CN110642625A - Novel ternary composite powder and preparation method and application thereof - Google Patents

Novel ternary composite powder and preparation method and application thereof Download PDF

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CN110642625A
CN110642625A CN201910932050.6A CN201910932050A CN110642625A CN 110642625 A CN110642625 A CN 110642625A CN 201910932050 A CN201910932050 A CN 201910932050A CN 110642625 A CN110642625 A CN 110642625A
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powder
sic
ternary composite
composite powder
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郭伟明
袁进豪
吴利翔
牛文彬
詹创添
朱林林
林华泰
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Guangdong University of Technology
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Abstract

The invention belongs to the technical field of ceramic materials, and discloses novel ternary composite powder (Al)4SiC4‑Al4O4C-SiC), a preparation method and application thereof. The composite powder is prepared by mixing Si powder, Al powder and C powder, adding a solvent, stirring, performing ultrasonic treatment and drying; and (3) carrying out dry pressing on the mixed powder, then carrying out cold isostatic pressing on the mixed powder to obtain a green body, heating the green body to 1500-1800 ℃ in a protective atmosphere with oxygen partial pressure, calcining the green body, and grinding and sieving the green body to obtain the nano-composite material. The ternary composite powder has the advantages of corrosion resistance, high temperature resistance, slag corrosion resistance and the like, has wide source of adopted raw materials and lower cost, and can be applied to the field of porous ceramics for smelting molten metalThe feasibility is provided for industrial production.

