CN117945736A - Ceramic setter plate and preparation method and application thereof - Google Patents

Ceramic setter plate and preparation method and application thereof Download PDF

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Publication number
CN117945736A
CN117945736A CN202410067340.XA CN202410067340A CN117945736A CN 117945736 A CN117945736 A CN 117945736A CN 202410067340 A CN202410067340 A CN 202410067340A CN 117945736 A CN117945736 A CN 117945736A
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powder
setter plate
plate
yttrium
ceramic setter
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万广宇
吴彩红
黄德宽
娄红涛
刘名惠
丁美蓉
夏云霞
梁家辉
何兵祥
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GUANGDONG LINGGUANG NEW MATERIAL CO LTD
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GUANGDONG LINGGUANG NEW MATERIAL CO LTD
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Abstract

The invention relates to a ceramic setter plate and a preparation method and application thereof. The ceramic setter plate is mainly prepared from the following raw materials in percentage by weight: 30-50% of yttrium stabilized zirconia, 45-65% of sintering bearing plate powder, 3-20% of additive and 2-4% of binder. According to the ceramic setter plate, the waste recycled materials are used as raw materials, so that the production cost is reduced, and the raw materials contain partial ingredients of the setter product, so that the reaction of the contact surface is avoided; meanwhile, the problem of easy desolventizing of yttrium-stabilized zirconia at high temperature is solved by adding a small amount of additive, so that the stabilization rate of powder can be improved, the normal-temperature flexural strength and the high-temperature thermal shock resistance of the setter plate are further improved, and the service life of the setter plate is prolonged.

Description

Ceramic setter plate and preparation method and application thereof
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a ceramic setter plate and a preparation method and application thereof.
Background
The firing plate is a functional ceramic, is a carrier of electronic components in the sintering process, and has quality and performance, and directly influences the quality, yield, energy consumption, cost and the like of fired products. The main properties of the qualified setter plate include: the electronic component is free from deformation, cracking and stable in chemical property and good in thermal shock resistance at high-temperature sintering temperature.
However, the conventional yttrium-stabilized zirconia setter plates have the problem of deformation and cracking when directly bearing and firing annular piezoresistor products, so that the cost is increased. The reason is that in the sintering process of the annular piezoresistor, the problem that part of low-melting matters adhere to the surface of the burning-supporting plate inevitably exists, and due to the difference of the thermal expansion coefficients of the low-melting matters and the burning-supporting plate, the burning-supporting plate can generate buckling deformation due to the action of surface thermal stress in the cooling process, and when the thermal stress is larger than the strength limit of the burning-supporting plate, the cracking phenomenon can occur.
Therefore, there is a need to develop a high-strength and high-temperature-resistant setter plate.
Disclosure of Invention
Based on the above, it is necessary to provide a ceramic setter plate, and a preparation method and application thereof, aiming at the problems that the existing setter plate is easy to deform and crack in the process of bearing and firing electronic components.
The ceramic setter plate is mainly prepared from the following raw materials in percentage by weight: 30-50% of yttrium stabilized zirconia, 45-65% of sintering bearing plate powder, 3-20% of additive and 2-4% of binder.
The ceramic setter plate adopts the waste recycled materials as raw materials, so that the production cost is reduced, and the raw materials contain partial ingredients of the setter product, so that the reaction of the contact surface is avoided; meanwhile, the problem of easy desolventizing of yttrium-stabilized zirconia at high temperature is solved by adding a small amount of additive, so that the stabilization rate of powder can be improved, the normal-temperature flexural strength and the high-temperature thermal shock resistance of the setter plate are further improved, and the service life of the setter plate is prolonged. The ceramic setter plate can effectively solve the problem that the setter plate is easy to deform and crack in the firing process of the annular piezoresistor product. The ceramic setter plate has the advantages of high strength, high temperature resistance, corrosion resistance, long service life, simple manufacture and the like, and can obviously reduce the production cost of the annular piezoresistor product on the premise of ensuring that each performance index of the annular piezoresistor product is qualified.
