CN116751035A - Alumina ceramic material for thermal quantity sensor - Google Patents

Alumina ceramic material for thermal quantity sensor Download PDF

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Publication number
CN116751035A
CN116751035A CN202310628058.XA CN202310628058A CN116751035A CN 116751035 A CN116751035 A CN 116751035A CN 202310628058 A CN202310628058 A CN 202310628058A CN 116751035 A CN116751035 A CN 116751035A
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parts
oxide
ceramic material
powder
alumina ceramic
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辛绍文
奉碧霞
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Xinhua Xintiandi Fine Ceramics Co ltd
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Xinhua Xintiandi Fine Ceramics Co ltd
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Abstract

The invention relates to the field of ceramic materials, in particular to an alumina ceramic material for a thermal quantity sensor, which comprises the following raw materials in parts by weight: 60-80 parts of titanium sol coated alumina powder, 20-30 parts of nano silicon dioxide, 0.1-0.5 part of graphene oxide, 10-20 parts of yttrium aluminum garnet pre-powder, 2-5 parts of rare earth oxide and 1-3 parts of sintering aid.

Description

Alumina ceramic material for thermal quantity sensor
Technical Field
The invention relates to the field of ceramic materials, in particular to an alumina ceramic material for a thermal quantity sensor.
Background
Thermal mass sensors are of various kinds, including but not limited to heat flow sensors, thermometers, temperature sensors, total radiation pyrometers, etc., and are widely used in many fields as a basic tool for measuring heat transfer (heat flux density or heat flux).
The thermal quantity sensor in the aerospace field must withstand the investigation of severe environments, especially repeated high-low temperature alternation, the plastic housing of the thermal quantity sensor generally cannot withstand repeated alternating cold and hot impact and is easy to crack, the metal housing is easy to become brittle due to expansion and contraction, the aluminum oxide ceramic has higher hardness and good mechanical property, the thermal expansion coefficient is low, the aluminum oxide ceramic is often used for manufacturing a substrate or a housing of an electronic component, and is an ideal material for manufacturing the housing of the thermal quantity sensor, but the use of the aluminum oxide ceramic in the aerospace field is restricted by the poor thermal shock property.
Disclosure of Invention
The invention aims to: in order to solve the technical problems, the invention provides an alumina ceramic material for a thermal quantity sensor.
The technical scheme adopted is as follows:
an alumina ceramic material for a thermal quantity sensor comprises the following raw materials in parts by weight:
60-80 parts of titanium sol coated alumina powder, 20-30 parts of nano silicon dioxide, 0.1-0.5 part of graphene oxide, 10-20 parts of yttrium aluminum garnet pre-powder, 2-5 parts of rare earth oxide and 1-3 parts of sintering aid.
Further, the alumina ceramic material comprises the following raw materials in parts by weight:
75 parts of titanium sol coated alumina powder, 25 parts of nano silicon dioxide, 0.25 part of graphene oxide, 18 parts of yttrium aluminum garnet pre-powder, 3 parts of rare earth oxide and 1 part of sintering aid.
Further, the preparation method of the titanium sol coated alumina powder comprises the following steps:
and (3) uniformly mixing butyl titanate, acetylacetone and the first part of absolute ethyl alcohol, heating to 60-70 ℃, dropwise adding a mixture consisting of water, concentrated hydrochloric acid and the second part of absolute ethyl alcohol, continuously stirring until a reaction system gradually turns into light yellowish green sol from colorless transparent liquid, mixing alumina powder with the sol, ball milling, and drying.
Further, acetic acid was added during ball milling.
Further, the preparation method of the yttrium aluminum garnet pre-powder comprises the following steps:
adding yttrium nitrate, aluminum nitrate and citric acid into a mixed solvent consisting of water and absolute ethyl alcohol, stirring and heating to 65-75 ℃, preserving heat for 1-3 hours, heating to 85-95 ℃, continuously stirring to evaporate the solvent to obtain gel, transferring the gel into a muffle furnace with the temperature of 200-250 ℃ for combustion, grinding the obtained product, heating to 750-850 ℃ and presintering for 1-2 hours.
Further, the ratio of the sum of the amounts of the substances of yttrium nitrate and aluminum nitrate to the amount of the substance of citric acid is 1:0.6-1.
Further, the rare earth oxide is any one or a combination of more of lanthanum oxide, cerium oxide, samarium oxide, neodymium oxide and yttrium oxide, preferably lanthanum oxide and neodymium oxide, and the weight ratio of the lanthanum oxide to the neodymium oxide is 1-5:1-5.
