A zirconia ceramic stacking sintering method

By using zirconia gaskets for stacking and sintering during the sintering process of zirconia ceramic substrates, the problems of warping, bending and cracking of the ceramic substrates during the sintering process are solved, the strength and pass rate of the product are improved, and the cost is reduced.

CN116573933BActive Publication Date: 2025-05-06PILOT THIN FILM MATERIALS (ZIBO) CO LTD
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Patent Information

Application Number
CN202310622928.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-30
Publication Date
2025-05-06
Estimated Expiration
2043-05-30

AI Technical Summary

Technical Problem

Zirconia ceramic substrates are prone to warping, bending and cracking during the sintering process, which affects strength and increases costs.

Method used

By zirconia ceramic stacking sintering method, by placing zirconia gaskets on top and bottom of the to-be-calcined flasks, and performing glue discharge and sintering, the thickness and length differences between the zirconia gaskets and the to-be-calcined flasks are controlled to prevent bending and warping.

Benefits of technology

It effectively reduces the bending, warping and cracking problems of the to-be-fired blank, improves the product's pass rate and bending strength, reduces production costs, and maintains the purity and conductivity of the ceramic.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a zirconia ceramic stacking sintering method, which belongs to the field of ceramic technology. The zirconia ceramic stacking sintering method comprises the following steps: preparing a green body, debinding and sintering the green body to obtain a zirconia ceramic; the green body comprises a support plate, a zirconia gasket, n green blanks to be fired, and a zirconia gasket from bottom to top; the thickness of the zirconia gasket is 100 to 500 μm, and the thickness of the green blank to be fired is 100 to 200 μm; wherein n ≥ 2, and n is a positive integer. The present invention places the zirconia gaskets above and below the green blank to be fired, respectively, and debinds and sinters them together, which can effectively reduce the problems of bending, warping, cracking, etc. of the green blank to be fired, greatly improve the qualified rate of the product, and reduce the cost; wherein the zirconia gasket and the green blank to be fired are made of the same zirconia material, the purity requirement is maintained, no new impurity elements are introduced, and the conductivity performance of the product is well guaranteed.
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Description

Technical Field

[0001] The invention relates to the technical field of ceramics, and in particular to a zirconia ceramic stacking sintering method. Background Art

[0002] Zirconia ceramic substrates are used as induction heating tubes, refractory materials, and heating elements due to their excellent high temperature resistance in functional ceramics. Zirconia ceramics have sensitive electrical performance parameters, high toughness, high bending strength and high wear resistance, excellent thermal insulation performance, and a thermal expansion coefficient close to that of steel. They are mainly used in ceramic knives, oxygen sensors, thermal substrates for fuel cells, solid oxide fuel cells, and high-temperature heating elements. Zirconia ceramics can be formed by dry pressing, isostatic pressing, grouting, hot die casting, tape casting, injection molding, plastic extrusion molding, and colloidal solidification molding.

[0003] At present, tape casting is the most popular method for forming zirconia ceramic substrates, because the blanks after tape casting can be made thinner and more uniform, and the surface is flat and clean, which are the strict standards required by the electronics industry. However, when the blank thickness is low, sintering is prone to problems such as warping, bending, and cracking, which affects the strength. At the same time, the materials used for ceramic substrates in the industry are mostly doped zirconia, among which YSZ is more common and has a higher cost. Therefore, this article focuses on a stacking sintering method for zirconia ceramic sheets, using undoped zirconia powder to prepare blanks, which are used in the tape casting preparation process of YSZ ceramic substrates as auxiliary materials to solve the problems of warping, bending, and cracking in the YSZ sintering process, improve the pass rate, and save costs. Summary of the invention

[0004] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a zirconia ceramic stacking sintering method, the prepared ceramic surface is smooth, will not warp, bend, crack, and has high bending strength.

[0005] To achieve the above object, the technical solution adopted by the present invention is:

[0006] A zirconia ceramic stacking sintering method comprises the following steps:

[0007] preparing a green body, debinding and sintering the green body to obtain zirconia ceramics;

[0008] The green body comprises, from bottom to top, a setter plate, a zirconia gasket, n biscuits to be fired, and a zirconia gasket;

[0009] The thickness of the zirconia gasket is 100-500 μm, and the thickness of the biscuit to be fired is 100-200 μm; wherein n≥2, and n is a positive integer.

[0010] As a preferred embodiment of the present invention, the thickness of the biscuit to be fired is smaller than the thickness of the zirconia gasket.

[0011] As a preferred embodiment of the present invention, n=3.