In one embodiment, the yttrium oxide content of the yttrium-stabilized zirconia is 3 to 10mol; the granularity of the yttrium-stabilized zirconia is 80-180 meshes.
In one embodiment, the firing plate powder comprises waste yttrium stable firing plate powder, the granularity is more than or equal to 1000 meshes, and the laser granularity D50 is 4-6 mu m.
The D50 refers to the particle size corresponding to a cumulative particle size distribution percentage of one sample reaching 50%. Its physical meaning is that the particle size is greater than 50% of its particles and less than 50% of its particles, also called median or median particle size, D50.
In one embodiment, the waste yttrium stable setter plate powder is obtained by crushing waste yttrium stable setter plates.
The reaction of avoiding the contact surface, specifically, the contact part of the annular piezoresistor and the burning plate when the annular piezoresistor is placed on the burning plate, the contact reaction can be inevitably generated due to the existence of a small amount of impurities of the burning plate, and the reaction can cause the piezoresistor to generate small particle crystallization or speck, and the proportion is about 5% -10%. The crystallization or the speckles have no adverse effect on the electrical performance of the annular piezoresistor, but affect the appearance, and when appearance detection is carried out, misoperation of equipment can be caused, qualified products are regarded as unqualified products (the proportion is about 40% of that of small-particle crystallization or speckles), manual return detection is needed, and therefore efficiency is low and waste of products is caused.
The waste yttrium stable burning plate used in the invention is the burning plate which is used for burning the piezoresistor product, and can be used as the raw material for burning the burning plate, so that on one hand, the aggregation of impurities can be dispersed, and on the other hand, the reaction of the impurities is basically finished, and a new substance is formed, and the substance does not react with the piezoresistor. The ceramic setter plate can effectively reduce crystallization or speckle products, obviously reduce misoperation of equipment and reduce the workload of manual rechecking.
In one embodiment, the additive is mainly composed of the following raw materials in parts by weight: 1 to 5 parts of yttrium oxide, 0.8 to 3 parts of strontium carbonate and 0.1 to 0.6 part of barium carbonate.
In one embodiment, the additive is mainly composed of the following raw materials in parts by weight: 1 to 4 parts of yttrium oxide, 1.4 to 1.7 parts of strontium carbonate and 0.3 to 0.6 part of barium carbonate.
In one embodiment, the binder is selected from at least one of polyvinyl alcohol, carboxymethyl cellulose, and dextrin.
In one embodiment, the dextrin comprises corn dextrin.
The invention also provides a preparation method of the ceramic setter plate, which comprises the following steps: weighing the raw materials according to the proportion; mixing the yttrium-stabilized zirconia, the sintering plate powder, the additive and the binder to obtain powder a; granulating the powder a to obtain powder b; pressing the powder b into a blank, and heating to obtain the product.
In one embodiment, the preparation method of the ceramic setter comprises the following steps: weighing the raw materials according to the proportion: mixing the yttrium-stabilized zirconia, the sintering plate powder and the additive; adding a binder, and stirring to obtain powder a; granulating the powder a to obtain powder b; pressing the powder b into a blank, and heating to obtain the product.
In one embodiment, the powder b has a laser particle size D50 of 3 to 5 μm.
In one embodiment, the conditions of the pressing are: the pressure is 100-150 Mpa; the heating conditions are as follows: the temperature is 1460-1520 ℃, and the temperature is kept for 3-5 h.
The invention also provides an application of the ceramic setter plate in preparing electronic components.
In one embodiment, the electronic component comprises a toroidal varistor.
