CN111087240A - Ceramic load bearing plate and preparation method and application thereof - Google Patents
Ceramic load bearing plate and preparation method and application thereof Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
Abstract
The invention provides a ceramic load bearing board and a preparation method and application thereof, and relates to the technical field of refractory materials. The ceramic setter plate comprises the following raw materials in parts by weight: 90-98 parts of yttrium-stabilized zirconia, 1-5 parts of calcium oxide, 0.8-3 parts of magnesium oxide, 0.1-0.6 part of titanium oxide and 1-3 parts of binder. The burning bearing plate has the characteristics of high strength and high temperature resistance, meets the sintering requirement of the annular piezoresistor, and has the advantages of corrosion resistance, low manufacturing cost and the like.
Description
Technical Field
The invention relates to the field of refractory ceramic materials, in particular to a ceramic load bearing plate and a preparation method and application thereof.
Background
The setter plate is a plate prepared from functional ceramics, can be used as a carrier in the sintering process of electronic components such as annular pressure-sensitive electronics, and the performance of the setter plate is closely related to the sintering effect of the electronic components. To obtain acceptable electronic components, the setter plates need to have stable chemical properties and good thermal shock resistance, and cannot deform or crack during high temperature sintering. With the updating and upgrading of electronic components, the requirements on the manufacturing process are more and more strict, for example, the sintering temperature of the annular piezoresistor is as high as 1100-1200 ℃, which puts higher requirements on the performance of the burning bearing plate.
Accordingly, an object of the present invention is to improve a setter plate and obtain a setter plate having excellent performance from a low-cost raw material.
Disclosure of Invention
Therefore, in order to solve the above problems, it is necessary to provide a ceramic setter plate, which has the characteristics of high strength and high temperature resistance, can meet the sintering requirements of the annular piezoresistor, and has the advantages of corrosion resistance, low manufacturing cost, and the like.
A ceramic setter plate comprises the following raw materials in parts by weight:
the ceramic setter plate is prepared by introducing calcium oxide, magnesium oxide and titanium oxide as auxiliary agents, wherein the metal ion radius is equal to that of Zr4+Similarly, solid solution can be formed at high temperature, the breaking strength and the high-temperature stability of the setter plate are improved, the service life of the setter plate is prolonged, and Ca2+、Mg2+、Ti4+With Zr4+The sintering temperature can be reduced under the action of ions, the sintering temperature range is expanded, the limit value of the sintering temperature is increased, and the phenomena of cracking, warping deformation and the like caused by overlarge thermal stress are reduced.
In one embodiment, the ceramic setter plate comprises the following raw materials in parts by weight:
the addition of the auxiliary agents of calcium oxide, magnesium oxide and titanium oxide is beneficial to improving the performance of the setter plate, but the content of the auxiliary agents of calcium oxide, magnesium oxide and titanium oxide is not excessive, otherwise, the performance of the setter plate is reduced, and cracking and breaking strength reduction can be seriously caused in the firing process.
In one embodiment, the yttrium-stabilized zirconia has an yttrium oxide content of 8.3% by mass.
In one embodiment, the yttrium-stabilized zirconia consists of yttrium-stabilized zirconia with a particle size of 15 to 50 mesh, 50 to 300 mesh, 325 to 1000 mesh.
In one embodiment, the yttrium-stabilized zirconia comprises the following weight percent yttrium-stabilized zirconia:
10 to 20 percent of yttrium-stabilized zirconia with the grain diameter of 15 to 50 meshes,
30 to 45 percent of yttrium stabilized zirconia with the grain diameter of 50 to 300 meshes,
45-60% of yttrium-stabilized zirconia with the grain size of 325-1000 meshes.
In one embodiment, the binder is selected from one or more of polyvinyl alcohol, carboxymethyl cellulose, dextrin, and pulp.
The invention also provides a preparation method of the ceramic setter plate, which comprises the following steps:
mixing: dissolving a binder in a solvent to obtain a binder solution, and uniformly mixing yttrium-stabilized zirconia, calcium oxide, magnesium oxide, titanium oxide and the binder solution to obtain powder;
and (3) granulation: drying the powder, and granulating to obtain granulated powder;
and (3) pressing and forming: pressing and molding the granulated powder to obtain a blank;
firing: and firing the blank body, and preserving heat to obtain the ceramic setter plate.