[0012] As a preferred embodiment of the present invention, the biscuit to be fired includes one of zirconia biscuit, YSZ biscuit and SSZ biscuit.

[0013] As a preferred embodiment of the present invention, the length of the zirconia gasket is a, the length of the biscuit to be fired is b, and 2mm≤ab≤5mm.

[0014] As a preferred embodiment of the present invention, the debinding temperature is 400-700° C. and the debinding time is 2-6 hours.

[0015] As a preferred embodiment of the present invention, the sintering temperature is 1280-1380° C., and the sintering time is 3-5 hours.

[0016] As a preferred embodiment of the present invention, the method for preparing the zirconium oxide gasket comprises the following steps:

[0017] Zirconia powder, toluene, anhydrous ethanol, a dispersant, a plasticizer, and a binder are ball-milled and mixed uniformly, vacuum degassing is performed to obtain a slurry, and the slurry is cast into a sheet with a thickness of 100 to 500 μm, which is sheared to a desired size, and the sheet is hydrostatically pressurized to obtain a zirconia gasket;

[0018] The mass ratio of the zirconium oxide powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder is 100:(30-40):(20-30):(2-8):(20-25):(10-15).

[0019] As a preferred embodiment of the present invention, the method for preparing the biscuit to be fired comprises the following steps:

[0020] The precursor powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder are ball-milled and mixed evenly, vacuum degassing is performed to obtain slurry, and the slurry is cast into a sheet with a thickness of 100 to 500 μm, which is sheared to a desired size, and the sheet is hydrostatically pressurized to obtain a biscuit to be fired;

[0021] The mass ratio of the precursor powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder is 100:(30-40):(20-30):(2-8):(20-25):(10-15).

[0022] As a preferred embodiment of the present invention, the precursor powder includes at least one of YSZ powder and zirconium oxide powder.

[0023] The beneficial effects of the present invention are as follows: (1) the present invention places the zirconia gaskets on the upper and lower parts of the biscuit to be fired respectively, and performs binder removal and sintering on them together, which can effectively reduce the bending, warping, cracking and other problems of the biscuit to be fired, greatly improve the qualified rate of the product, and reduce the cost; (2) the zirconia gasket and the biscuit to be fired are made of the same zirconia material, which maintains the purity requirement, does not introduce new impurity elements, and well guarantees the electrical conductivity performance of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a schematic diagram of the structure of the zirconium oxide gasket prepared in the example.

[0025] Figure 2 This is a schematic diagram of the structure of the YSZ green billet to be fired prepared in Example.

[0026] Figure 3 It is a schematic diagram of the structure of the blank of the embodiment.

[0027] Figure 4 This is a schematic diagram of the structure of the blank of Comparative Example 1.

[0028] Figure 5 It is a schematic diagram of the structure of the blank of comparative example 2.

[0029] Figure 6 Schematic diagram of the structure of the blank of comparative example 3. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application are described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present application.

[0031] In the present application, the technical features described in an open manner include closed technical solutions composed of the listed features, and also include open technical solutions containing the listed features.

[0032] In this application, when it comes to numerical ranges, unless otherwise specified, the above numerical ranges are deemed to be continuous and include the minimum and maximum values ​​of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values ​​of the range is included. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be merged. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges included therein.

[0033] In the present application, there is no particular limitation on the specific dispersion and stirring treatment methods.

[0034] The reagents or instruments used in this application without indicating the manufacturer are all conventional products that can be obtained through commercial purchase.

[0035] The present invention provides a method for sintering a zirconia ceramic stack, comprising the following steps:

[0036] preparing a green body, debinding and sintering the green body to obtain zirconia ceramics;

[0037] The green body comprises, from bottom to top, a setter plate, a zirconia gasket, n biscuits to be fired, and a zirconia gasket;

[0038] The thickness of the zirconia gasket is 100-500 μm, and the thickness of the biscuit to be fired is 100-200 μm;

[0039] Where n≥2, and n is a positive integer.

[0040] The present invention creatively places zirconia gaskets on the upper and lower parts of the biscuit to be fired, and performs binder removal and sintering together, which can effectively reduce the bending, warping, cracking and other problems of the biscuit to be fired, greatly improve the qualified rate of the product and reduce the cost.

[0041] The zirconium oxide gasket and the biscuit to be fired are made of the same zirconium oxide material, which maintains the purity requirements and does not introduce new impurity elements, thus ensuring the electrical conductivity performance of the product.

[0042] Among them, by controlling the thickness of the zirconia gasket and the biscuit to be fired, the bending, warping, cracking and other problems of the biscuit to be fired can be effectively prevented, which greatly improves the product qualification rate and reduces the cost.

