CN110922195A - Method for preparing magnesium aluminate spinel-silicon carbide composite material by in-situ reaction - Google Patents

Method for preparing magnesium aluminate spinel-silicon carbide composite material by in-situ reaction Download PDF

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CN110922195A
CN110922195A CN201910983956.0A CN201910983956A CN110922195A CN 110922195 A CN110922195 A CN 110922195A CN 201910983956 A CN201910983956 A CN 201910983956A CN 110922195 A CN110922195 A CN 110922195A
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composite material
mgal
sic
situ reaction
silicon carbide
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CN110922195B (en
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石春杰
邰燕芳
李倩
杨青
陈雪
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Bengbu College
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    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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Abstract

The invention discloses a method for preparing a magnesium aluminate spinel-silicon carbide composite material by an in-situ reaction, which comprises the following steps: 1) weighing 3-30% of Mg, 10-50% of Al, 30-50% of phenolic resin and 30-50% of Si powder according to mass percent, and fully grinding; 2) fully and uniformly stirring the obtained mixed powder, heating to 650-1000 ℃ at the speed of 5-10 ℃/min under the condition of vacuum or argon atmosphere, and sintering for 2 h; 3) after the obtained loose block material is primarily crushed, ethanol is used as a dispersing agent, and the mass ratio of the crushed material to the ethanol to the balls is controlled to be 1: 3: 8, placing the mixture into a ball millBall milling for 1-2h to mix them thoroughly; 4) placing the material obtained after ball milling into a high-temperature furnace, and firing for 2-3h in the atmosphere of 1300-1500 ℃ air to obtain MgAl2O4a/SiC composite material. The invention firstly utilizes metal to assist in-situ reaction to generate nano SiC composite powder, and MgAl is formed after low-temperature oxidation2O4The SiC composite material has the advantages of simple process, low preparation temperature, good powder uniformity and low cost, and has higher application value in the field of refractory materials.

