintering the body at 1220℃ for 540 min, then sintering the body at 1250℃ for 300 min, and finally sintering the body at 1000℃ for 200 min to obtain a zirconia ceramic plate.
[0102] Comparative Example 3
[0103] The sintering of the present comparative example is different from that of Example 1, and the others are the same.
[0104] A method for preparing a zirconia ceramic plate which is not completely sintered, comprising the following steps:
[0105] (1) uniformly mixing yttria-doped zirconia powder, solvent, methyl amyl alcohol, phthalate, and PVB to obtain a slurry;
[0106] The yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is 3:97;
[0107] The solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene to the isopropyl alcohol is 3:1;
[0108] The mass ratio of the yttria-doped zirconia powder, the solvent, the methyl amyl alcohol, the phthalate, and the PVB is 100:75:2.5:6:9.
[0109] (2) ball-milling the slurry in a nylon jar, the ball-milling speed is 250 rpm, the ball-milling time is 24 h, the mass ratio of zirconium balls to the slurry is 1:2 during the ball-milling, the zirconium balls comprise zirconium balls with a diameter of 10 mm and zirconium balls with a diameter of 15 mm, and the mass ratio of the zirconium balls with a diameter of 10 mm to the zirconium balls with a diameter of 15 mm is 2:1;
[0110] (3) transferring the ball-milled slurry to a vacuum tank for defoaming, defoaming for 1 h under a vacuum degree of -0.08 MPa, and the discharge viscosity is 5000 mPa·s;
[0111] (4) using a casting machine to cast the defoamed slurry, controlling the casting speed to be 0.3 m / min, the front oven temperature to be 35℃, and the rear oven temperature to be 70℃, and controlling the discharge green body thickness to be 1.5 mm;
[0112] (5) cutting the green body into a square block with a size of 150*150 mm, vacuum packaging the square block together with a glass with a size of 150*150*5 mm, and isostatic pressing for 60 min under the conditions of 80 MPa and 60℃;
[0113] (6) stacking the isostatic pressed green body in 5 layers, first discharging the stacked green body at 280℃ for 300 min, then discharging the green body at 350℃ for 200 min, and finally discharging the green body at 380℃ for 240 min to obtain a body;
[0114] (7) The green body is sintered at 800°C for 600 min, then sintered at 1250°C for 300 min, and then sintered at 1220°C for 540 min to obtain the zirconia ceramic plate.
[0115] Test Example
[0116] The zirconia ceramic plate prepared above is fixed with one end horizontal, and the distance of the other end deviating from the horizontal position is measured as the warpage / mm.
[0117] Table 1
[0118]
[0119] It should be noted that the above examples are only used to illustrate the technical solutions of the present application, and are not intended to limit the scope of protection of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the spirit and scope of the present application.
Claims
1. A method for producing a zirconia ceramic plate which is not fully sintered, characterized by, The method comprises the following steps: (1) uniformly mixing yttria-doped zirconia powder, solvent, dispersant, plasticizer and binder to obtain slurry; (2) ball milling and defoaming the slurry; (3) performing flow casting and isostatic pressing on the defoamed slurry to obtain a green body; (4) stacking the green body and removing glue to obtain a blank; (5) sintering the blank at 780-820℃ for 480-720min, then at the first temperature for 450-600min, then at the second temperature for 180-360min, and finally at 950-1050℃ for 180-240min to obtain a zirconia ceramic plate; the first temperature is 1200-1300℃, the second temperature is 1200-1300℃, and the first temperature is less than the second temperature; the glue removal is specifically: removing glue at 250-300℃ for 200-400min, then at the third temperature for 180-240min, and finally at the fourth temperature for 180-360min; the third temperature is 350-400℃, the fourth temperature is 350-400℃, and the third temperature is less than the fourth temperature; the zirconia ceramic plate is used as a gasket for sintering of a SOFC electrolyte sheet.
2. The method of producing a not fully sintered zirconia ceramic plate according to claim 1, characterized by, The yttria-doped zirconia powder comprises yttria powder and zirconia powder, and the molar ratio of the yttria powder to the zirconia powder is (2-4):(96-98); the average particle size of the yttria-doped zirconia powder is 0.5-1μm.
3. The method of producing a not fully sintered zirconia ceramic plate according to claim 1, characterized by, The solvent comprises toluene and isopropyl alcohol, and the mass ratio of the toluene to the isopropyl alcohol is (2-4):1; the dispersant is methyl pentanol; the plasticizer is phthalate ester; the binder is PVB.
4. The method of producing a not fully sintered zirconia ceramic plate according to claim 1, characterized by, The mass ratio of the yttria-doped zirconia powder, the solvent, the dispersant, the plasticizer and the binder is 100:(70-90):(2-4):(5-8):(7-12).
5. The method of producing a not fully sintered zirconia ceramic plate according to claim 1, characterized by, The ball milling is specifically: the ball milling is performed in a ball mill tank, the ball milling speed is 200-400rpm, the ball milling time is 18-28h, and the mass ratio of zirconium balls to the slurry is 1:(1-2); the zirconium balls comprise zirconium balls with a diameter of 10mm and zirconium balls with a diameter of 15mm, and the mass ratio of the zirconium balls with a diameter of 10mm to the zirconium balls with a diameter of 15mm is (1-2):
1.
6. The method of producing a not fully sintered zirconia ceramic plate according to claim 1, characterized by, The defoaming is performed at a vacuum degree of less than-0.05MPa, and the defoaming time is 1-3h.
7. The method of producing a not fully sintered zirconia ceramic plate according to claim 1, characterized by, The flow casting is performed in a flow casting machine, and the temperature of the oven of the flow casting machine is divided into two sections during the flow casting, the temperature of the first half section is 30-40℃, and the temperature of the second half section is 50-75℃.
8. The method of producing a not fully sintered zirconia ceramic plate according to claim 1, characterized by, The pressure of the isostatic pressing is 50-100MPa, and the time is 30-120min.
9. A zirconia ceramic plate which is not fully sintered, characterized in that, The zirconia ceramic plate is prepared by the preparation method of any one of claims 1-8.
Citation Information
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