A large-sized composite carrier plate and its preparation method

Abstract

The present invention belongs to the field of preparation of advanced structural ceramics, and particularly relates to a large-sized composite carrier plate and a preparation method thereof. The outer surface layer of the carrier plate of the present invention is composed of a load-bearing isolation layer mainly composed of tabular corundum, and the inner surface layer is composed of a load-bearing support layer mainly composed of silicon carbide. A bonding layer is arranged between the outer surface layer and the inner surface layer. The bonding layer is composed of a zirconia-based main layer and upper and lower interface layers. The raw materials after mixing treatment are sequentially placed into a mold frame, scraped and evenly distributed, and then formed under high pressure. After the green body is dried, it is sintered at a temperature of 1400-1550 °C to obtain a composite carrier plate with excellent thermal shock resistance and good bonding strength. Through the innovation of the bonding layer and process setting, the present invention solves the problems of thermal shock cracking and peeling of the inner and outer layers of the carrier plate caused by large size factors, extends the service life of the composite carrier plate to more than 80 times, and improves the economy and competitiveness of the use of the carrier plate.

Description

Technical Field

[0001] The present invention belongs to the field of preparation of advanced structural ceramics, and particularly relates to a large-size composite carrier plate and a preparation method thereof. Background Art

[0002] The composite carrier plate is a carrier kiln tool for sintering electronic components, generally having a composite structure with silicon carbide as the intermediate layer and alumina as the wrapping layer. The intermediate layer utilizes the characteristics of silicon carbide having good high-temperature flexural strength and thermal shock resistance to provide good load-bearing strength and thermal shock resistance for the carrier plate. The outer layer of alumina of the composite carrier plate can play an isolation role. For example, electronic components represented by magnetic materials contain elements such as iron, oxygen, manganese, and zinc, which are prone to react with elements such as silicon during high-temperature sintering. The outer alumina layer of the composite carrier plate directly contacts the sintered products, which can reduce the pollution of magnetic materials caused by the volatilization of impurities in the inner layer. Currently, large-size composite carrier plates are relatively prone to thermal shock cracking under high-temperature load conditions. After repeated use, cracks or cracks are likely to appear between the inner and outer layers, and even delamination or spalling may occur, seriously affecting the service life of the composite carrier plate.

[0003] Chinese Patent: CN202322165986.5 discloses a large-size composite carrier plate with a breathable loading surface, which significantly improves the fluidity of the firing atmosphere on the loading surface of the carrier plate for large-sized carrier plates, making the firing atmosphere around the entire electronic component more uniform and the ventilation more unobstructed. At the same time, it avoids perforation on the carrier plate surface and the situation where the volatilization of high-temperature atmosphere in the silicon carbide inner layer causes pollution to the components and affects the performance of electronic components; it can not only meet the sintering requirements of electronic components but also meet the technical characteristic requirements of high-performance electronic components, with remarkable effects. The large-size composite carrier plate enhances the fluidity of the atmosphere and avoids the pollution of the opening through structural improvement. However, under actual high-temperature use conditions, due to the large size specifications, with the original raw material ratio and structural settings, cracks or detachment are likely to occur at the joint parts of the composite carrier plate, and thermal shock cracking problems are also likely to occur on the entire plate surface, affecting the service life of the composite carrier plate, and the general number of use times is only about 50 times. Summary of the Invention

[0004] Aiming at the above deficiencies, the present invention provides a large-size composite carrier plate, which has good bonding strength and thermal shock resistance, and has a long service life.

[0005] A large-size composite carrier plate according to a specific embodiment of the present invention is fired from a stacked body. By weight, the stacked body sequentially includes from top to bottom: 5-10 parts of a plate-shaped corundum outer layer, 6-10 parts of a bonding layer, 60-70 parts of a silicon carbide inner layer, 6-10 parts of a bonding layer, and 5-10 parts of a plate-shaped corundum outer layer, wherein,

[0006] The bonding layer sequentially includes an interface material layer, a main material layer, and an interface material layer from top to bottom, and the mass ratio of the interface material layer, the main material layer, and the interface material layer is 1-2:8-9:1-2;

[0007] According to parts by weight, the preparation raw materials of the interface material layer include:

[0008] Activated silica ≤50um 0.5-1.0 part,

[0009] Aluminum oxide fine powder ≤50um 1-2 parts,

[0010] According to parts by weight, the preparation raw materials of the main material layer include:

[0011] Zircon 0.075-0.15mm 8-9 parts.

