CN114315347B - Barium zirconate/magnesium oxide composite ceramic material and preparation method thereof - Google Patents
Barium zirconate/magnesium oxide composite ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a barium zirconate/magnesium oxide composite ceramic material and a preparation method thereof. The technical scheme is as follows: and mixing the barium source and the zirconium source, performing dry ball milling, preserving heat at 1200-1500 ℃, cooling along with a furnace, and crushing to obtain the pre-sintered barium zirconate powder. And mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder to obtain a mixture I. And mixing the fused magnesia particles I and the fused magnesia particles II to obtain a mixture II. And mixing the mixture I and the mixture II to obtain the barium zirconate/magnesium oxide composite ceramic powder. And (3) performing mechanical pressing, namely heating the barium zirconate/magnesium oxide composite ceramic blank to 1500-1600 ℃ under the air atmosphere and normal pressure, and preserving the heat for 3-5 hours to prepare the barium zirconate/magnesium oxide composite ceramic material. The invention has simple process, short production period, low cost and environmental protection, and the prepared barium zirconate/magnesium oxide composite ceramic material has high normal-temperature compressive strength and low normal-temperature thermal conductivity coefficient.
Description
Technical Field
The present invention belongs to the field of composite ceramic material technology. In particular to a barium zirconate/magnesium oxide composite ceramic material and a preparation method thereof.
Background
Barium zirconate has small thermal expansion coefficient (8.7 multiplied by 10) -6 ℃ -1 25-1080 ℃), lower thermal conductivity compared with magnesium oxide, higher melting point (2700 ℃), lower chemical reaction activation energy, good thermal shock resistance and excellent corrosion resistance, but barium zirconate has high manufacturing cost and cracking is easy to occur in sintering of products with larger volume.
The magnesia (MgO) has high melting point (2800 deg.C), high thermal conductivity (60W/(m.K) at 25 deg.C and 13W/(m.K) at 1000 deg.C]Excellent chemical stability, good corrosion resistance and high load fire resistance, but the ceramic has low strength, low toughness and coefficient of thermal expansion (CTE-10) -5 ℃ -1 ) Higher and poor thermal shock resistance.
The patent technology of 'a preparation method of a zirconia-magnesia ceramic material' (CN 201710801029.3[ P ]), which discloses a sol-gel method for preparing the zirconia-magnesia ceramic material by using a zirconium oxychloride-magnesium salt solution as a raw material, and the prepared zirconia-magnesia ceramic material has better bending strength and fracture toughness. However, the preparation process is complex, the preparation period is long, and the cost is high. In addition, magnesium salt solution is selected from magnesium nitrate solution, magnesium sulfate solution and the like, air pollution is generated in the production process, and the environment is not friendly. Meanwhile, the composite material has a large coefficient of heat conductivity at normal temperature, and is easy to cause heat loss.
"an aluminium-spinel-magnesia composite refractory material and its preparation method and application" (CN 201210104103.3[ P ]) patent technology, this technology discloses a method for preparing aluminium-spinel-magnesia composite refractory material by using magnesia, magnesia-alumina spinel or magnesia-alumina spinel and metal aluminium powder as raw materials; the low-temperature heat treatment in the preparation process and the introduction of aluminum powder improve the slag penetration resistance, but the normal-temperature mechanical property of the composite material is not high, and the normal-temperature compressive strength is 48-69 MPa; the introduced aluminum powder is easy to generate volume effect and crack at high temperature.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a barium zirconate/magnesium oxide composite ceramic material, which is environment-friendly, simple in process, short in production period and low in cost; the barium zirconate/magnesium oxide composite ceramic material prepared by the method has high normal-temperature compressive strength and low normal-temperature heat conductivity coefficient.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following specific steps:
step one, mixing a barium source and a zirconium source according to the molar ratio of 1: 1, performing dry ball milling for 3-4 h, keeping the temperature for 3-4 h at 1200-1500 ℃, cooling along with a furnace, and crushing to obtain the pre-sintered barium zirconate powder.
And step two, mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder according to the mass ratio of the pre-sintered barium zirconate powder to the fused magnesia fine powder of 1 to (0.5-5) to obtain a mixture I.
Mixing the fused magnesia particles I and the fused magnesia particles II according to the mass ratio of 1 to (0.4-0.75) of the fused magnesia particles I to the fused magnesia particles II to obtain a mixture II.
The particle size of the fused magnesia particles I is less than 1mm, and the particle size of the fused magnesia particles II is 1-2 mm.