Further, the sintering aid comprises aluminum trifluoride, vanadium oxide and lithium carbonate, wherein the weight ratio of the aluminum trifluoride to the vanadium oxide to the lithium carbonate is 4-8:4-8:0.5-2.
The invention also provides a preparation method of the alumina ceramic material, which comprises the following steps:
mixing titanium sol coated alumina powder, nano silicon dioxide, graphene oxide, yttrium aluminum garnet pre-powder, rare earth oxide and sintering aid, ball milling, granulating, performing cold isostatic pressing, and obtaining a blank, heating the blank to 800-900 ℃ in the first stage under ammonia atmosphere, performing heat preservation and sintering for 3-5h, replacing ammonia with air, heating to 1600-1700 ℃ in the second stage, and performing heat preservation and sintering for 2-4h.
Further, the first stage heating speed is 10-30 ℃/min, and the second stage heating speed is 1-5 ℃/min.
The invention has the beneficial effects that:
the invention provides an alumina ceramic material for a thermal quantity sensor, which can better improve the sintering activity of alumina by coating the alumina powder with titanium sol, reduce the sintering temperature, wherein during the sintering process, the titanium sol is peeled off from the surface of the alumina powder into fine particles, the filling effect is achieved on the pores inside the ceramic material, nano silicon dioxide can obtain stable silicate liquid phase at high temperature, promote sintering, reduce the sintering temperature, refine crystal grains, improve the mechanical property of the alumina ceramic material, and under the action of a sintering auxiliary agent, mullite whiskers are generated, the pinning and bridging effects of the mullite whiskers can obstruct microcrack aggregation into critical cracks, so that the thermal shock resistance of the alumina ceramic material is improved, the adding of yttrium aluminum garnet pre-powder can not only play a role of enhancing the high temperature, but also can improve the mechanical property of the alumina ceramic material to a certain extent, the graphene oxide can also improve the mechanical property of the alumina ceramic material, and can be used as a reducing agent during the sintering under the ammonia atmosphere, the generation of metal nitride with excellent thermal conductivity is promoted, the thermal shock resistance of the alumina ceramic material is improved, the thermal shock resistance of the ceramic material is improved, and the thermal shock resistance of the ceramic material prepared with good thermal shock resistance is better than 10% and the thermal shock resistance is better than the thermal shock resistance of the ceramic material, and the thermal shock resistance is not lost after the thermal shock resistance is 20%.
Drawings
FIG. 1 is an SEM image of an alumina ceramic material prepared in example 1 of the invention.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Example 1:
an alumina ceramic material for a thermal quantity sensor comprises the following raw materials in parts by weight:
75 parts of titanium sol coated alumina powder, 25 parts of nano silicon dioxide, 0.25 part of graphene oxide, 18 parts of yttrium aluminum garnet pre-powder, 2 parts of lanthanum oxide, 1 part of neodymium oxide, 0.4 part of aluminum trifluoride, 0.4 part of vanadium oxide and 0.2 part of lithium carbonate.
The preparation method of the titanium sol coated alumina powder comprises the following steps:
mixing 85g of butyl titanate, 7.5g of acetylacetone and 150ml of absolute ethyl alcohol uniformly, heating to 70 ℃, dropwise adding a mixture consisting of 18ml of water, 42ml of concentrated hydrochloric acid and 100ml of absolute ethyl alcohol, continuously stirring for 2.5h, gradually changing the reaction system from colorless transparent liquid into light yellowish green sol, stopping heating until the reaction system naturally cools, adding 100g of alumina powder together with the sol into a ball milling tank, adding grinding balls and 1ml of acetic acid to promote gelation, mixing and ball milling for 5h after the ball milling tank is sealed, taking out the obtained mixture, and drying for 24h at 80 ℃.
The preparation method of the yttrium aluminum garnet pre-powder comprises the following steps:
82.5g of yttrium nitrate, 106.5g of aluminum nitrate and 122.9g of citric acid are added into a mixed solvent consisting of 250ml of water and 250ml of absolute ethyl alcohol, the temperature is raised to 75 ℃ for 2 hours, the temperature is raised to 95 ℃ after the temperature is kept for 2 hours, the solvent is continuously stirred to evaporate for 5 hours, gel is obtained, the gel is transferred into a muffle furnace with 220 ℃ for burning, and the obtained product is ground and then is raised to 800 ℃ for presintering for 1-2 hours.