[0012] The outer layer of the firing plate of the present invention is mainly composed of tabular corundum, and the inner layer is a bearing and supporting layer mainly composed of silicon carbide. A bonding layer is arranged between the outer layer and the inner layer, and the bonding layer is composed of a zircon main layer and upper and lower interface layers.

[0013] According to the large-size composite firing plate of the specific embodiment of the present invention, according to parts by weight, the preparation raw materials of the tabular corundum outer layer include:

[0014] Tabular corundum fine powder ≤50um 5.0-6.0 parts,

[0015] Tabular corundum 0.075-0.18mm 3.0-4.0 parts,

[0016] Aluminum oxide fine powder ≤50um 0.5-1.0 part.

[0017] According to the large-size composite firing plate of the specific embodiment of the present invention, according to parts by weight, the preparation raw materials of the silicon carbide inner layer include:

[0018] Silicon carbide 0.6-2mm 3.5-5.0 parts,

[0019] Silicon carbide 0.125-0.25mm 3.0-4.5 parts,

[0020] Silicon carbide ≤50um 1.0-2.0 parts,

[0021] Kaolin 0.045-0.075mm 1.0-2.0 parts.

[0022] According to the preparation method of the large-size composite firing plate of the specific embodiment of the present invention, the preparation method includes the following steps:

[0023] (1) Stacking and forming: The raw materials are sequentially placed into the mold to obtain a stacked body. The stacked body includes, from top to bottom in sequence: a plate-shaped corundum outer layer, a bonding layer, a silicon carbide inner layer, a bonding layer, and a plate-shaped corundum outer layer; after high-pressure forming, a formed blank is obtained;

[0024] The bonding layer includes, from top to bottom in sequence, an interface material layer, a main material layer, and an interface material layer.

[0025] By weight, the preparation raw materials of the interface material layer include:

[0026] Active silica ≤50um 0.5 - 1.0 part,

[0027] Aluminum oxide fine powder ≤50um 1 - 2 parts,

[0028] By weight, the preparation raw materials of the main material layer include:

[0029] Zircon 0.075 - 0.15mm 8 - 9 parts.

[0030] (2) Dry the formed blank until the water content is less than 1.5% to obtain a dry blank;

[0031] (3) Sinter the dry blank at 1400 - 1550 °C for 3 - 5 hours to obtain a sintered bearing plate.

[0032] Preferably, store the formed blank naturally for 24 - 48 hours, release the internal stress, then place it in a drying oven for drying. After drying at a temperature of 60 - 100 °C, obtain a dry blank with a water content less than 1.5%, and reserve it for loading into the kiln.

[0033] Preferably, the preparation method of the raw materials of the main material layer is: take 8.0 - 9.0 parts of zircon 0.075 - 0.15mm, add an aqueous PVA solution, and mix evenly to obtain the main material layer liquid, the water content of which is 3 - 6%.

[0034] Preferably, the preparation method of the raw materials of the interface material layer: take 0.5 - 1.0 part of active silica ≤50um, 1.0 - 2.0 parts of aluminum oxide fine powder ≤50um, add an aqueous PVA solution, and mix evenly to obtain the interface material liquid, the water content of which is 2 - 5%.

[0035] Preferably, the thickness of the main material layer is 1 - 1.5mm, and the thickness of the interface material layer is 0.1 - 0.5mm. During the firing process, the interface layer penetrates with the inner layer and the outer layer. Part of the main material layer of the bonding layer dissociates into a silica liquid phase and a monoclinic zirconia phase at high temperature, and reacts with the mixture of active silica and aluminum oxide fine powder in the interface layer, and can form a zircon corundum mullite composite phase network interlaced structure doped and toughened with baddeleyite phase.

[0036] The mixture of reactive silica and alumina micro-powders in the interface layer and the tabular corundum and alumina micro-powders in the outer layer are pressed by high pressure, enhancing the bonding force between particles. At high temperatures, they react to form a corundum-mullite composite structure, strengthening the bonding strength between the bonding layer and the outer layer, and having good bonding strength and excellent thermal shock resistance.