In one embodiment, the solvent in the mixing step is water and/or alcohol.
In one embodiment, the drying temperature in the granulating step is 60-90 ℃, and the drying time is 20-30 min.
In one embodiment, in the step of press forming, the pressing pressure is 100-150 Mpa.
In one embodiment, the firing step is carried out in a tunnel kiln, the firing temperature is 1520-1600 ℃, and the holding time is 3-5 h.
The invention also provides an application of the ceramic burning bearing plate in preparation of an annular piezoresistor. The sintering temperature of the annular piezoresistor is higher, the requirement on the high temperature resistance degree of the burning bearing plate is higher, and the burning bearing plate can meet the requirement on the sintering temperature.
Compared with the prior art, the invention has the following beneficial effects:
the ceramic load bearing board of the invention introduces calcium oxide, magnesium oxide and titanium oxide as auxiliary agents, wherein the metal ion radius is equal to Zr4+Similarly, solid solution can be formed at high temperature, the breaking strength and the high-temperature stability of the setter plate are improved, the service life of the setter plate is prolonged, and Ca2+、Mg2+、Ti4+With Zr4+The sintering temperature can be reduced under the action of ions, the sintering temperature range is expanded, the limit value of the sintering temperature is increased, and the phenomena of cracking, warping deformation and the like caused by overlarge thermal stress are reduced.
The preparation method is simple and easy to operate, and the prepared ceramic setter plate has the advantages of high strength, high temperature resistance, corrosion resistance, low manufacturing cost and the like.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the preferred embodiments. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
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 in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 1g of polyvinyl alcohol, 96g of yttrium-stabilized zirconia, 2g of calcium oxide, 1.5g of magnesium oxide and 0.5g of titanium oxide to obtain powder;
wherein, the mass content of yttrium oxide in the yttrium-stabilized zirconia is 8.6 percent; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 13% of 15-50 mesh yttrium-stabilized zirconia, 33% of 50-300 mesh yttrium-stabilized zirconia and 54% of 325-1000 mesh yttrium-stabilized zirconia;
(2) and (3) granulation: placing the powder in an oven, drying at 60 deg.C for 30min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 100MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the green body in a tunnel kiln, firing at 1550 ℃, and keeping the temperature for 4 hours to obtain the ceramic setter plate.
Example 2
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 1g of carboxymethyl cellulose, 94g of yttrium-stabilized zirconia, 4g of calcium oxide, 1.4g of magnesium oxide and 0.6g of titanium oxide to obtain powder;
wherein, the mass content of yttrium oxide in the yttrium-stabilized zirconia is 8.5%; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 12% of 15-50 mesh yttrium-stabilized zirconia, 39% of 50-300 mesh yttrium-stabilized zirconia and 49% of 325-1000 mesh yttrium-stabilized zirconia;
(2) and (3) granulation: placing the powder in an oven, baking at 90 deg.C for 20min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 150MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the green body in a tunnel kiln, firing at 1600 ℃, and preserving heat for 3 hours to obtain the ceramic setter plate.
Example 3
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 2g of dextrin water solution, 97g of yttrium-stabilized zirconia, 1g of calcium oxide, 1.7g of magnesium oxide and 0.3g of titanium oxide to obtain powder;
wherein, the mass content of yttrium oxide in the yttrium-stabilized zirconia is 9.6 percent; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 18% of 15-50 mesh yttrium-stabilized zirconia, 35% of 50-300 mesh yttrium-stabilized zirconia and 47% of 325-1000 mesh yttrium-stabilized zirconia;
(2) and (3) granulation: placing the powder in an oven, baking at 80 deg.C for 25min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 100MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the blank body in a tunnel kiln, firing at 1520 ℃, and preserving heat for 5 hours to obtain the ceramic setter plate.