The preparation method of the alumina ceramic material comprises the following steps:
mixing titanium sol coated alumina powder, nano silicon dioxide, graphene oxide, yttrium aluminum garnet pre-powder, lanthanum oxide, neodymium oxide, aluminum trifluoride, vanadium oxide and lithium carbonate, ball milling for 10 hours, drying, adding 8wt% of PVA aqueous solution for granulation, adding the obtained granules into a die, performing cold isostatic pressing for 100 seconds under 120MPa to form a blank, heating the blank to 800 ℃ at a speed of 20 ℃/min under an ammonia atmosphere, performing heat preservation and sintering for 4 hours, replacing ammonia with air, heating to 1650 ℃ at a speed of 2 ℃/min, and performing heat preservation and sintering for 3 hours.
Example 2:
an alumina ceramic material for a thermal quantity sensor comprises the following raw materials in parts by weight:
80 parts of titanium sol coated alumina powder, 30 parts of nano silicon dioxide, 0.1-0.5 part of graphene oxide, 20 parts of yttrium aluminum garnet pre-powder, 2 parts of lanthanum oxide, 1 part of neodymium oxide, 0.4 part of aluminum trifluoride, 0.4 part of vanadium oxide and 0.2 part of lithium carbonate.
Wherein, the preparation method of titanium sol coated alumina powder and yttrium aluminum garnet pre-powder is the same as in example 1.
The preparation method of the alumina ceramic material comprises the following steps:
mixing titanium sol coated alumina powder, nano silicon dioxide, graphene oxide, yttrium aluminum garnet pre-powder, lanthanum oxide, neodymium oxide, aluminum trifluoride, vanadium oxide and lithium carbonate, ball milling, granulating, performing cold isostatic pressing to obtain a blank, heating the blank to 900 ℃ at a speed of 30 ℃/min under an ammonia atmosphere, performing heat preservation and sintering for 5 hours, replacing ammonia with air, heating to 1700 ℃ at a speed of 5 ℃/min, and performing heat preservation and sintering for 4 hours.
Example 3:
an alumina ceramic material for a thermal quantity sensor comprises the following raw materials in parts by weight:
60 parts of titanium sol coated alumina powder, 20 parts of nano silicon dioxide, 0.1-0.5 part of graphene oxide, 10 parts of yttrium aluminum garnet pre-powder, 2 parts of lanthanum oxide, 1 part of neodymium oxide, 0.4 part of aluminum trifluoride, 0.4 part of vanadium oxide and 0.2 part of lithium carbonate.
Wherein, the preparation method of titanium sol coated alumina powder and yttrium aluminum garnet pre-powder is the same as in example 1.
The preparation method of the alumina ceramic material comprises the following steps:
mixing titanium sol coated alumina powder, nano silicon dioxide, graphene oxide, yttrium aluminum garnet pre-powder, lanthanum oxide, neodymium oxide, aluminum trifluoride, vanadium oxide and lithium carbonate, ball milling, granulating, performing cold isostatic pressing to obtain a blank, heating the blank to 800 ℃ at a speed of 10 ℃/min under an ammonia atmosphere, performing heat preservation and sintering for 3 hours, replacing ammonia with air, heating to 1600 ℃ at a speed of 1 ℃/min, and performing heat preservation and sintering for 2 hours.
Example 4:
an alumina ceramic material for a thermal quantity sensor comprises the following raw materials in parts by weight:
80 parts of titanium sol coated alumina powder, 20 parts of nano silicon dioxide, 0.1-0.5 part of graphene oxide, 20 parts of yttrium aluminum garnet pre-powder, 2 parts of lanthanum oxide, 1 part of neodymium oxide, 0.4 part of aluminum trifluoride, 0.4 part of vanadium oxide and 0.2 part of lithium carbonate.
Wherein, the preparation method of titanium sol coated alumina powder and yttrium aluminum garnet pre-powder is the same as in example 1.
The preparation method of the alumina ceramic material comprises the following steps:
mixing titanium sol coated alumina powder, nano silicon dioxide, graphene oxide, yttrium aluminum garnet pre-powder, lanthanum oxide, neodymium oxide, aluminum trifluoride, vanadium oxide and lithium carbonate, ball milling, granulating, performing cold isostatic pressing to obtain a blank, heating the blank to 900 ℃ at a speed of 10 ℃/min under an ammonia atmosphere, performing heat preservation and sintering for 3 hours, replacing ammonia with air, heating to 1700 ℃ at a speed of 5 ℃/min, and performing heat preservation and sintering for 4 hours.
Example 5:
an alumina ceramic material for a thermal quantity sensor comprises the following raw materials in parts by weight:
60 parts of titanium sol coated alumina powder, 30 parts of nano silicon dioxide, 0.1-0.5 part of graphene oxide, 10 parts of yttrium aluminum garnet pre-powder, 2 parts of lanthanum oxide, 1 part of neodymium oxide, 0.4 part of aluminum trifluoride, 0.4 part of vanadium oxide and 0.2 part of lithium carbonate.