[0037] The reactive silica and alumina micro-powder mixture in the interface layer and the silica in kaolin in the inner layer and the silica generated by the high-temperature oxidation of silicon carbide react at high temperatures to form a corundum-mullite composite structure, strengthening the bonding strength between the bonding layer and the inner layer, and having good bonding strength and excellent thermal shock resistance.

[0038] Preferably, the preparation method of the raw materials for the tabular corundum outer layer: Take 5.0 - 6.0 parts of tabular corundum micro-powder ≤50um, 3.0 - 4.0 parts of tabular corundum 0.075 - 0.18mm, 0.5 - 1.0 parts of alumina micro-powder ≤50um, add an aqueous PVA solution, mix evenly to obtain the outer layer liquid, and its moisture content is 3 - 6%.

[0039] Preferably, the preparation method of the raw materials for the silicon carbide inner layer: Take 3.5 - 5.0 parts of silicon carbide 0.6 - 2mm, 3.0 - 4.5 parts of silicon carbide 0.125 - 0.25mm, 1.0 - 2.0 parts of silicon carbide ≤50um, 1.0 - 2.0 parts of kaolin 0.045 - 0.075mm, add PVA and mix evenly to obtain the inner layer liquid, and its moisture content is 3 - 8%.

[0040] The beneficial effects of the present invention:

[0041] On the basis of fully understanding the main reasons for the damage of large-size composite carrier plates during use, through the innovation of the bonding layer and process improvement, the bonding strength and thermal shock resistance of the carrier plate are greatly enhanced, solving the problems of thermal shock cracking and peeling of the inner and outer layers of the carrier plate caused by large-size factors, increasing the service life of the composite carrier plate to more than 80 times, reducing the manufacturing cost of the user unit, and enhancing the economy and competitiveness of the use of the carrier plate.

[0042] The bonding layer material uses zirconia as the main raw material, and the interface material selects a mixture of reactive silica micro-powder and alumina micro-powder. Among them, zirconia has a small thermal expansion coefficient and good toughness. Select fine powder of zirconia 0.075 - 0.15mm, which decomposes into monoclinic zirconia phase and silica liquid phase during firing at high temperatures. It can react with the reactive silica micro-powder and alumina micro-powder of the interface material to form a columnar mullite network composite structure with monoclinic zirconia phase doping and toughening, having good bonding strength and excellent thermal shock resistance.

[0043] The present invention optimizes the particle size distribution of silicon carbide in the inner layer material, and adopts a laminated feeding method, which promotes the partial embedding of reactive silica powder and alumina powder in the interface material into the gaps between silicon carbide particles. Through the firing reaction, the silica in kaolin of the inner layer material and the silica generated by the high-temperature oxidation of silicon carbide form an integrated mullite network composite intersection structure with the bonding layer, and at the same time, it can also improve the load-bearing performance and thermal shock resistance of the silicon carbide base layer of the support plate.

[0044] The optimized particle size distribution and composition of the outer layer material, through the firing reaction, the tabular corundum powder is more conducive to the formation of a mullite network composite intersection structure together with the reactive silica powder and alumina powder in the interface layer, improving the bonding strength and spalling resistance of the support plate. Detailed implementation mode

[0045] To make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be described in detail below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other implementation manners obtained by those of ordinary skill in the art without creative efforts belong to the scope protected by the present invention.

[0046] In the present invention, the large-size support plate refers to a support plate with at least one side length ≥ 350 mm.

[0047] The present invention provides a method for preparing a large-size composite support plate, including the following steps:

[0048] (1) Raw material preparation:

[0049] Outer layer material:

[0050] Mix 5.0 - 6.0 parts of tabular corundum powder ≤ 50um, 3.0 - 4.0 parts of tabular corundum 0.075 - 0.18mm, and 0.5 - 1.0 parts of alumina powder ≤ 50um, add PVA aqueous solution to obtain the outer layer material liquid, the moisture content of the outer layer material liquid is 3 - 6%, and keep it in storage for later use.

[0051] Main body material: 8.0 - 9.0 parts of zircon sand 0.075 - 0.15mm, put it into a three-dimensional mixer, add PVA aqueous solution, mix evenly to obtain the main body material liquid, its moisture content is 3 - 6%, and keep it in storage for later use;

[0052] Interface layer material: 0.5 - 1.0 parts of reactive silica ≤ 50um, 1.0 - 2.0 parts of alumina powder ≤ 50um, add PVA aqueous solution, mix evenly to obtain the interface layer material liquid, its moisture content is 2 - 5%, and keep it in storage for later use, wherein both the reactive silica powder and the alumina powder are powders treated by spray granulation.