[0043] Among them, in the present invention, the size of the setter plate is not limited, and the size of the setter plate can bear the zirconia gasket and the biscuit to be fired above.

[0044] In one embodiment, the thickness of the biscuit to be fired is less than the thickness of the zirconia gasket. Controlling the thickness of the biscuit to be fired to be less than the thickness of the zirconia gasket can prevent the product from warping by subjecting the biscuit to a vertical downward and uniform force. If the thickness of the zirconia gasket is less than the thickness of the biscuit to be fired, it will not have a flattening effect, resulting in an uneven surface, which will also affect the bending strength.

[0045] In one embodiment, n=3. Controlling n=3 can effectively reduce the bending, warping, cracking and other problems of the biscuit to be fired, greatly improve the qualified rate of the product, and reduce the cost. If n is greater than 3, it will not have the effect of flattening, resulting in an uneven surface, which will also affect the bending strength. If n is less than 3, it will be too large to cause the product to be difficult to shrink during the debinding process, resulting in cracking.

[0046] In one embodiment, the biscuit to be fired includes one of a zirconia biscuit, a YSZ biscuit, and a SSZ biscuit.

[0047] In one embodiment, the length of the zirconia gasket is a, the length of the biscuit to be fired is b, and 2mm≤ab≤5mm. Controlling ab within this range can effectively prevent problems such as bending, warping, and cracking, greatly improve the qualified rate of products, and reduce costs.

[0048] In one embodiment, the debinding temperature is and the debinding time is.

[0049] In one embodiment, the sintering temperature is and the sintering time is.

[0050] In one embodiment, the method for preparing the zirconium oxide gasket comprises the following steps:

[0051] Zirconia powder, toluene, anhydrous ethanol, a dispersant, a plasticizer, and a binder are ball-milled and mixed uniformly, vacuum degassing is performed to obtain a slurry, and the slurry is cast into a sheet with a thickness of 100 to 500 μm, which is sheared to a desired size, and the sheet is hydrostatically pressurized to obtain a zirconia gasket;

[0052] The mass ratio of the zirconium oxide powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder is 100:(30-40):(20-30):(2-8):(20-25):(10-15).

[0053] In one embodiment, the method for preparing the biscuit to be fired comprises the following steps:

[0054] The precursor powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder are ball-milled and mixed evenly, vacuum degassing is performed to obtain slurry, and the slurry is cast into a sheet with a thickness of 100 to 500 μm, which is sheared to a desired size, and the sheet is hydrostatically pressurized to obtain a biscuit to be fired;

[0055] The mass ratio of the precursor powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder is 100:(30-40):(20-30):(2-8):(20-25):(10-15).

[0056] In one embodiment, the precursor powder includes at least one of YSZ powder and zirconium oxide powder.

[0057] The present invention is further described below with specific embodiments:

[0058] Example 1

[0059] A zirconia ceramic stacking sintering method comprises the following steps:

[0060] (1) Preparation of zirconia gasket: Zirconia powder, toluene, anhydrous ethanol, dispersant (triethanolamine), plasticizer (DEP), and binder (PVB) were ball-milled and mixed in a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0061] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0062] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 1 The zirconia gasket shown has a thickness of D1 and a length of a;

[0063] In this embodiment, the thickness D1 of the zirconia gasket is 250 μm, and the length a is 145 mm.

[0064] (2) Preparing a YSZ green body to be fired: YSZ powder, toluene, anhydrous ethanol, a dispersant (triethanolamine), a plasticizer (DEP), and a binder (PVB) were uniformly mixed by ball milling in a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0065] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0066] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 2 The YSZ blank to be fired shown has a thickness of D2 and a length of b;

[0067] The thickness D2 of the YSZ gasket to be fired in this embodiment is 150 μm, and the length b is 140 mm, where ab = 5 mm;

[0068] (3) Figure 3As shown, the zirconia gasket prepared in step (1) is placed on a support plate (length 180 mm, width 170 mm, thickness 10 mm), and then three (i.e., n=3) pieces of YSZ blanks to be fired prepared in step (2) are placed, and then the zirconia gasket is placed on the top layer of YSZ blanks to be fired to obtain a blank;

[0069] (4) The green body is debinded at 500°C for 5 h, and then sintered at 1280°C for 5 h, and the support plate and zirconia gasket are removed to obtain YSZ ceramics.