Wherein, the preparation method of titanium sol coated alumina powder and yttrium aluminum garnet pre-powder is the same as in example 1.
The preparation method of the alumina ceramic material comprises the following steps:
mixing titanium sol coated alumina powder, nano silicon dioxide, graphene oxide, yttrium aluminum garnet pre-powder, lanthanum oxide, neodymium oxide, aluminum trifluoride, vanadium oxide and lithium carbonate, ball milling, granulating, performing cold isostatic pressing to obtain a blank, heating the blank to 800 ℃ at a speed of 30 ℃/min under an ammonia atmosphere, performing heat preservation and sintering for 5 hours, replacing ammonia with air, heating to 1700 ℃ at a speed of 1 ℃/min, and performing heat preservation and sintering for 2 hours.
Comparative example 1:
substantially the same as in example 1, except that the alumina powder was directly added without being subjected to the titanium sol coating.
Comparative example 2:
substantially the same as in example 1, except that no nanosilica was added.
Comparative example 3:
substantially the same as in example 1, except that graphene oxide was not added.
Comparative example 4:
substantially the same as in example 1, except that the yttrium aluminum garnet preform powder was not added.
Performance test:
the alumina ceramic materials prepared in examples 1 to 5 and comparative examples 1 to 4 of the present invention were used as test pieces;
bending strength test: the test is carried out according to GB/T6569-2006, the loading speed is 0.5mm/min, unit: MPa;
the fracture toughness characterization material has the capability of preventing crack propagation, is a quantitative index for measuring the toughness of ceramics, and is calculated by adopting an indentation method after a sample is ground and polished, and the unit is: MPa.m 1/2 ；
The thermal shock treatment method comprises the following steps: heating the sample to 1100 ℃ and preserving heat for 30min, taking out the sample, cooling to room temperature by air, cooling to-40 ℃ and preserving heat for 10min, taking out the sample, cooling to room temperature by air, repeating the cycle for 20 times, testing the bending strength and the fracture toughness of the sample, and calculating the loss rate of the bending strength and the fracture toughness of the sample in units: in%, if a crack visually observable at the time of the test appears, the test is stopped and the number of cycles is recorded.
The performance test results are shown in table 1:
table 1:
as shown in the table 1, the alumina ceramic material prepared by the invention has good mechanical property, good thermal shock resistance, no crack after 20 times of cold and hot alternation, and the loss rate of bending strength and fracture toughness is less than 10%.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. An alumina ceramic material for a thermal quantity sensor is characterized by comprising the following raw materials in parts by weight:
60-80 parts of titanium sol coated alumina powder, 20-30 parts of nano silicon dioxide, 0.1-0.5 part of graphene oxide, 10-20 parts of yttrium aluminum garnet pre-powder, 2-5 parts of rare earth oxide and 1-3 parts of sintering aid.
2. The alumina ceramic material of claim 1, comprising the following raw materials in parts by weight:
75 parts of titanium sol coated alumina powder, 25 parts of nano silicon dioxide, 0.25 part of graphene oxide, 18 parts of yttrium aluminum garnet pre-powder, 3 parts of rare earth oxide and 1 part of sintering aid.
3. The alumina ceramic material of claim 1, wherein the titanium sol coated alumina powder is prepared by the following method:
and (3) uniformly mixing butyl titanate, acetylacetone and the first part of absolute ethyl alcohol, heating to 60-70 ℃, dropwise adding a mixture consisting of water, concentrated hydrochloric acid and the second part of absolute ethyl alcohol, continuously stirring until a reaction system gradually turns into light yellowish green sol from colorless transparent liquid, mixing alumina powder with the sol, ball milling, and drying.
4. An alumina ceramic material according to claim 3, wherein acetic acid is added during ball milling.
5. The alumina ceramic material of claim 1, wherein the yttrium aluminum garnet pre-powder is prepared by the following method:
adding yttrium nitrate, aluminum nitrate and citric acid into a mixed solvent consisting of water and absolute ethyl alcohol, stirring and heating to 65-75 ℃, preserving heat for 1-3 hours, heating to 85-95 ℃, continuously stirring to evaporate the solvent to obtain gel, transferring the gel into a muffle furnace with the temperature of 200-250 ℃ for combustion, grinding the obtained product, heating to 750-850 ℃ and presintering for 1-2 hours.