[0053] Inner layer material: 3.5 - 5.0 parts of silicon carbide with a particle size of 0.6 - 2 mm, 3.0 - 4.5 parts of silicon carbide with a particle size of 0.125 - 0.25 mm, 1.0 - 2.0 parts of silicon carbide with a particle size of ≤50 μm, and 1.0 - 2.0 parts of kaolin with a particle size of 0.045 - 0.075 mm are added to an aqueous PVA solution, mixed evenly to obtain an inner layer material liquid with a moisture content of 3 - 8%, and stored for later use after aging.

[0054] (2) Stacking and forming:

[0055] The outer layer material, bonding layer material, interface layer material, and inner layer mixture that have been aged for 24 - 36 hours are layered into a mold in the order of outer layer material, bonding layer material, interface layer material, bonding layer material, inner layer material, bonding layer material, interface layer material, bonding layer material, and outer layer material to obtain a stacked body. By weight, the stacked body sequentially includes from top to bottom: 5 - 10 parts of tabular corundum outer layer, 6 - 10 parts of bonding layer, 60 - 70 parts of silicon carbide inner layer, 6 - 10 parts of bonding layer, and 5 - 10 parts of tabular corundum outer layer. Among them,

[0056] By weight, the bonding layer sequentially includes 1.0 - 2.0 parts of interface material layer, 8.0 - 9.0 parts of main body material layer, and 1.0 - 2.0 parts of interface material layer from top to bottom;

[0057] The stacked body is formed under high pressure to obtain a formed blank;

[0058] (3) Drying the formed blank until the water content is less than 1.5% to obtain a dry blank;

[0059] (4) High-temperature firing:

[0060] The dried qualified blank is sintered at 1400 - 1550 °C and held for 3 - 5 hours to obtain a large-sized composite carrier plate with good bonding strength and excellent thermal shock resistance.

[0061] Preferably, the weight of tabular corundum micropowder ≤50 μm is 5.2 - 5.7 parts, the weight of tabular corundum with a particle size of 0.075 - 0.18 mm is 3.2 - 3.8 parts, and the weight of alumina micropowder ≤50 μm is 0.6 - 0.8 parts.

[0062] Preferably, the tabular corundum micropowder and alumina micropowder are powders obtained by spray granulation.

[0063] Preferably, 8.2 - 8.8 parts of zircon with a particle size of 0.075 - 0.15 mm, and the water content of the inner layer material liquid is preferably 4 - 5%.

[0064] Preferably, 0.6 - 0.8 parts of reactive silica ≤50 μm and 1.0 - 1.3 - 1.8 parts of alumina micropowder ≤50 μm, and the water content of the interface layer material liquid is preferably 3 - 4%.

[0065] Preferably, both the activated silica fine powder and the alumina fine powder are powders processed by spray granulation.

[0066] Preferably, 3.8 - 4.6 parts of silicon carbide with a size of 0.6 - 2 mm, 3.4 - 4.2 parts of silicon carbide with a size of 0.125 - 0.25 mm, 1.4 - 1.8 parts of silicon carbide with a size of ≤50 μm, and 1.2 - 1.8 parts of kaolin with a size of 0.045 - 0.075 mm. The water content of the inner layer liquid is preferably 3 - 4%.

[0067] The mass concentration of the PVA aqueous solution is preferably 1 - 1.5%.

[0068] Preferably, a pressure of 150 - 200 MPa is applied by a molding hydraulic press to perform high - pressure molding on the stacked body, and then a molded blank is obtained; the molded blank is stored naturally for 24 - 48 hours, and after releasing the internal stress, it is placed in a drying oven for drying. After drying at a temperature of 60 - 100°C, a dry blank with a water content of less than 1.5% is obtained and reserved for loading into the kiln.