[0070] Example 2

[0071] A zirconia ceramic stacking sintering method comprises the following steps:

[0072] (1) Preparation of zirconia gasket: Zirconia powder, toluene, anhydrous ethanol, dispersant (triethanolamine), plasticizer (DEP), and binder (PVB) were ball-milled and mixed in a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0073] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0074] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 1 The zirconia gasket shown has a thickness of D1 and a length of a;

[0075] In this embodiment, the thickness D1 of the zirconia gasket is 500 μm, and the length a is 142 mm.

[0076] (2) Preparing a YSZ green body to be fired: YSZ powder, toluene, anhydrous ethanol, a dispersant (triethanolamine), a plasticizer (DEP), and a binder (PVB) were uniformly mixed by ball milling in a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0077] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0078] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 2 The YSZ blank to be fired shown has a thickness of D2 and a length of b;

[0079] The thickness D2 of the YSZ gasket to be fired in this embodiment is 200 μm, and the length b is 140 mm, where ab = 2 mm;

[0080] (3) Figure 3 As shown, the zirconia gasket prepared in step (1) is placed on a support plate, and then three (i.e., n=3) YSZ blanks to be fired prepared in step (2) are placed, and then the zirconia gasket is placed on the topmost YSZ blank to be fired to obtain a blank;

[0081] (4) The green body is debinded at 400°C for 6 h, and then sintered at 1350°C for 4 h, and the support plate and zirconia gasket are removed to obtain YSZ ceramics.

[0082] Example 3

[0083] A zirconia ceramic stacking sintering method comprises the following steps:

[0084] (1) Preparation of zirconia gasket: Zirconia powder, toluene, anhydrous ethanol, dispersant (triethanolamine), plasticizer (DEP), and binder (PVB) were ball-milled and mixed in a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0085] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0086] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 1 The zirconia gasket shown has a thickness of D1 and a length of a;

[0087] In this embodiment, the thickness D1 of the zirconia gasket is 200 μm, and the length a is 143 mm.

[0088] (2) Preparing a YSZ green body to be fired: YSZ powder, toluene, anhydrous ethanol, a dispersant (triethanolamine), a plasticizer (DEP), and a binder (PVB) were uniformly mixed by ball milling in a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0089] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0090] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 2 The YSZ blank to be fired shown has a thickness of D2 and a length of b;

[0091] The thickness D2 of the YSZ gasket to be fired in this embodiment is 100 μm, and the length b is 140 mm, where ab = 3 mm;

[0092] (3) Figure 3 As shown, the zirconia gasket prepared in step (1) is placed on a support plate, and then three (i.e., n=3) YSZ blanks to be fired prepared in step (2) are placed, and then the zirconia gasket is placed on the topmost YSZ blank to be fired to obtain a blank;

[0093] (4) The green body is debinded at 650°C for 2.5 h, and then sintered at 1380°C for 3 h, and the support plate and zirconia gasket are removed to obtain YSZ ceramics.

[0094] Example 4

[0095] A zirconia ceramic stacking sintering method comprises the following steps:

[0096] (1) Preparation of zirconia gasket: Zirconia powder, toluene, anhydrous ethanol, dispersant (triethanolamine), plasticizer (DEP), and binder (PVB) were ball-milled and mixed in a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0097] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0098] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 1 The zirconia gasket shown has a thickness of D1 and a length of a;

[0099] In this embodiment, the thickness D1 of the zirconia gasket is 250 μm, and the length a is 145 mm.

[0100] (2) preparing the SSZ green body to be fired: SSZ powder, toluene, anhydrous ethanol, dispersant (triethanolamine), plasticizer (DEP), and binder (PVB) were mixed uniformly by ball milling at a mass ratio of 100:35:25:5:25:12 to obtain a mixture with a viscosity of 4000 mPa·s;

[0101] The mixed material was transferred to a vacuum degassing tank for degassing at a vacuum degree of -0.08Mpa for 1h, and the mixture was discharged to obtain a slurry;

[0102] The slurry was cast using a casting machine, the casting speed was controlled to be 0.1 m / min, the drying temperature was 70°C, the thickness of the discharged green billet was controlled, and the green billet was cut to the required length to obtain the following: Figure 2 The SSZ blank to be fired shown has a thickness of D2 and a length of b;

[0103] The thickness D2 of the SSZ gasket to be fired in this embodiment is 150 μm, and the length b is 140 mm, where ab = 5 mm;

[0104] (3) Figure 3 As shown, the zirconia gasket prepared in step (1) is placed on a support plate (length 180 mm, width 170 mm, thickness 10 mm), and then three (i.e., n=3) pieces of SSZ blanks to be fired prepared in step (2) are placed, and then the zirconia gasket is placed on the topmost SSZ blank to be fired to obtain a blank;

[0105] (4) The green body is debinded at 500°C for 5 h, and then sintered at 1280°C for 5 h, and the support plate and zirconia gasket are removed to obtain SSZ ceramics.