Description

Novel ternary composite powder and preparation method and application thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to novel ternary composite powder (Al)4SiC4-Al4O4C-SiC), a preparation method and application thereof.
Background
Aluminum-containing ternary carbides are of interest because of their high temperature and chemical resistance, and can retain strength at high temperatures. Two of the most promising aluminum-containing ternary carbides are reported to be Al4SiC4And Al4O4C, these two materials have become the two most promising high temperature ceramics for engineering applications and are now used as refractory materials. Al (Al)4O4C is a promising antioxidant with low density, high temperature stability, good oxidation and hydration resistance, while Al is a promising antioxidant4SiC4Has the remarkable characteristics of high melting point, low density, relatively high toughness, high compressive strength, excellent oxidation resistance and hydration action at high temperature and the like, in Al4SiC4The surface of the protective layer can improve the oxidation resistance, Al4SiC4Can effectively promote the refinement of SiC grains. But the practical application is due to the production of high-purity Al4SiC4Difficulty in sampling and Al containing by-product having poor water-solubility4C3Limit Al4SiC4The use of (1).
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a novel ternary composite powder (Al)4SiC4-Al4O4C-SiC)。
Another object of the present invention is to provide the above Al4SiC4-Al4O4A preparation method of C-SiC ternary composite powder. The preparation process is simple, low in cost, easy to realize industrial production and controllable in powder purity and particle size.
It is still another object of the present invention to provide the above Al4SiC4-Al4O4Application of C-SiC ternary composite powder.
The purpose of the invention is realized by the following technical scheme:
novel ternary composite powder, wherein the molecular formula of the ternary composite powder is Al4SiC4-Al4O4C-SiC, mixing Si powder, Al powder and C powder, adding a solvent, stirring, performing ultrasonic treatment, and drying to obtain mixed powder; and then, carrying out dry pressing on the mixed powder, then carrying out cold isostatic pressing on the mixed powder to obtain a green body, heating the green body to 1500-1800 ℃ in a protective atmosphere with oxygen partial pressure, calcining the green body, and grinding and sieving the green body to obtain the nano-composite material.
Preferably, the molar ratio of the Si powder, the Al powder and the C powder is 1: (3-5): (3-5).
Preferably, the Al4SiC4-Al4O4Al in C-SiC powder4SiC4The particle size of (A) is 0.1-10 μm; al (Al)4O4The particle size of C is 0.1-10 μm; SiC with a particle size of 0.01 to 1 μm, the Al4SiC4-Al4O4The purity of the C-SiC powder is 95-99.9%.
Preferably, the solvent is one or more of ethanol, acetone, methanol or butanol.
Preferably, the protective atmosphere is N2Or Ar, wherein the oxygen mole percentage of the oxygen partial pressure is 0.1-5%.
Preferably, the stirring time is 10-30 min, the calcining time is 0.5-3 h, the pressure of the cold isostatic pressing is 100-300 MPa, the pressure maintaining time of the cold isostatic pressing is 1-30 min, and the rate of heating to 1500-1800 ℃ is 5-20 ℃/min.
The preparation method of the novel ternary composite powder comprises the following specific steps:
s1, mixing Si powder, Al powder and C powder, and performing magnetic stirring, ultrasonic treatment and drying to obtain mixed powder;
s2, mixing the mixed powderPlacing the body molded blank into a graphite crucible, then dry-pressing the mixed powder, then cooling and statically pressing the mixed powder into a blank, heating to 1500-1800 ℃ at the speed of 5-20 ℃/min under the protective atmosphere with oxygen partial pressure, preserving heat for 0.5-3 h, grinding and sieving to obtain Al4SiC4-Al4O4C-SiC ternary composite powder.
The novel ternary composite powder is applied to the field of porous ceramics smelted by molten metal.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention synthesizes Al in situ4SiC4-Al4O4The C-SiC ternary composite powder can realize the uniform distribution of the ternary composite powder, and Al4SiC4-Al4O4Al in C-SiC ternary composite powder4SiC4The SiC crystal grains can be obviously refined, so that the fine-grained SiC is dispersed and distributed in the ternary composite powder. When the composite powder is used as a raw material to prepare the porous ceramic of the system, the bending strength of the porous ceramic is obviously improved.
2. The invention is due to Al4SiC4And Al4O4The C bond formed a layer of calcium hexaaluminate (CA6) on the hot surface exhibiting good slag resistance, Al4SiC4And Al4O4The composition of the C powder has very good performances of oxidation resistance, high temperature resistance, slag erosion resistance and the like, while SiC has higher hardness and better performances of corrosion resistance, high temperature resistance and the like as a hard phase, so that SiC is applied to Al4SiC4-Al4O4The dispersion distribution of the C powder can obviously improve the performance of the composite powder for preparing the porous ceramic, so that the Al4SiC4-Al4O4The C-SiC ternary composite powder has great industrial application value, and is especially suitable for porous ceramic field in smelting molten metal.
3. The invention takes Si powder, Al powder and C powder as raw materials, the powders are fully mixed by magnetic stirring and ultrasonic, and Al is generated after calcination4SiC4-Al4O4C-SiC IIIA composite powder. Al prepared by the in-situ synthesis method in an adjustable and controllable manner4SiC4-Al4O4The powder of C-SiC has a high purity and a small particle diameter and does not contain Al having poor water resistance4C3。
4. The invention synthesizes Al in situ4SiC4-Al4O4The C-SiC ternary composite powder has low raw material cost and wide source, and is easy for industrial production.
Drawings
FIG. 1 shows Al in example 14SiC4-Al4O4XRD pattern of C-SiC powder.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. Al (purity of powder 99.9%, particle diameter 3 μm), Si (purity of powder 99.9%, particle diameter 1 μm) powder and carbon black (purity of 99.9%, particle diameter 1 μm) were used as raw materials, wherein Al: si: and C is in a molar ratio of 4:1:4, ethanol is used as a solvent, the mixture is mixed for 10min under magnetic stirring, ultrasonic dispersion is carried out for 10min, and the mixed powder is obtained after rotary evaporation and drying.
2. Molding the mixed powder for 2min at a pressure of 3MPa, continuously keeping the pressure of 200MPa for 5min at cold isostatic pressure, putting the blank into a graphite crucible, heating to 1700 ℃ at a speed of 15 ℃/min, keeping the temperature for 1h, wherein the protective atmosphere is argon, the oxygen content in the protective atmosphere is 1%, grinding and sieving the composite powder obtained by heat treatment to obtain Al4SiC4-Al4O4C-SiC ternary composite powder.