[0069] Preferably, the high - temperature sintering system of the present invention is as follows:

[0070]

[0071] Example 1

[0072] The preparation method of the large - size composite carrier plate of the present invention includes the following steps:

[0073] 1. Preparation of raw materials:

[0074] Outer layer material: 5.0 parts of tabular corundum fine powder with a size of ≤50 μm, 3.0 parts of tabular corundum with a size of 0.075 - 0.18 mm, and 0.5 part of alumina fine powder with a size of ≤50 μm are put into a three - dimensional mixer and dry - mixed for 0.5 hour. Then, 1% PVA aqueous solution is added, and the mixture is further mixed for 0.5 - 1 hour until evenly mixed. The water content of the outer layer liquid is controlled at 3%, and it is stored for later use after aging. Among them, the tabular corundum fine powder and the alumina fine powder are powders processed by spray granulation;

[0075] Main body material: 8.0 parts of zircon with a size of 0.075 - 0.15 mm are put into a three - dimensional mixer, 1% PVA aqueous solution is added, and the mixture is mixed for 0.5 hour until evenly mixed. The water content of the main body liquid is controlled at 3%, and it is stored for later use after aging;

[0076] Interface layer material: 0.5 part of activated silica with a size of ≤50 μm and 1.0 part of alumina fine powder with a size of ≤50 μm are put into a three - dimensional mixer, 1% PVA aqueous solution is added, and the mixture is mixed for 0.5 hour until evenly mixed. The water content of the interface layer liquid is controlled at 2%, and it is stored for later use after aging. Among them, both the activated silica fine powder and the alumina fine powder are powders processed by spray granulation;

[0077] Inner layer material: Put 3.5 parts of silicon carbide with a particle size of 0.6 - 2 mm, 3.0 parts of silicon carbide with a particle size of 0.125 - 0.25 mm, 1.0 part of silicon carbide with a particle size of ≤50 μm, and 1.0 part of kaolin with a particle size of 0.045 - 0.075 mm into a mixer, dry mix for 0.5 hours, add 1% PVA aqueous solution, and then mix for another 0.5 hours until evenly mixed. Control the moisture content of the inner layer material at 3%, and let it stand for later use;

[0078] 2. Pressing and drying of molding:

[0079] Take 1 / 2 of the outer layer material, 1 / 4 of the interface layer material, 1 / 2 of the bonding layer material, 1 / 4 of the interface material, the inner layer material, 1 / 4 of the interface material, 1 / 2 of the bonding layer material, 1 / 4 of the interface material, and 1 / 2 of the outer layer material, and lay them in sequence into the mold cavity. After scraping the material flat, apply a pressure of 100 MPa through a molding hydraulic press for high-pressure molding to obtain a molded blank;

[0080] By weight, 5 parts of plate-shaped corundum outer layer, 6 parts of bonding layer, 60 parts of silicon carbide inner layer, 6 parts of bonding layer, and 5 parts of plate-shaped corundum outer layer; the mass ratio of the interface material layer, the main body material layer, and the interface material layer is 1:8:1.

[0081] Let the molded blank stand naturally for 24 hours to release internal stress, then put it into a drying oven for drying. After drying at a temperature of 60°C, obtain a dry blank with a moisture content of less than 1.5% for later use in loading the kiln;

[0082] 3. High-temperature firing:

[0083] The qualified dried blank is sintered through the following procedures to obtain a large-sized composite carrier plate,

[0084]

[0085]

[0086] Example 2

[0087] The preparation method of the large-sized composite carrier plate of the present invention includes the following steps:

[0088] 1. Preparation of raw materials:

[0089] Outer layer material: Put 5.5 parts of plate-shaped corundum fine powder with a particle size of ≤50 μm, 3.5 parts of plate-shaped corundum with a particle size of 0.075 - 0.18 mm, and 0.8 part of alumina fine powder with a particle size of ≤50 μm into a three-dimensional mixer, dry mix for 0.8 hours, add 1.2% PVA aqueous solution, and then mix for another 0.8 hours to obtain a uniform mixture. Control the moisture content of the mixture at 4%, and let it stand for later use. Among them, the plate-shaped corundum fine powder and alumina fine powder are powders treated by spray granulation;

[0090] Main material: 8.5 parts of zircon 0.075 - 0.15 mm are put into a three-dimensional mixer, and 1.2% PVA aqueous solution is added. After mixing for 0.8 hours, the main material liquid is obtained, with a moisture content of 4%. It is stored for later use after aging;