And step three, mixing the mixture I and the mixture II according to the mass ratio of 1: 1 (1-2) of the mixture I to the mixture II to obtain the barium zirconate/magnesium oxide composite ceramic powder.
And fourthly, performing machine pressing molding on the barium zirconate/magnesium oxide composite ceramic powder under the condition of 100-200 MPa to prepare a barium zirconate/magnesium oxide composite ceramic blank.
And fifthly, heating the barium zirconate/magnesium oxide composite ceramic blank to 1500-1600 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 3-5 hours to prepare the barium zirconate/magnesium oxide composite ceramic material.
The barium source is barium hydroxide or barium carbonate, and the purity of the barium source is more than 99.9%; the particle size of the barium source is less than 100 mu m.
The zirconium source is one of zirconium hydroxide, basic zirconium carbonate and zirconium oxide, and the purity of the zirconium source is more than 99.0%; the particle size of the zirconium source is less than 100 μm.
The purity of the fused magnesia fine powder is more than 98.0 percent; the grain size of the fused magnesia fine powder is less than 0.074mm.
The purity of the fused magnesia particles I is more than 95.0 percent.
The purity of the fused magnesia particles II is more than 95.0 percent.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. mixing a barium source and a zirconium source, presintering, adding fused magnesia fine powder, and mixing with fused magnesia particles I and fused magnesia particles II to obtain barium zirconate/magnesium oxide composite ceramic powder; then the barium zirconate/magnesium oxide composite ceramic material is prepared by mechanical pressing and sintering, and the process is simple.
2. The invention adopts a solid-phase sintering method, does not use acidic salt solution, does not generate harmful gas, is environment-friendly and has short production period; the fused magnesia fine powder and the fused magnesia particles adopted by the invention have low cost, are convenient for batch production and have low production cost.
3. The invention takes the zirconium source, the barium source and the fused magnesia as raw materials to prepare the barium zirconate/magnesium oxide composite ceramic material, thereby effectively reducing the sintering temperature, reducing the energy consumption and lowering the production cost.
4. The composite ceramic material prepared by the invention has solid solution, improves the mechanical property and reduces the heat conductivity coefficient at normal temperature.
The barium zirconate/magnesium oxide composite ceramic material prepared by the invention is detected as follows: the volume density is 2.96-3.21 g/cm 3 (ii) a The apparent porosity is 15.7-20.4%; the normal temperature compressive strength is 52.2-108.6 MPa; the normal-temperature elastic modulus is 27.8-102 GPa; the thermal conductivity coefficient at normal temperature is 10.9-20.3W/(m.K).
Therefore, the invention has simple process, short production period, low cost and environmental protection, and the prepared barium zirconate/magnesium oxide composite ceramic material has high normal-temperature compressive strength and low normal-temperature heat conductivity coefficient compared with a single-phase fused magnesia material.
Detailed Description
The invention is further described with reference to specific embodiments, which do not limit the scope of the invention.
A barium zirconate/magnesium oxide composite ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps
Step one, mixing a barium source and a zirconium source according to the molar ratio of 1: 1, performing dry ball milling for 3-4 h, keeping the temperature for 3-4 h at 1200-1500 ℃, cooling along with a furnace, and crushing to obtain the pre-sintered barium zirconate powder.
And step two, mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder according to the mass ratio of 1 to (0.5-5) of the pre-sintered barium zirconate powder to the fused magnesia fine powder to obtain a mixture I.
Mixing the fused magnesia particles I and the fused magnesia particles II according to the mass ratio of 1 to (0.4-0.75) of the fused magnesia particles I to the fused magnesia particles II to obtain a mixture II.
And step three, mixing the mixture I and the mixture II according to the mass ratio of 1: 1 (1-2) to obtain the barium zirconate/magnesium oxide composite ceramic powder.
And fourthly, performing machine pressing molding on the barium zirconate/magnesium oxide composite ceramic powder under the condition of 100-200 MPa to prepare a barium zirconate/magnesium oxide composite ceramic blank.
And fifthly, heating the barium zirconate/magnesium oxide composite ceramic blank to 1500-1600 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 3-5 hours to prepare the barium zirconate/magnesium oxide composite ceramic material.
The barium source is barium hydroxide or barium carbonate.
The zirconium source is one of zirconium hydroxide, zirconium basic carbonate and zirconium oxide.
In this embodiment:
the particle size of the fused magnesia particles I is less than 1mm, and the particle size of the fused magnesia particles II is 1-2 mm.