Comparative example 1
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 3g of dextrin water solution, 95g of yttrium-stabilized zirconia, 4g of calcium oxide and 1g of magnesium oxide to obtain powder;
wherein, the mass content of yttrium oxide in the yttrium-stabilized zirconia is 10 percent; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 15-50 meshes of yttrium-stabilized zirconia account for 15%, 50-300 meshes of yttrium-stabilized zirconia account for 37%, and 325-1000 meshes of yttrium-stabilized zirconia account for 48%;
(2) and (3) granulation: placing the powder in an oven, drying at 60 deg.C for 30min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 100MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the green body in a tunnel kiln, firing at 1550 ℃, and keeping the temperature for 5 hours to obtain the ceramic setter plate.
Comparative example 2
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 2.8g of carboxymethyl cellulose, 93g of yttrium-stabilized zirconia, 4g of calcium oxide and 1.4g of magnesium oxide to obtain powder;
wherein, the mass content of yttrium oxide in the yttrium-stabilized zirconia is 9 percent; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 12% of 15-50 mesh yttrium-stabilized zirconia, 39% of 50-300 mesh yttrium-stabilized zirconia and 49% of 325-1000 mesh yttrium-stabilized zirconia;
(2) and (3) granulation: placing the powder in an oven, drying at 60 deg.C for 30min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 100MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the green body in a tunnel kiln, firing at 1600 ℃, and preserving heat for 3 hours to obtain the ceramic setter plate.
Comparative example 3
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 2.8g of carboxymethyl cellulose, 95.6g of yttrium-stabilized zirconia, 4g of calcium oxide and 0.4g of titanium oxide to obtain powder;
wherein, the mass content of yttrium oxide in the yttrium-stabilized zirconia is 8.9%; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 16% of 15-50 mesh yttrium-stabilized zirconia, 37% of 50-300 mesh yttrium-stabilized zirconia and 47% of 325-1000 mesh yttrium-stabilized zirconia;
(2) and (3) granulation: placing the powder in an oven, drying at 60 deg.C for 30min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 100MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the blank body in a tunnel kiln, firing at 1520 ℃, and preserving heat for 5 hours to obtain the ceramic setter plate.
Comparative example 4
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 3g of carboxymethyl cellulose, 97.5g of yttrium-stabilized zirconia, 2g of magnesium oxide and 0.5g of titanium oxide to obtain powder;
wherein the mass content of yttrium oxide in the yttrium-stabilized zirconia is 8%; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 18% of 15-50 mesh yttrium-stabilized zirconia, 35% of 50-300 mesh yttrium-stabilized zirconia and 47% of 325-1000 mesh yttrium-stabilized zirconia;
(2) and (3) granulation: placing the powder in an oven, drying at 70 deg.C for 30min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 100MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the green body in a tunnel kiln, firing at 1550 ℃, and keeping the temperature for 4 hours to obtain the ceramic setter plate.
Comparative example 5
A ceramic setter plate is prepared by the following method:
(1) mixing: uniformly mixing 2.5g of polyvinyl alcohol, 97.5g of yttrium-stabilized zirconia, 10g of calcium oxide, 5g of magnesium oxide and 3g of titanium oxide to obtain powder;
wherein, the mass content of yttrium oxide in the yttrium-stabilized zirconia is 9.5%; the mass percentage of the yttrium-stabilized zirconia of each particle size in the total yttrium-stabilized zirconia is as follows: 18% of 15-50 mesh yttrium-stabilized zirconia, 35% of 50-300 mesh yttrium-stabilized zirconia and 47% of 325-1000 mesh yttrium-stabilized zirconia;
(2) and (3) granulation: placing the powder in an oven, drying at 70 deg.C for 30min, and granulating to obtain granulated powder;
(3) and (3) pressing and forming: putting the granulated powder into a die, pressing and forming under 100MPa to obtain a blank, and drying at room temperature for 1 day;
(4) firing: and (3) placing the green body in a tunnel kiln, firing at 1550 ℃, and keeping the temperature for 4 hours to obtain the ceramic setter plate.