[0091] Interface layer material: 0.6 part of active silica ≤50 um and 1.3 parts of alumina micropowder ≤50 um are put into a three-dimensional mixer, and 1.2% PVA aqueous solution is added. After mixing for 0.8 hours and mixing evenly, the moisture content of the interface material liquid is 3%. It is stored for later use after aging, where both the active silica micropowder and the alumina micropowder are powders treated by spray granulation;

[0092] Inner layer material: 4 parts of silicon carbide 0.6 - 2 mm, 4 parts of silicon carbide 0.125 - 0.25 mm, 1.5 parts of silicon carbide ≤50 um, and 1.5 parts of kaolin 0.045 - 0.075 mm are put into a mixer and dry-mixed for 0.8 hours. Then 1.2% PVA aqueous solution is added, and it is mixed for another 0.8 hours and mixed evenly. The moisture content of the inner layer material is 4%. It is stored for later use after aging;

[0093] 2. Pressing and drying of molding:

[0094] Take 1 / 2 of the outer layer material, 1 / 4 of the interface layer material, 1 / 2 of the bonding layer material, 1 / 4 of the interface material, the inner layer material, 1 / 4 of the interface material, 1 / 2 of the bonding layer material, 1 / 4 of the interface material, and 1 / 2 of the outer layer material, and cloth them in sequence into the mold cavity. After scraping the material flat, apply a pressure of 100 MPa through a molding hydraulic press for high-pressure molding to obtain a molded blank;

[0095] By weight, 7 parts of plate-shaped corundum outer layer, 8 parts of bonding layer, 65 parts of silicon carbide inner layer, 8 parts of bonding layer, and 7 parts of plate-shaped corundum outer layer; the mass ratio of the interface material layer, the main material layer, and the interface material layer is 1.5:8.5:1.5.

[0096] Let the molded blank be stored naturally for 36 hours. After releasing the internal stress, put it into a drying oven for drying. After drying at a temperature of 60 - 100 °C, a dry blank with a moisture content less than 1.5% is obtained and reserved for loading into the kiln;

[0097] 3. High-temperature firing:

[0098] The qualified dried blank is sintered through the following procedures to obtain a large-sized composite carrier plate,

[0099]

[0100] Example 3

[0101] The preparation method of the large-sized composite carrier plate of the present invention includes the following steps:

[0102] 1. Preparation of raw materials:

[0103] Outer layer material: Put 6.0 parts of tabular corundum micropowder ≤50um, 4.0 parts of tabular corundum 0.075 - 0.18mm, and 1.0 part of alumina micropowder ≤50um into a three-dimensional mixer, dry mix for 0.5 - 1 hour, add 1.5% PVA aqueous solution, then mix for another 1 hour until evenly mixed. The water content of the outer layer material liquid is 6%, and let it stand for later use. Among them, the tabular corundum micropowder and alumina micropowder are powders processed by spray granulation;

[0104] Main body material: Put 9.0 parts of zircon 0.075 - 0.15mm into a three-dimensional mixer, add 1.5% PVA aqueous solution, mix for 1 hour until evenly mixed. The water content of the main body material liquid is 6%, and let it stand for later use;

[0105] Interface layer material: Put 1.0 part of reactive silica ≤50um and 2.0 parts of alumina micropowder ≤50um into a three-dimensional mixer, add 1.5% PVA aqueous solution, mix for 1 hour until evenly mixed. The water content of the interface layer material liquid is 5%, and let it stand for later use. Among them, the reactive silica micropowder and alumina micropowder are both powders processed by spray granulation;

[0106] Inner layer material: Put 5.0 parts of silicon carbide 0.6 - 2mm, 4.5 parts of silicon carbide 0.125 - 0.25mm, 2.0 parts of silicon carbide ≤50um, and 2.0 parts of kaolin 0.045 - 0.075mm into a mixer, dry mix for 1 hour, add 1.5% PVA aqueous solution, then mix for another 1 hour until evenly mixed. The water content of the inner layer material liquid is 8%, and let it stand for later use;

[0107] 2. Pressing and drying of molding:

[0108] Take 1 / 2 of the outer layer material, 1 / 4 of the interface layer material, 1 / 2 of the bonding layer material, 1 / 4 of the interface material, the inner layer material, 1 / 4 of the interface material, 1 / 2 of the bonding layer material, 1 / 4 of the interface material, and 1 / 2 of the outer layer material, and cloth them in sequence into the mold cavity. After scraping the material flat, apply a pressure of 200 MPa through a molding hydraulic press for high-pressure molding to obtain a molded blank;

[0109] By weight, 10 parts of tabular corundum outer layer, 10 parts of bonding layer, 70 parts of silicon carbide inner layer, 10 parts of bonding layer, and 10 parts of tabular corundum outer layer; the mass ratio of the interface material layer, the main body material layer, and the interface material layer is 1:9:2.