The purity of the barium source is more than 99.9%; the particle size of the barium source is less than 100 mu m.
The purity of the zirconium source is more than 99.0%; the particle size of the zirconium source is less than 100 μm.
The purity of the fused magnesia fine powder is more than 98.0 percent; the grain size of the fused magnesia fine powder is less than 0.074mm.
The purity of the fused magnesia particles I is more than 95.0 percent.
The purity of the fused magnesia particles II is more than 95.0 percent.
The detailed description is omitted in the embodiments.
Example 1
A barium zirconate/magnesium oxide composite ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing a barium source and a zirconium source according to the molar ratio of 1: 1, carrying out dry ball milling for 3h, keeping the temperature at 1200 ℃ for 3h, cooling along with a furnace, and crushing to obtain the pre-sintered barium zirconate powder.
And step two, mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder according to the mass ratio of the pre-sintered barium zirconate powder to the fused magnesia fine powder of 1: 5 to obtain a mixture I.
Mixing the fused magnesia particles I and the fused magnesia particles II according to the mass ratio of 1: 0.4 of the fused magnesia particles I to the fused magnesia particles II to obtain a mixture II.
And step three, mixing the mixture I and the mixture II according to the mass ratio of 1: 1 of the mixture I to the mixture II to obtain the barium zirconate/magnesium oxide composite ceramic powder.
And fourthly, performing machine pressing on the barium zirconate/magnesium oxide composite ceramic powder under the condition of 100MPa to prepare a barium zirconate/magnesium oxide composite ceramic blank.
And fifthly, heating the barium zirconate/magnesium oxide composite ceramic blank to 1500 ℃ under the conditions of air atmosphere and normal pressure, and preserving heat for 3 hours to obtain the barium zirconate/magnesium oxide composite ceramic material.
The barium source is barium hydroxide.
The zirconium source is zirconium hydroxide.
The barium zirconate/magnesium oxide composite ceramic material prepared by the invention is detected as follows: the bulk density is 2.99/cm 3 (ii) a The apparent porosity is 20.4%; the normal temperature compressive strength is 52.4MPa; the normal-temperature elastic modulus is 95.1GPa; the thermal conductivity at room temperature is 20.3W/(mK).
Example 2
A barium zirconate/magnesium oxide composite ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing a barium source and a zirconium source according to the molar ratio of 1: 1, performing dry ball milling for 3.5h, preserving heat for 3.5h at 1300 ℃, cooling along with a furnace, and crushing to obtain the pre-sintered barium zirconate powder.
And step two, mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder according to the mass ratio of the pre-sintered barium zirconate powder to the fused magnesia fine powder of 1: 2 to obtain a mixture I.
Mixing the fused magnesia particles I and the fused magnesia particles II according to the mass ratio of 1: 0.5 of the fused magnesia particles I to the fused magnesia particles II to obtain a mixture II.
And step three, mixing the mixture I and the mixture II according to the mass ratio of 1: 1.5 to obtain the barium zirconate/magnesium oxide composite ceramic powder.
And fourthly, performing machine pressing on the barium zirconate/magnesium oxide composite ceramic powder under the condition of 150MPa to prepare a barium zirconate/magnesium oxide composite ceramic blank.
And fifthly, heating the barium zirconate/magnesium oxide composite ceramic blank to 1550 ℃ under the air atmosphere and normal pressure, and preserving the temperature for 4 hours to obtain the barium zirconate/magnesium oxide composite ceramic material.
The barium source is barium carbonate.
The zirconium source is basic zirconium carbonate.
The barium zirconate/magnesium oxide composite ceramic material prepared by the invention is detected as follows: the bulk density is 3.15/cm 3 (ii) a The apparent porosity is 15.7%; the normal temperature compressive strength is 90.2MPa; the normal-temperature elastic modulus is 27.2GPa; the heat conductivity coefficient at normal temperature is 10.91W/(mK).
Example 3
A barium zirconate/magnesium oxide composite ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing a barium source and a zirconium source according to the molar ratio of 1: 1, performing dry ball milling for 3.5h, preserving heat for 3.5h at 1400 ℃, cooling along with a furnace, and crushing to obtain the pre-sintered barium zirconate powder.
And step two, mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder according to the mass ratio of the pre-sintered barium zirconate powder to the fused magnesia fine powder of 1: 1 to obtain a mixture I.