Compared with the prior art, the invention has the following beneficial effects:
According to the ceramic setter plate, the waste recycled materials are used as raw materials, so that the production cost is reduced, and the raw materials contain partial ingredients of the setter product, so that the reaction of the contact surface is avoided; meanwhile, the problem of easy desolventizing of yttrium-stabilized zirconia at high temperature is solved by adding a small amount of additive, so that the stabilization rate of powder can be improved, the normal-temperature flexural strength and the high-temperature thermal shock resistance of the setter plate are further improved, and the service life of the setter plate is prolonged. The ceramic setter plate can effectively solve the problem that the setter plate is easy to deform and crack in the firing process of the annular piezoresistor product. The ceramic setter plate has the advantages of high strength, high temperature resistance, corrosion resistance, long service life, simple manufacture and the like, and can obviously reduce the production cost of the annular piezoresistor product on the premise of ensuring that each performance index of the annular piezoresistor product is qualified. According to the invention, the firing plate for firing the piezoresistor product is used as a raw material for firing the firing plate, so that on one hand, aggregation of impurities can be dispersed, and on the other hand, the reaction of the impurities is basically finished, so that a novel substance is formed, and the substance does not react with the piezoresistor. The ceramic setter plate can effectively reduce crystallization or speckle products, obviously reduce misoperation of equipment and reduce the workload of manual rechecking.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The reagents used in the following examples, unless otherwise specified, are all commercially available; the methods used in the examples below, unless otherwise specified, were all conventional.
Table 1 mass percentages of the respective raw materials in examples and comparative examples
Example 1
And preparing the ceramic setter plate.
Weighing the raw materials according to the proportion of the table 1, wherein the yttrium oxide content of yttrium stabilized zirconia (the annular piezoresistor product is burnt) is 3mol, and the granularity is 80-180 meshes; crushing the waste yttrium stable sintering plate which is sintered by the annular piezoresistor product into sintering plate powder, wherein the mesh number of the sintering plate powder is more than 1000 meshes, and the laser granularity D50 is 4 mu m.
Placing yttrium-stabilized zirconia, the sintering plate powder and the additive into a mixer, stirring and uniformly mixing;
adding a binder, continuing stirring, and uniformly mixing to obtain powder a;
Granulating the powder a in a spray tower to ensure that the laser granularity D50 of the granulated powder reaches 3-5 mu m to obtain powder b;
weighing the powder b, and then, putting the powder b into a mould for compression molding, wherein the molding pressure is 100-150 Mpa, so as to obtain a blank;
And (3) placing the blank body into a furnace for firing, wherein the firing temperature is 1460-1520 ℃, and the heat preservation is carried out for 3-5 hours, thus obtaining the ceramic setter plate.
Example 2
And preparing the ceramic setter plate.
Weighing the raw materials according to the proportion of the table 1, wherein the yttrium oxide content of yttrium stabilized zirconia (the annular piezoresistor product is burnt) is 3mol, and the granularity is 80-180 meshes; crushing the waste yttrium stable sintering plate which is sintered by the annular piezoresistor product into sintering plate powder, wherein the mesh number of the sintering plate powder is more than 1000 meshes, and the laser granularity D50 is 5 mu m.
Placing yttrium-stabilized zirconia, the sintering plate powder and the additive into a mixer, stirring and uniformly mixing;
adding a binder, continuing stirring, and uniformly mixing to obtain powder a;
Granulating the powder a in a spray tower to ensure that the laser granularity D50 of the granulated powder reaches 3-5 mu m to obtain powder b;
weighing the powder b, and then, putting the powder b into a mould for compression molding, wherein the molding pressure is 100-150 Mpa, so as to obtain a blank;
And (3) placing the blank body into a furnace for firing, wherein the firing temperature is 1460-1520 ℃, and the heat preservation is carried out for 3-5 hours, thus obtaining the ceramic setter plate.
Example 3
And preparing the ceramic setter plate.
Weighing the raw materials according to the proportion of the table 1, wherein the yttrium oxide content of yttrium stabilized zirconia (the annular piezoresistor product is burnt) is 3mol, and the granularity is 80-180 meshes; crushing the waste yttrium stable sintering plate which is sintered by the annular piezoresistor product into sintering plate powder, wherein the mesh number of the sintering plate powder is more than 1000 meshes, and the laser granularity D50 is 6 mu m; corn dextrin is prepared into an aqueous solution with a mass concentration of 15%.