Al produced in this example4SiC4-Al4O4The phase of the C-SiC ternary composite powder is shown in FIG. 1, and as can be seen from FIG. 1, the main phase of the powder prepared is Al4SiC4Besides, it is mainly Al4O4C and SiC phase, Al is realized for the first time4SiC4-Al4O4And (3) synthesizing C-SiC ternary composite powder. Al produced in this example4SiC4-Al4O4Al in C-SiC ternary composite powder4SiC4Has a particle diameter of 1 μm, Al4O4The grain diameter of C is 1 μm, the grain diameter of SiC is 0.1 μm, and the Al4SiC4-Al4O4The purity of the C-SiC ternary composite powder is 99%.
Example 2
Using Al (purity of powder 99.9%, particle size 0.1 μm), Si (purity of powder 99.9%, particle size 0.1 μm) powder and amorphous carbon (purity of 99.9%, particle size 0.1 μm) as raw materials, mixing Al: si: mixing the components according to the embodiment 1 with the molar ratio of C of 4.5:1:4, molding the mixed powder, heating to 1500 ℃ at the speed of 5 ℃/min, keeping the temperature for 0.5h, wherein the protective atmosphere is argon and the oxygen content in the protective atmosphere is 0.1%, grinding and sieving the composite powder obtained by heat treatment to obtain Al4SiC4-Al4O4C-SiC ternary composite powder.
Al produced in this example4SiC4-Al4O4Al in C-SiC ternary composite powder4SiC4Has a particle diameter of 0.1 μm, Al4O4The grain diameter of C is 0.1 μm, the grain diameter of SiC is 0.01 μm, and the Al4SiC4-Al4O4The purity of the C-SiC ternary composite powder is 99%.
Example 3
Using Al (purity of powder 99.9%, particle size 10 μm), Si (purity of powder 99.9%, particle size 10 μm) powder and graphite (purity of 99.9%, particle size 10 μm) as raw materials, mixing Al: si: mixing the components according to the embodiment 1 with the molar ratio of C of 4:1:4, molding the mixed powder, heating to 1800 ℃ at the speed of 5 ℃/min, keeping the temperature for 1h, grinding and sieving the composite powder obtained by heat treatment to obtain Al, wherein the protective atmosphere is argon and the oxygen content in the protective atmosphere is 5 percent4SiC4-Al4O4C-SiC ternary composite powder.
The true bookAl obtained in examples4SiC4-Al4O4Al in C-SiC ternary composite powder4SiC4Has a particle diameter of 5 μm, Al4O4The grain diameter of C is 5 μm, the grain diameter of SiC is 0.1 μm, and the Al4SiC4-Al4O4The purity of the C-SiC ternary composite powder is 99%.
Example 4
Using Al (purity of powder 99.9%, particle size 5 μm), Si (purity of powder 99.9%, particle size 5 μm) powder and amorphous carbon (purity of 99.9%, particle size 5 μm) as raw materials, mixing Al: si: mixing the components according to the embodiment 1 with the molar ratio of C of 4.5:1:4, molding the mixed powder, heating to 1600 ℃ at the speed of 5 ℃/min, keeping the temperature for 3 hours, grinding and sieving the composite powder obtained by heat treatment, wherein the protective atmosphere is argon and the oxygen content in the protective atmosphere is 2.5%, and Al is obtained4SiC4-Al4O4C-SiC ternary composite powder.
Al produced in this example4SiC4-Al4O4Al in C-SiC ternary composite powder4SiC4Has a particle diameter of 1 μm, Al4O4The grain diameter of C is 1 μm, the grain diameter of SiC is 0.1 μm, and the Al4SiC4-Al4O4The purity of the C-SiC ternary composite powder is 99%.
Example 5
Using Al (purity of powder 99.9%, particle size 0.01 μm), Si (purity of powder 99.9%, particle size 0.01 μm) powder and amorphous carbon (purity of 96.3%, particle size 0.01 μm) as raw materials, mixing Al: si: mixing the components according to the embodiment 1 with the molar ratio of C of 4.5:1:4, molding the mixed powder, heating to 1700 ℃ at the speed of 5 ℃/min, keeping the temperature for 0.5h, wherein the protective atmosphere is argon and the oxygen content in the protective atmosphere is 0.1%, grinding and sieving the composite powder obtained by heat treatment to obtain Al4SiC4-Al4O4C-SiC ternary composite powder.
Al produced in this example4SiC4-Al4O4Al in C-SiC ternary composite powder4SiC4Has a particle diameter of 0.1 μm, Al4O4C ofGrain size of 0.1 μm, grain size of SiC of 0.01 μm, and the Al4SiC4-Al4O4The purity of the C-SiC ternary composite powder is 99%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. The novel ternary composite powder is characterized in that the molecular formula of the ternary composite powder is Al4SiC4-Al4O4C-SiC, mixing Si powder, Al powder and C powder, adding a solvent, stirring, performing ultrasonic treatment, and drying to obtain mixed powder; and then dry-pressing the mixed powder, then performing isostatic pressing to prepare a blank, heating the blank to 1500-1800 ℃ in a protective atmosphere with oxygen partial pressure, calcining, grinding and sieving to obtain the powder.
2. The novel ternary composite powder according to claim 1, wherein the molar ratio of the Si powder to the Al powder to the C powder is 1: (3-5): (3-5).
3. The novel ternary composite powder according to claim 1, wherein Al in the composite powder is4SiC4The particle size of (A) is 0.1-10 μm; al (Al)4O4The particle size of C is 0.1-10 μm; the SiC grain diameter is 0.01-1 mu m, and the purity of the composite powder is 95-99.9%.
4. The ternary composite powder according to claim 1, wherein the solvent is one or more selected from ethanol, acetone, methanol and butanol.
5. The novel ternary composite powder according to claim 1, wherein the purities of the Al powder, the Si powder and the C powder are all 95 to 99%, and the particle diameters of the Al powder, the Si powder and the C powder are all 0.01 to 10 μm.
6. The ternary composite powder according to claim 1, wherein said protective atmosphere is N2Or Ar, wherein the oxygen mole percentage of the oxygen partial pressure is 0.1-5%.
7. The novel ternary composite powder according to claim 1, wherein the stirring time is 10 to 30min, and the calcining time is 0.5 to 3 hours.
8. The novel ternary composite powder according to claim 1, wherein the cold isostatic pressing pressure is 100 to 300MPa, the cold isostatic pressing dwell time is 1 to 30min, and the rate of temperature rise to 1500 to 1800 ℃ is 5 to 20 ℃/min.
9. The method for preparing the novel ternary composite powder according to any one of claims 1 to 8, comprising the following specific steps:
s1, mixing Si powder, Al powder and C powder, and performing magnetic stirring, ultrasonic treatment and drying to obtain mixed powder;
s2, placing the mixed powder molded blank into a graphite crucible, performing dry pressing, performing isostatic pressing to obtain a blank, heating to 1500-1800 ℃ at the speed of 5-20 ℃/min under the protective atmosphere with oxygen partial pressure, preserving heat for 0.5-3 h, grinding, and sieving to obtain Al4SiC4-Al4O4C-SiC ternary composite powder.
10. The use of the novel ternary composite powder of any one of claims 1 to 8 in the field of porous ceramics in molten metal melting.
CN201910932050.6A 2019-09-29 2019-09-29 Novel ternary composite powder and preparation method and application thereof Pending CN110642625A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116120070A (en) * 2023-02-27 2023-05-16 宜兴金君耐火炉料有限公司 Silicon oxynitride-silicon carbide composite brick with enhanced oxidation resistance and preparation method thereof