[0110] Let the molded blank be stored naturally for 48 hours, release the internal stress, then put it into a drying oven for drying. After drying at a temperature of 100°C, obtain a dry blank with a water content less than 1.5%, and reserve it for loading into the kiln;

[0111] 3. High-temperature firing:

[0112] The qualified dried green parts are sintered through the following process to obtain large-sized composite carrier plates,

[0113]

[0114]

[0115] Comparative Example 1

[0116] The raw materials of the main material layer are replaced with monoclinic zirconia granular materials, and other components and preparation methods are the same as those in Example 1.

[0117] Comparative Example 2

[0118] The raw materials of the interface layer are replaced with silica particles and alumina particle materials, wherein the silica is 0.063 - 0.18 mm and the alumina powder is 0.075 - 0.18 mm, and other components and preparation methods are the same as those in Example 1.

[0119] Comparative Example 3

[0120] All of the silicon carbide ≤ 50 um in the inner layer material is replaced with silicon carbide of 0.6 - 2 mm, and other components and preparation methods are the same as those in Example 1.

[0121] Comparative Example 4

[0122] In the outer layer material, all of the tabular corundum micropowder ≤ 50 um is replaced with tabular corundum of 0.075 - 0.18 mm, and other components and preparation methods are the same as those in Example 1.

[0123] Take the carrier plates obtained in Examples 1 - 3 and Comparative Examples 1 - 4, and test their thermal shock resistance and service life respectively.

[0124] Thermal shock resistance test method: YB / T376.1 - 1995 Test method for thermal shock resistance of refractories (water quenching method). The service life is counted by the counting method, with one operation of the carrier plate counted as one time, and record the actual service life of the carrier plate.

[0125] The results are shown in Table 1.

[0126] Table 1 Performance test results of carrier plates

[0127] Number of thermal shock cycles Number of uses Example 1 62 83 Example 2 61 84 Example 3 65 86 Comparative Example 1 53 52 Comparative Example 2 62 56 Comparative Example 3 58 53 Comparative Example 4 45 56

[0128] As can be seen from Table 1, the thermal shock times of the carrier plates obtained by the present invention exceed 60 times, and the service life can reach more than 80 times.

[0129] Zircon partially dissociates into a silicon dioxide liquid phase and a monoclinic zirconium dioxide phase under high temperature conditions, and reacts with a mixture of interfacially active silicon dioxide and alumina powder to form a complex network interlaced structure of zirconium corundum mullite doped with a badly zirconium crystal phase for toughening. When used as the main material of the bonding layer, the more monoclinic zirconium dioxide particles in Comparative Example 1 will aggregate, and the structure presented will destroy the network structure of the corundum mullite, affecting the strength of the bonding layer.

[0130] In Comparative Example 2, the raw materials of the interface layer replace the silica particles and alumina particles, which is not conducive to forming a corundum-mullite complex phase structure with the plate-like corundum micropowder of the outer layer. The single phase structure of the corundum phase or mullite phase may be formed, which affects the bonding strength of the support plate. At the same time, the outer layer may form a reticulation or peel off.

[0131] In Comparative Example 3, the amount of silicon carbide powder is reduced, which affects the reaction between the active silica powder and alumina powder of the bonding layer interface material and the silica powder, thereby affecting the formation of the zirconium corundum mullite complex network staggered structure bonding layer and reducing the bonding strength of the product.

[0132] In Comparative Example 4, reducing the amount of plate-like corundum powder affects the formation of the corundum-mullite structure of the outer layer, thereby affecting the strength and wear resistance of the surface layer, and the surface layer is prone to powdering and even peeling.