Placing yttrium-stabilized zirconia, the sintering plate powder and the additive into a mixer, stirring and uniformly mixing;
adding a binder, continuing stirring, and uniformly mixing to obtain powder a;
Granulating the powder a in a spray tower to ensure that the laser granularity D50 of the granulated powder reaches 3-5 mu m to obtain powder b;
weighing the powder b, and then, putting the powder b into a mould for compression molding, wherein the molding pressure is 100-150 Mpa, so as to obtain a blank;
And (3) placing the blank body into a furnace for firing, wherein the firing temperature is 1460-1520 ℃, and the heat preservation is carried out for 3-5 hours, thus obtaining the ceramic setter plate.
Comparative example 1
And preparing the ceramic setter plate.
Weighing the raw materials according to the proportion of the table 1, wherein the yttrium oxide content of yttrium stabilized zirconia (the annular piezoresistor product is burnt) is 3mol, and the granularity is 80-180 meshes; crushing the waste yttrium stable sintering plate which is sintered by the annular piezoresistor product into sintering plate powder, wherein the mesh number of the sintering plate powder is more than 1000 meshes, and the laser granularity D50 is 6 mu m; corn dextrin is prepared into an aqueous solution with a mass concentration of 15%.
Placing yttrium-stabilized zirconia, the sintering plate powder and the additive into a mixer, stirring and uniformly mixing;
adding a binder, continuing stirring, and uniformly mixing to obtain powder a;
Granulating the powder a in a spray tower to ensure that the laser granularity D50 of the granulated powder reaches 3-5 mu m to obtain powder b;
weighing the powder b, and then, putting the powder b into a mould for compression molding, wherein the molding pressure is 100-150 Mpa, so as to obtain a blank;
And (3) placing the blank body into a furnace for firing, wherein the firing temperature is 1460-1520 ℃, and the heat preservation is carried out for 3-5 hours, thus obtaining the ceramic setter plate.
Comparative example 2
And preparing the ceramic setter plate.
Weighing the raw materials according to the proportion of the table 1, wherein the yttrium oxide content of yttrium stabilized zirconia (the annular piezoresistor product is burnt) is 3mol, and the granularity is 80-180 meshes; crushing the waste yttrium stable sintering plate which is sintered by the annular piezoresistor product into sintering plate powder, wherein the mesh number of the sintering plate powder is more than 1000 meshes, and the laser granularity D50 is 6 mu m.
Placing yttrium-stabilized zirconia, the sintering plate powder and the additive into a mixer, stirring and uniformly mixing;
adding a binder, continuing stirring, and uniformly mixing to obtain powder a;
Granulating the powder a in a spray tower to ensure that the laser granularity D50 of the granulated powder reaches 3-5 mu m to obtain powder b;
weighing the powder b, and then, putting the powder b into a mould for compression molding, wherein the molding pressure is 100-150 Mpa, so as to obtain a blank;
And (3) placing the blank body into a furnace for firing, wherein the firing temperature is 1460-1520 ℃, and the heat preservation is carried out for 3-5 hours, thus obtaining the ceramic setter plate.
Comparative example 3
And preparing the ceramic setter plate.
Weighing the raw materials according to the proportion of the table 1, wherein the yttrium oxide content of yttrium stabilized zirconia (the annular piezoresistor product is burnt) is 3mol, and the granularity is 80-180 meshes; crushing the waste yttrium stable sintering plate which is sintered by the annular piezoresistor product into sintering plate powder, wherein the mesh number of the sintering plate powder is more than 1000 meshes, and the laser granularity D50 is 5 mu m.