Description

Method for preparing magnesium aluminate spinel-silicon carbide composite material by in-situ reaction
Technical Field
The invention belongs to the field of material science, and particularly relates to a method for preparing nano MgAl through in-situ reaction2O4The method of the/SiC composite material is mainly applied to refractory material raw materials and additives.
Background
The magnesia-alumina spinel refractory material has excellent thermal shock resistance, good erosion resistance and abrasion resistance, and the SiC material has the characteristics of high temperature resistance, abrasion resistance, high strength, good thermal conductivity, excellent thermal shock resistance and the like, and has strong alkali metal oxide erosion resistance. Therefore, the magnesium aluminate spinel and the silicon carbide material are compounded to obtain a new material with better performance. At present, the relevant refractory materials are applied to high-temperature thermal equipment with harsh conditions and complex working conditions, such as blast furnace tapping runners, carbon sintering furnaces, coal water slurry gasification furnaces and other fields.
Because of the strong covalent nature of the Si-C bond, the sintering diffusion rate of SiC is very low, and in addition, SiO is on the surface of SiC particles2The barrier effect of the film, SiC is difficult to sinter, and a dense sintered body can be obtained by means of additives or pressure, and the like, namely, a second phase is required to be introduced as a binding phase in the conventional preparation process of the SiC refractory material. MgAl2O4As an excellent refractory material, the high expansion coefficient of the MgAl alloy can well supplement sintering pores and improve high-temperature compactness in the preparation of refractory materials, but extensive research is already carried out due to the MgAl alloy2O4The preparation temperature is high (1800 ℃), the process is complex, the composite material prepared from the composite material is not introduced as a raw material or an additive, and the nano composite material combined with SiC is not reported. In addition, due to the influence of high hardness of SiC, it is difficult to obtain nano SiC by a mechanical method, and further difficult to obtain microscopically uniform MgAl2O4The SiC material cannot obtain a high-performance refractory material.
The invention has O at lower temperature for the first time2Under the participation condition, SiC-bonded magnesium aluminate spinel phase (MgAl) can be generated in the SiC/Al composite material2O4) Provides a new way for preparing the ultra-high temperature refractory material at low temperature.
Disclosure of Invention
The object of the invention is to have O at lower temperatures2Under the participation condition, SiC-bonded magnesium aluminate spinel phase (MgAl) can be generated in the SiC/Al composite material2O4) Further replace the traditional physical mixing process to prepare MgAl2O4the/SiC is more uniform. Compared with the traditional preparation of MgAl2O4Compared with the SiC technology, the preparation temperature of the composite material is low, the preparation technology is relatively simple, and the obtained MgAl2O4Can be microscopically combined with SiC materials, and provides a new way for preparing the ultrahigh temperature refractory material at low temperature.
The technical scheme of the invention is summarized as follows:
al synthesized by the invention2O3a/Al-based soluble composite material consisting of MgAl2O4And a nano SiC phase, and can be regulated and controlled by the proportion of the raw materials to obtain MgO-MgAl2O4/SiC and Al2O3-MgAl2O4The refractory composite material powder of/SiC is widely applied.
The above MgAl2O4The initial raw material composition of the/SiC composite material is proportioned according to the following reaction formula: si + C ═ SiC, Mg + Al + O2→MgAl2O4. The preparation method comprises the following steps of preparing materials according to the proportion of introduced Mg and Al, and processing to obtain composite powder, wherein the composite powder is prepared according to the following specific proportion: mg: 3-30%, Al: 10-50%, phenolic resin: 30-50%, Si powder: 30-50 percent.
MgAl2O4The preparation process of the/SiC composite material comprises the following steps:
1) weighing 3-30% of Mg, 10-50% of Al, 30-50% of phenolic resin and 30-50% of Si powder according to mass percent, and fully grinding to prepare mixed powder;
2) fully and uniformly stirring the mixed powder obtained in the step 1, putting the mixed powder into a vacuum furnace or an atmosphere furnace, heating the mixed powder to 650-1000 ℃ at the speed of 5-10 ℃/min under the condition of vacuum or argon atmosphere, and sintering the mixed powder for 2 hours to obtain a loose block material;
3) and (3) after the loose block material obtained in the step (2) is primarily crushed, adopting ethanol as a dispersing agent, and controlling the mass ratio of the crushed material to the ethanol to the balls to be 1: 3: 8, putting the mixture into a ball mill for ball milling for 1-2h, and fully mixing the mixture;
4) putting the material obtained after ball milling in the step 3 into a high-temperature furnace, and firing for 2-3h in an air atmosphere of 1300-1500 ℃ to obtain MgAl2O4a/SiC composite material.
Preferably, the ball milling speed is 350 rpm.
Preferably, the MgAl is2O4the/SiC composite material at least comprises MgO-MgAl2O4/SiC and Al2O3-MgAl2O4One kind of SiC material.
The invention has the beneficial effects that:
the invention firstly utilizes metal to assist in-situ reaction to generate nano SiC composite powder, and MgAl is formed after low-temperature oxidation2O4A composite material of/SiC. The material has simple process, low preparation temperature and good powder uniformity, and can be well adjusted to form MgO-MgAl through the raw material proportion2O4/SiC and Al2O3-MgAl2O4the/SiC composite material has low cost and higher application value in the field of refractory materials, and provides a new way for preparing the ultrahigh-temperature refractory material at low temperature.
Drawings
FIG. 1 is the preparation of nano MgAl according to the invention2O4A process flow diagram for a/SiC composite material;
FIG. 2 is MgAl2O4XRD analysis result of the/SiC sample shows that the main crystal phase is SiC and the other phases are MgAl2O4；
FIG. 3 is MgAl2O4A microscopic structure chart and an energy spectrum of the/SiC composite powder.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
Example 1
1) Weighing 3% of Mg, 27% of Al, 35% of phenolic resin and 35% of Si powder according to mass percent, and fully grinding to prepare mixed powder;
2) fully and uniformly stirring the mixed powder obtained in the step 1, heating to 800 ℃ at the speed of 9 ℃/min under the condition of vacuum or argon atmosphere, and sintering for 2h to obtain a loose block material;
3) and (3) after the loose block material obtained in the step (2) is primarily crushed, adopting ethanol as a dispersing agent, and controlling the mass ratio of the crushed material to the ethanol to the balls to be 1: 3: 8, putting the mixture into a ball mill to perform ball milling for 2 hours at the rotating speed of 350rpm so as to fully mix the mixture;
4) putting the material obtained after ball milling in the step 3 into a high-temperature furnace, and firing for 2h at 1350 ℃ in air atmosphere to obtain MgAl2O4a/SiC composite material of the MgAl2O4the/SiC composite material is Al2O3-MgAl2O4a/SiC composite material.
Example 2
1) Weighing 10% of Mg, 20% of Al, 35% of phenolic resin and 35% of Si powder according to the mass percentage, and fully grinding to prepare mixed powder;
2) fully and uniformly stirring the mixed powder obtained in the step 1, heating to 750 ℃ at the speed of 10 ℃/min under the condition of vacuum or argon atmosphere, and sintering for 2h to obtain a loose block material;
3) and (3) after the loose block material obtained in the step (2) is primarily crushed, adopting ethanol as a dispersing agent, and controlling the mass ratio of the crushed material to the ethanol to the balls to be 1: 3: 8, putting the mixture into a ball mill to perform ball milling for 2 hours at the rotating speed of 350rpm so as to fully mix the mixture;
4) putting the material obtained after ball milling in the step 3 into a high-temperature furnace, and firing for 2h at 1350 ℃ in air atmosphere to obtain MgAl2O4a/SiC composite material of the MgAl2O4the/SiC composite material comprises Al2O3-MgAl2O4(iii) SiC and MgO-MgAl2O4a/SiC composite material.
Example 3
1) Weighing 15% of Mg, 15% of Al, 35% of phenolic resin and 35% of Si powder according to mass percent, and fully grinding to prepare mixed powder;
2) fully and uniformly stirring the mixed powder obtained in the step 1, heating to 800 ℃ at the speed of 8 ℃/min under the condition of vacuum or argon atmosphere, and sintering for 2h to obtain a loose block material;
3) and (3) after the loose block material obtained in the step (2) is primarily crushed, adopting ethanol as a dispersing agent, and controlling the mass ratio of the crushed material to the ethanol to the balls to be 1: 3: 8, putting the mixture into a ball mill to perform ball milling for 2 hours at the rotating speed of 350rpm so as to fully mix the mixture;
4) putting the material obtained after ball milling in the step 3 into a high-temperature furnace, and firing for 3 hours at 1450 ℃ in air atmosphere to obtain MgAl2O4a/SiC composite material of the MgAl2O4the/SiC composite material is MgO-MgAl2O4a/SiC composite material.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.