Mixing the fused magnesia particles I and the fused magnesia particles II according to the mass ratio of 1: 0.6 of the fused magnesia particles I to the fused magnesia particles II to obtain a mixture II.
And step three, mixing the mixture I and the mixture II according to the mass ratio of 1: 2 of the mixture I to the mixture II to obtain the barium zirconate/magnesium oxide composite ceramic powder.
And fourthly, performing machine pressing on the barium zirconate/magnesium oxide composite ceramic powder under the condition of 180MPa to prepare a barium zirconate/magnesium oxide composite ceramic blank.
And fifthly, heating the barium zirconate/magnesium oxide composite ceramic blank to 1580 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 4 hours to obtain the barium zirconate/magnesium oxide composite ceramic material.
The barium source is barium hydroxide.
The zirconium source is zirconia.
The barium zirconate/magnesium oxide composite ceramic material prepared by the invention is detected as follows: the bulk density is 2.96/cm 3 (ii) a The apparent porosity is 19.8%; the normal temperature compressive strength is 108.6MPa; the normal-temperature elastic modulus is 91.3GPa; the thermal conductivity at normal temperature is 16.8W/(mK).
Example 4
A barium zirconate/magnesium oxide composite ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing a barium source and a zirconium source according to the molar ratio of 1: 1, performing dry ball milling for 4 hours, keeping the temperature for 4 hours at 1500 ℃, cooling along with a furnace, and crushing to obtain the pre-sintered barium zirconate powder.
And step two, mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder according to the mass ratio of 1: 0.5 of the pre-sintered barium zirconate powder to the fused magnesia fine powder to obtain a mixture I.
Mixing the fused magnesia particles I and the fused magnesia particles II according to the mass ratio of 1: 0.75 of the fused magnesia particles I to the fused magnesia particles II to obtain a mixture II.
And step three, mixing the mixture I and the mixture II according to the mass ratio of 1: 2 of the mixture I to the mixture II to obtain the barium zirconate/magnesium oxide composite ceramic powder.
And fourthly, performing machine pressing molding on the barium zirconate/magnesium oxide composite ceramic powder under the condition of 200MPa to prepare a barium zirconate/magnesium oxide composite ceramic blank.
And fifthly, heating the barium zirconate/magnesium oxide composite ceramic blank to 1600 ℃ under the conditions of air atmosphere and normal pressure, and preserving heat for 5 hours to obtain the barium zirconate/magnesium oxide composite ceramic material.
The barium source is barium carbonate.
The zirconium source is zirconium hydroxide.
The barium zirconate/magnesium oxide composite ceramic material prepared by the invention is detected as follows: the bulk density is 3.21/cm 3 (ii) a The apparent porosity is 17.2%; the normal-temperature compressive strength is 72.1MPa; the normal-temperature elastic modulus is 10.7GPa; the thermal conductivity at room temperature is 5.4W/(mK).
Compared with the prior art, the specific implementation mode has the following positive effects:
1. mixing a barium source and a zirconium source, pre-sintering, adding fused magnesia fine powder, and mixing with fused magnesia particles I and fused magnesia particles II to obtain barium zirconate/magnesium oxide composite ceramic powder; then the barium zirconate/magnesium oxide composite ceramic material is prepared by mechanical pressing and sintering, and the process is simple.
2. The solid-phase sintering method is adopted in the specific embodiment, an acidic salt solution is not used, harmful gas is not generated, the environment is friendly, and the production period is short; the fused magnesia fine powder and the fused magnesia particles adopted by the embodiment have low cost, are convenient for batch production and have low production cost.
3. According to the specific embodiment, the barium zirconate/magnesium oxide composite ceramic material is prepared by taking a zirconium source, a barium source and fused magnesia as raw materials, so that the sintering temperature is effectively reduced, the energy consumption is reduced, and the production cost is reduced.
4. The composite ceramic material prepared by the specific embodiment has solid solution, so that the mechanical property is improved, and the heat conductivity coefficient at normal temperature is reduced.
The barium zirconate/magnesium oxide composite ceramic material prepared by the specific embodiment is detected as follows: the volume density is 2.96-3.21 g/cm 3 (ii) a The apparent porosity is 15.7-20.4%; the normal temperature compressive strength is 52.2 to 108.6MPa; the normal temperature elastic modulus is 27.8-102 GPa; the thermal conductivity coefficient at normal temperature is 10.9-20.3W/(m.K).