Examples of the experiments
The setter plates of the above examples and comparative examples were subjected to performance tests, which were as follows:
(1) and (3) apparent porosity testing: and calculating the volume density of the calculated product and the water absorption data of the measured product.
The calculation method comprises the following steps:
apparent porosity (%) -. bulk density (g/cm)3) X Water absorption (%)
(2) And (3) testing the breaking strength:
① drying the sample in a drying oven at 110 + -5 deg.C to constant weight, and taking out;
②, measuring the size of the sample, wherein the width b of the sample is vertical to the applied load force, the thickness H of the sample is the middle thickness of the edge of the applied load, and then the sample is symmetrically placed on and parallel to the lower knife edge clamp of the digital display bending resistance instrument of the loading device;
③ applying load to the sample at normal temperature until breaking;
④ record the load data at break of the sample;
⑤ calculation method:
flexural strength
R-flexural strength (MPa); p-applied pressure (N); l-distance between knife edges (60 mm); b-sample width (mm); h-sample thickness (mm)
(3) And (3) testing thermal shock resistance: and (3) placing the product at 1000 ℃ for heat preservation for 30min, cooling the product to room temperature by air until the burning board cracks, and calculating the cycle number, wherein the thermal shock resistance is low when the cycle number is lower than 20.
The test results are shown in table 1 below:
table 1 results of performance testing
As can be seen from Table 1, the setter plate of the embodiment of the invention has high breaking strength and good thermal shock resistance; in comparative examples 1 to 4, three kinds of additives (i.e., calcium oxide, magnesium oxide, and titanium oxide) were not used simultaneously, and the obtained product had relatively poor performance, poor breaking strength, low thermal shock resistance, and easy cracking, and it can be inferred from the results that the additive composition of the present invention had synergistic effects. The higher content of the assistants such as calcium oxide, magnesium oxide and titanium oxide in comparative example 5 resulted in cracking and low flexural strength during firing, indicating that the assistant combination of the present invention needs to be maintained at a lower doping level.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The ceramic setter plate is characterized by comprising the following raw materials in parts by weight:
2. the ceramic setter plate of claim 1, wherein the yttrium-stabilized zirconia has a mass content of yttrium oxide of 8 to 10%.
3. The ceramic setter plate of claim 1, wherein the yttrium-stabilized zirconia is composed of yttrium-stabilized zirconia having a particle size of 15 to 50 mesh, 50 to 300 mesh, 325 to 1000 mesh.
4. The ceramic setter plate of claim 3, wherein the yttrium-stabilized zirconia comprises the following weight percentages of yttrium-stabilized zirconia:
10 to 20 percent of yttrium-stabilized zirconia with the grain diameter of 15 to 50 meshes,
30 to 45 percent of yttrium stabilized zirconia with the grain diameter of 50 to 300 meshes,
45-60% of yttrium-stabilized zirconia with the grain size of 325-1000 meshes.
5. The ceramic setter plate of claim 1, wherein the binder is one or more selected from polyvinyl alcohol, carboxymethyl cellulose, dextrin, and pulp.
6. A method for preparing the ceramic setter plate of any one of claims 1 to 5, comprising the steps of:
mixing: dissolving a binder in a solvent to obtain a binder solution, and uniformly mixing yttrium-stabilized zirconia, calcium oxide, magnesium oxide, titanium oxide and the binder solution to obtain powder;
and (3) granulation: drying the powder, and granulating to obtain granulated powder;
and (3) pressing and forming: pressing and molding the granulated powder to obtain a blank;
firing: and firing the blank body, and preserving heat to obtain the ceramic setter plate.
7. The method according to claim 6, wherein the solvent in the mixing step is water and/or alcohol; the drying temperature in the granulating step is 60-90 ℃, and the drying time is 20-30 min.
8. The preparation method according to claim 6, wherein in the step of press forming, the pressing pressure is 100 to 150 MPa.
9. The preparation method according to claim 6, wherein the firing step is carried out in a tunnel kiln, the firing temperature is 1520-1600 ℃, and the holding time is 3-5 h.
10. Use of the ceramic setter plate of any of claims 1 to 5 in the manufacture of an annular varistor.
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