Claims (3)

1. A method for preparing a magnesium aluminate spinel-silicon carbide composite material through in-situ reaction is characterized by comprising the following steps:
1) weighing 3-30% of Mg, 10-50% of Al, 30-50% of phenolic resin and 30-50% of Si powder according to mass percent, and fully grinding to prepare mixed powder;
2) fully and uniformly stirring the mixed powder obtained in the step 1, heating to 650-1000 ℃ at the speed of 5-10 ℃/min under the condition of vacuum or argon atmosphere, and sintering for 2h to obtain a loose block material;
3) and (3) after the loose block material obtained in the step (2) is primarily crushed, adopting ethanol as a dispersing agent, and controlling the mass ratio of the crushed material to the ethanol to the balls to be 1: 3: 8, putting the mixture into a ball mill for ball milling for 1-2h, and fully mixing the mixture;
4) putting the material obtained after ball milling in the step 3 into a high-temperature furnace, and firing for 2-3h in an air atmosphere of 1300-1500 ℃ to obtain MgAl2O4a/SiC composite material.
2. The method for preparing the magnesium aluminate spinel-silicon carbide composite material through the in-situ reaction is characterized in that the ball milling rotating speed is 350 rpm.
3. The method for preparing the magnesium aluminate spinel-silicon carbide composite material through the in-situ reaction according to claim 1, wherein the MgAl is2O4the/SiC composite material at least comprises MgO-MgAl2O4/SiC and Al2O3-MgAl2O4One kind of SiC material.
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CN111704466A (en) * 2020-07-07 2020-09-25 中钢集团洛阳耐火材料研究院有限公司 Silicon carbide-magnesium aluminate spinel-aluminum composite refractory material
CN115504449A (en) * 2022-06-10 2022-12-23 四川大学 Method and material for F-doped modified phenolic resin base

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111704466A (en) * 2020-07-07 2020-09-25 中钢集团洛阳耐火材料研究院有限公司 Silicon carbide-magnesium aluminate spinel-aluminum composite refractory material
CN111704466B (en) * 2020-07-07 2021-09-21 中钢集团洛阳耐火材料研究院有限公司 Silicon carbide-magnesium aluminate spinel-aluminum composite refractory material
CN115504449A (en) * 2022-06-10 2022-12-23 四川大学 Method and material for F-doped modified phenolic resin base
CN115504449B (en) * 2022-06-10 2023-11-03 四川大学 F-doped modified phenolic resin based method and material

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