[0106] Comparative Example 1

[0107] The difference between Comparative Example 1 and Example 1 is that in Comparative Example 1, n=1, that is, in this comparative example, the number of YSZ green blanks to be fired is one. Figure 4 As shown, other things being the same, this comparative example has too low efficiency and can only produce one piece at a time, so it is not compared.

[0108] Comparative Example 2

[0109] The difference between Comparative Example 2 and Example 1 is that in Comparative Example 2, n=5, that is, in this comparative example, there are 5 YSZ green blanks to be fired. Figure 5 As shown, everything else is the same.

[0110] Comparative Example 3

[0111] The difference between Comparative Example 3 and Example 1 is that, in Comparative Example 3, the YSZ green billet to be sintered is directly placed on a support plate for sintering, and the other aspects are the same.

[0112] Comparative Example 4

[0113] The difference between Comparative Example 4 and Example 1 is that the thickness of the YSZ blank to be fired in Comparative Example 4 is greater than the thickness of the zirconia gasket, and the other aspects are the same.

[0114] The thickness D1 of the zirconia gasket in this comparative example is 150 μm.

[0115] The thickness D2 of the YSZ gasket to be fired in this comparative example is 250 μm.

[0116] Comparative Example 5

[0117] The difference between Comparative Example 5 and Example 1 is that the length of the YSZ blank to be fired and the length of the zirconia gasket in Comparative Example 5 are different from those in Example 1, and the others are the same.

[0118] The length of the zirconia gasket in this comparative example is a=140 mm.

[0119] The length of the YSZ gasket to be fired in this comparative example is b=145 mm.

[0120] Among them, ba=5mm.

[0121] Test Case

[0122] The surfaces of the products of Examples 1 to 3 and Comparative Examples 1 to 5 were observed to see whether they were intact, whether there was bending, warping or cracking, and the bending strength was tested. The test results are shown in Table 1.

[0123] Table 1

[0124]

[0125]

[0126] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A zirconia ceramic stacking sintering method, characterized in that: The following steps are involved: preparing a green body, debinding and sintering the green body to obtain zirconia ceramics; The green body comprises, from bottom to top, a setter plate, a zirconia gasket, n biscuits to be fired, and a zirconia gasket; The thickness of the zirconia gasket is 100-500 μm, and the thickness of the biscuit to be fired is 100-200 μm; Where n = 3; The thickness of the biscuit to be fired is less than the thickness of the zirconia gasket; The length of the zirconia gasket is a, the length of the biscuit to be fired is b, and 2mm≤ab≤5mm.

2. The zirconia ceramic stacking sintering method according to claim 1, characterized in that: The biscuit to be fired includes one of a zirconia biscuit, a YSZ biscuit and a SSZ biscuit.

3. The zirconia ceramic stacking sintering method according to claim 1, characterized in that: The debinding temperature is 400-700° C., and the debinding time is 2-6 hours.

4. The zirconia ceramic stacking sintering method according to claim 1, characterized in that: The sintering temperature is 1280-1380° C., and the sintering time is 3-5 hours.

5. The zirconia ceramic stacking sintering method according to claim 1, characterized in that: The preparation method of the zirconium oxide gasket comprises the following steps: Zirconia powder, toluene, anhydrous ethanol, a dispersant, a plasticizer, and a binder are ball-milled and mixed uniformly, vacuum degassing is performed to obtain a slurry, and the slurry is cast into a sheet with a thickness of 100 to 500 μm, which is sheared to a desired size, and the sheet is hydrostatically pressurized to obtain a zirconia gasket; The mass ratio of the zirconium oxide powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder is 100: (30-40): (20-30): (2-8): (20-25): (10-15).

6. The zirconia ceramic stacking sintering method according to claim 1, characterized in that: The method for preparing the biscuit to be fired comprises the following steps: The precursor powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder are ball-milled and mixed evenly, vacuum degassing is performed to obtain slurry, and the slurry is cast into a sheet with a thickness of 100 to 500 μm, which is sheared to a desired size, and the sheet is hydrostatically pressurized to obtain a biscuit to be fired; The mass ratio of the precursor powder, toluene, anhydrous ethanol, dispersant, plasticizer and binder is 100: (30-40): (20-30): (2-8): (20-25): (10-15).

7. The zirconia ceramic stacking sintering method according to claim 6, characterized in that: The precursor powder includes at least one of YSZ powder and zirconium oxide powder.

Citation Information

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