Placing yttrium-stabilized zirconia, the sintering plate powder and the additive into a mixer, stirring and uniformly mixing;
adding a binder, continuing stirring, and uniformly mixing to obtain powder a;
Granulating the powder a in a spray tower to ensure that the laser granularity D50 of the granulated powder reaches 3-5 mu m to obtain powder b;
weighing the powder b, and then, putting the powder b into a mould for compression molding, wherein the molding pressure is 100-150 Mpa, so as to obtain a blank;
And (3) placing the blank body into a furnace for firing, wherein the firing temperature is 1460-1520 ℃, and the heat preservation is carried out for 3-5 hours, thus obtaining the ceramic setter plate.
Experimental example
The apparent porosities of the ceramic setter plates prepared in examples 1 to 3 and the ceramic setter plates prepared in comparative examples 1 to 3 were measured, respectively, for the percentage ratio of the volume of open pores (refer to pores communicating with the atmosphere) in the sample to the total volume of the sample (including the solid volume and the total pore volume). The larger the apparent porosity is, the better the thermal shock resistance is proved.
The flexural strength of the ceramic setter plates prepared in examples 1 to 3 and the flexural strength of the ceramic setter plates prepared in comparative examples 1 to 3 were examined, respectively, according to a three-point bending method. The higher the flexural strength, the better the thermal shock resistance is proved.
The ceramic setter plates prepared in examples 1 to 3 and the ceramic setter plates prepared in comparative examples 1 to 3 were heated to 1000 ℃ respectively, and after 30 minutes of heat preservation, air was cooled to room temperature, and then the number of cycles of cracking of the setter plates was recorded.
Internal decision criteria: the apparent porosity is more than 14%, the flexural strength is more than 12Mpa, and the thermal shock resistance is more than 20 times.
Table 2 test results of experimental examples
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (10)

1. The ceramic setter plate is characterized by being prepared from the following raw materials in percentage by weight: 30-50% of yttrium stabilized zirconia, 45-65% of sintering bearing plate powder, 3-20% of additive and 2-4% of binder.
2. The ceramic setter plate of claim 1, wherein the yttria content of the yttria-stabilized zirconia is from 3 to 10mol; the granularity of the yttrium-stabilized zirconia is 80-180 meshes.
3. The ceramic setter plate of claim 1, wherein the setter plate powder comprises waste yttrium stabilized setter plate powder with a particle size of greater than or equal to 1000 mesh and a laser particle size D50 of 4-6 μm.
4. The ceramic setter plate of claim 1, wherein the additive consists essentially of the following raw materials in parts by weight: 1 to 5 parts of yttrium oxide, 0.8 to 3 parts of strontium carbonate and 0.1 to 0.6 part of barium carbonate.
5. The ceramic setter plate of claim 4, wherein the additive consists essentially of the following raw materials in parts by weight: 1 to 4 parts of yttrium oxide, 1.4 to 1.7 parts of strontium carbonate and 0.3 to 0.6 part of barium carbonate.
6. The ceramic setter plate of claim 1, wherein the binder is selected from at least one of polyvinyl alcohol, carboxymethyl cellulose, dextrin.
7. The method for producing a ceramic setter plate as claimed in any one of claims 1 to 6, comprising the steps of: weighing the raw materials according to the proportion; mixing the yttrium-stabilized zirconia, the sintering plate powder, the additive and the binder to obtain powder a; granulating the powder a to obtain powder b; pressing the powder b into a blank, and heating to obtain the product.
8. The process according to claim 7, wherein the powder b has a laser particle size D50 of 3 to 5. Mu.m.
9. The method according to claim 7, wherein the pressing conditions are: the pressure is 100-150 Mpa; the heating conditions are as follows: the temperature is 1460-1520 ℃, and the temperature is kept for 3-5 h.
10. Use of a ceramic setter plate as defined in any one of claims 1 to 6 in the manufacture of electronic components.
CN202410067340.XA 2024-01-17 2024-01-17 Ceramic setter plate and preparation method and application thereof Pending CN117945736A (en)

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