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CN106631026A (en) * 2017-01-09 2017-05-10 武汉科技大学 Al<4>SiC<4>-Al<4>O<4>C compound materials and preparation method thereof
CN107687025A (en) * 2017-09-06 2018-02-13 武汉科技大学 A kind of Al4O4The synthetic method of C whiskers/carbon nano tube compound material
CN107814575A (en) * 2017-11-03 2018-03-20 江苏高淳陶瓷股份有限公司 A kind of Al4SiC4Silicon carbide honeycomb ceramics of enhancing and preparation method thereof
CN107814583A (en) * 2017-11-03 2018-03-20 江苏高淳陶瓷股份有限公司 A kind of Al4O4Silicon carbide honeycomb ceramics of C enhancings and preparation method thereof

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CN101659554A (en) * 2009-09-02 2010-03-03 中钢集团洛阳耐火材料研究院有限公司 Preparation process of antioxidant composite powder
CN106631026A (en) * 2017-01-09 2017-05-10 武汉科技大学 Al<4>SiC<4>-Al<4>O<4>C compound materials and preparation method thereof
CN107687025A (en) * 2017-09-06 2018-02-13 武汉科技大学 A kind of Al4O4The synthetic method of C whiskers/carbon nano tube compound material
CN107814575A (en) * 2017-11-03 2018-03-20 江苏高淳陶瓷股份有限公司 A kind of Al4SiC4Silicon carbide honeycomb ceramics of enhancing and preparation method thereof
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116120070A (en) * 2023-02-27 2023-05-16 宜兴金君耐火炉料有限公司 Silicon oxynitride-silicon carbide composite brick with enhanced oxidation resistance and preparation method thereof

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Application publication date: 20200103