Therefore, the specific implementation mode has the advantages of simple process, short production period, low cost and environmental friendliness, and the prepared barium zirconate/magnesium oxide composite ceramic material has high normal-temperature compressive strength and low normal-temperature heat conductivity coefficient.
Claims (7)
1. A preparation method of a barium zirconate/magnesium oxide composite ceramic material is characterized by comprising the following steps:
step one, mixing a barium source and a zirconium source according to the molar ratio of the barium source to the zirconium source of 1: 1, performing dry ball milling for 3-4 h, keeping the temperature for 3-4 h at 1200-1500 ℃, cooling along with a furnace, and crushing to obtain pre-sintered barium zirconate powder;
step two, mixing the pre-sintered barium zirconate powder and the fused magnesia fine powder according to the mass ratio of 1: 0.5-5 to obtain a mixture I;
mixing the fused magnesia particles I and the fused magnesia particles II according to the mass ratio of 1: 0.4-0.75 of the fused magnesia particles I to the fused magnesia particles II to obtain a mixture II;
the grain size of the fused magnesia particles I is less than 1mm, and the grain size of the fused magnesia particles II is 1-2 mm;
mixing the mixture I and the mixture II according to the mass ratio of 1: 1 (1-2) of the mixture I to the mixture II to obtain barium zirconate/magnesium oxide composite ceramic powder;
fourthly, performing machine pressing molding on the barium zirconate/magnesium oxide composite ceramic powder under the condition of 100-200 MPa to prepare a barium zirconate/magnesium oxide composite ceramic blank;
and fifthly, heating the barium zirconate/magnesium oxide composite ceramic blank to 1500-1600 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 3-5 hours to prepare the barium zirconate/magnesium oxide composite ceramic material.
2. The method for preparing a barium zirconate/magnesium oxide composite ceramic material according to claim 1, wherein the barium source is barium hydroxide or barium carbonate, and the purity of the barium source is more than 99.9%; the particle size of the barium source is less than 100 mu m.
3. The method of making a barium zirconate/magnesium oxide composite ceramic material according to claim 1, wherein the zirconium source is one of zirconium hydroxide, zirconium basic carbonate and zirconium oxide, the zirconium source having a purity of greater than 99.0%; the particle size of the zirconium source is less than 100 μm.
4. The method for preparing a barium zirconate/magnesium oxide composite ceramic material according to claim 1, wherein the purity of the fused magnesite powder is more than 98.0%; the grain size of the fused magnesia fine powder is less than 0.074mm.
5. The method for preparing a barium zirconate/magnesium oxide composite ceramic material according to claim 1, wherein the purity of the fused magnesite grain i is more than 95.0%.
6. The process for preparing a barium zirconate/magnesium oxide composite ceramic material according to claim 1, wherein the purity of the fused magnesite grain II is more than 95.0%.
7. A barium zirconate/magnesium oxide composite ceramic material, characterized in that the barium zirconate/magnesium oxide composite ceramic material is a barium zirconate/magnesium oxide composite ceramic material prepared by the method for preparing a barium zirconate/magnesium oxide composite ceramic material according to any one of claims 1 to 6.
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| CN102227591A (en) * | 2008-09-29 | 2011-10-26 | 西门子公司 | Material mixture for producing fireproof material, fireproof molded body and method for manufacturing thereof |
| CN107216132A (en) * | 2017-06-06 | 2017-09-29 | 武汉科技大学 | A kind of MgO MA unburned bricks and preparation method thereof of RH refining furnaces |
| CN113336545A (en) * | 2021-06-04 | 2021-09-03 | 武汉科技大学 | Compact barium zirconate-based composite ceramic and preparation method thereof |
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| US6656590B2 (en) * | 2001-01-10 | 2003-12-02 | Cabot Corporation | Coated barium titanate-based particles and process |
| US10370744B2 (en) * | 2016-06-14 | 2019-08-06 | King Fahd University Of Petroleum And Minerals | Reinforced magnesium composite and a method of producing thereof |
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| CN102227591A (en) * | 2008-09-29 | 2011-10-26 | 西门子公司 | Material mixture for producing fireproof material, fireproof molded body and method for manufacturing thereof |
| CN107216132A (en) * | 2017-06-06 | 2017-09-29 | 武汉科技大学 | A kind of MgO MA unburned bricks and preparation method thereof of RH refining furnaces |
| CN113336545A (en) * | 2021-06-04 | 2021-09-03 | 武汉科技大学 | Compact barium zirconate-based composite ceramic and preparation method thereof |
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