6. The alumina ceramic material of claim 5, wherein the ratio of the sum of the amounts of the substances of yttrium nitrate and aluminum nitrate to the amount of the substance of citric acid is 1:0.6-1.
7. The alumina ceramic material of claim 1, wherein the rare earth oxide is any one or more of lanthanum oxide, cerium oxide, samarium oxide, neodymium oxide, and yttrium oxide, preferably lanthanum oxide and neodymium oxide, and the weight ratio of lanthanum oxide to neodymium oxide is 1-5:1-5.
8. The alumina ceramic material of claim 1, wherein the sintering aid comprises aluminum trifluoride, vanadium oxide, and lithium carbonate in a weight ratio of 4-8:4-8:0.5-2.
9. A method for preparing an alumina ceramic material according to any one of claims 1 to 8, characterized by the following:
mixing titanium sol coated alumina powder, nano silicon dioxide, graphene oxide, yttrium aluminum garnet pre-powder, rare earth oxide and sintering aid, ball milling, granulating, performing cold isostatic pressing, and obtaining a blank, heating the blank to 800-900 ℃ in the first stage under ammonia atmosphere, performing heat preservation and sintering for 3-5h, replacing ammonia with air, heating to 1600-1700 ℃ in the second stage, and performing heat preservation and sintering for 2-4h.
10. The method for producing an alumina ceramic material according to claim 9, wherein the first stage is heated at a rate of 10 to 30 ℃/min and the second stage is heated at a rate of 1 to 5 ℃/min.
CN202310628058.XA 2023-05-31 2023-05-31 Alumina ceramic material for thermal quantity sensor Pending CN116751035A (en)

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* Cited by examiner, † Cited by third party
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JPH07165462A (en) * 1993-12-13 1995-06-27 Kurosaki Refract Co Ltd Alumina-beta-sialon-yag composite material
JPH11335159A (en) * 1998-05-25 1999-12-07 Kyocera Corp High-strength, high-hardness alumina ceramics and its production
KR101247125B1 (en) * 2011-10-19 2013-04-01 한국세라믹기술원 Manufacturing method of ceramic composites with high fracture strength
CN103922704A (en) * 2013-01-11 2014-07-16 罗伯特·博世有限公司 Ceramic Composition And Ceramic Injection-molding Process
US20170152424A1 (en) * 2015-11-26 2017-06-01 Korea Institute Of Ceramic Engineering & Technology Alumina Composite Ceramic Composition and Method of Manufacturing the Same
CN107793138A (en) * 2017-12-23 2018-03-13 刘彪 A kind of aluminium oxide ceramics
CN113277859A (en) * 2021-05-06 2021-08-20 郑州磨料磨具磨削研究所有限公司 Nano-coated alumina particles and high-purity thermal shock resistant alumina ceramic material prepared from same
CN114275767A (en) * 2021-12-27 2022-04-05 华中科技大学 Transition metal nitride/two-dimensional nitrogen-doped carbon composite material and preparation method thereof
CN114436632A (en) * 2022-01-19 2022-05-06 山东工业陶瓷研究设计院有限公司 High-temperature thermal shock resistant ceramic material and preparation method thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07165462A (en) * 1993-12-13 1995-06-27 Kurosaki Refract Co Ltd Alumina-beta-sialon-yag composite material
JPH11335159A (en) * 1998-05-25 1999-12-07 Kyocera Corp High-strength, high-hardness alumina ceramics and its production
KR101247125B1 (en) * 2011-10-19 2013-04-01 한국세라믹기술원 Manufacturing method of ceramic composites with high fracture strength
CN103922704A (en) * 2013-01-11 2014-07-16 罗伯特·博世有限公司 Ceramic Composition And Ceramic Injection-molding Process
US20170152424A1 (en) * 2015-11-26 2017-06-01 Korea Institute Of Ceramic Engineering & Technology Alumina Composite Ceramic Composition and Method of Manufacturing the Same
CN107793138A (en) * 2017-12-23 2018-03-13 刘彪 A kind of aluminium oxide ceramics
CN113277859A (en) * 2021-05-06 2021-08-20 郑州磨料磨具磨削研究所有限公司 Nano-coated alumina particles and high-purity thermal shock resistant alumina ceramic material prepared from same
CN114275767A (en) * 2021-12-27 2022-04-05 华中科技大学 Transition metal nitride/two-dimensional nitrogen-doped carbon composite material and preparation method thereof
CN114436632A (en) * 2022-01-19 2022-05-06 山东工业陶瓷研究设计院有限公司 High-temperature thermal shock resistant ceramic material and preparation method thereof

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