[0133] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A large-size composite setter, characterized in that: The support plate is formed by firing a stacked body, and the stacked body comprises, from top to bottom, in parts by weight: 5 to 10 parts of a plate-shaped corundum outer layer, 6 to 10 parts of a bonding layer, 60 to 70 parts of a silicon carbide inner layer, 6 to 10 parts of a bonding layer, and 5 to 10 parts of a plate-shaped corundum outer layer, wherein: The bonding layer includes an interface material layer, a main material layer, and an interface material layer from top to bottom, and the mass ratio of the interface material layer, the main material layer, and the interface material layer is 1-2:8-9:1-2; In parts by weight, the raw materials for preparing the interface material layer include: Active silicon dioxide ≤50um 0.5~1.0 parts, Alumina powder ≤50um 1-2 parts, In terms of weight, the raw materials for preparing the main material layer include: Zircon 0.075~0.15mm 8~9 parts.

2. The large-size composite setter according to claim 1, characterized in that: According to weight percentage, the raw materials for preparing the outer layer of tabular corundum include: Plate-shaped corundum powder ≤50um 5.0~6.0 parts, Plate-shaped corundum 0.075~0.18mm 3.0~4.0 parts, Alumina powder ≤50um 0.5~1.0 part.

3. The large-size composite setter according to claim 1, characterized in that: According to weight percentage, the raw materials for preparing the silicon carbide inner layer include: Silicon carbide 0.6~2mm 3.5~5.0 parts, Silicon carbide 0.125~0.25mm 3.0~4.5 parts, Silicon carbide ≤50um 1.0~2.0 parts, Kaolin 0.045~0.075mm 1.0~2.0 parts.

4. The method for preparing the large-size composite setter plate according to any one of claims 1 to 3, characterized in that: The preparation method comprises the following steps: (1) Stacking molding: placing the raw materials into a mold in sequence to obtain a stacked body, wherein the stacked body comprises, from top to bottom, a plate-shaped corundum outer layer, a bonding layer, a silicon carbide inner layer, a bonding layer, and a plate-shaped corundum outer layer; after high-pressure molding, a molded blank is obtained; The bonding layer includes the interface material layer, the main material layer and the interface material layer from top to bottom. In parts by weight, the raw materials for preparing the interface material layer include: Active silicon dioxide ≤50um 0.5~1.0 parts, Alumina powder ≤50um 1-2 parts, In terms of weight, the raw materials for preparing the main material layer include: Zircon 0.075~0.15mm 8~9 parts, (2) drying the formed blank until the moisture content is less than 1.5% to obtain a dry blank; (3) Sintering the dry blank at 1400-1550° C. and keeping the temperature for 3-5 hours to obtain a composite support plate.

5. The preparation method according to claim 4, characterized in that: The preparation method of the raw material of the main material layer is: take 8.0-9.0 parts of zircon with a size of 0.075-0.15 mm, add PVA aqueous solution, mix evenly, and obtain the main material liquid with a water content of 3-6%.

6. The preparation method according to claim 4, characterized in that: The preparation method of the raw materials of the interface material layer is as follows: take 0.5-1.0 parts of active silicon dioxide ≤50um and 1.0-2.0 parts of alumina powder ≤50um, add PVA aqueous solution, mix evenly, and obtain an interface material liquid with a water content of 2-5%.

7. The preparation method according to claim 4, characterized in that: Preparation method of raw materials for the outer layer of plate-like corundum: take 5.0-6.0 parts of plate-like corundum powder ≤50um, 3.0-4.0 parts of plate-like corundum 0.075-0.18mm, and 0.5-1.0 parts of alumina powder ≤50um, add PVA aqueous solution, mix evenly, and obtain outer layer liquid, whose water content is 3-6%.

8. The preparation method according to claim 4, characterized in that: The preparation method of the raw materials for the silicon carbide inner layer is as follows: 3.5-5.0 parts of silicon carbide 0.6-2mm, 3.0-4.5 parts of silicon carbide 0.125-0.25mm, 1.0-2.0 parts of silicon carbide ≤50um, and 1.0-2.0 parts of kaolin 0.045-0.075mm, add PVA and mix evenly to obtain an inner layer liquid with a water content of 3-8%.

9. The preparation method according to claim 4, characterized in that: The thickness of the main material layer is 1 to 1.5 mm, and the thickness of the interface material layer is 0.1 to 0.5 mm.

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