CN103274701A - Preparation method of carbonous refractory material antioxidant Al4O4C - Google Patents
Preparation method of carbonous refractory material antioxidant Al4O4C Download PDFInfo
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- CN103274701A CN103274701A CN2013101850460A CN201310185046A CN103274701A CN 103274701 A CN103274701 A CN 103274701A CN 2013101850460 A CN2013101850460 A CN 2013101850460A CN 201310185046 A CN201310185046 A CN 201310185046A CN 103274701 A CN103274701 A CN 103274701A
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Abstract
The invention discloses a preparation method of a carbonous refractory material antioxidant Al4O4C. The preparation method comprises the following steps of: (1) weighing raw materials including Al2O3 powder, Al powder and graphite powder in a molar ratio of n(Al2O3) to n(Al) to n(C) of a:b:3, and performing ball milling on the prepared raw materials in a ball milling pot for 4-12 hours at a rotating speed of 200-600r/min, wherein a is more than or equal to 1.0 and less than or equal to 6.0, and b is more than or equal to 1.0 and less than or equal to 6.0; and (2) putting the powder obtained after ball milling into a graphite or hard alloy mold, putting the mold into an SPS (Spark Plasma Sintering) sintering cavity, applying an axial pressure of 10-50MPa, sintering under a vacuum condition that the atmospheric pressure of a sintering atmosphere is lower than 10Pa, raising the temperature at a temperature rise rate of 100-150 DEG C/min, maintaining the sintering temperature to be 1000-1500 DEG C for 5-15minutes, and cooling to the room temperature together with a furnace to obtain a single-phase block material of which the phase composition is an Al4O4C crystalline phase. The preparation method is simple, low in cost, high in sintering temperature rise speed, low in sintering temperature, short in sintering time and capable of obtaining a single-phase material without impurity phases.
Description
Technical field
The invention belongs to the refractory materials preparing technical field, be particularly related to a kind of preparation method of carbon containing refractory antioxidant.
Background technology
Al
2O
3Carbon containing refractories such as-C system and MgO-C system are in order to prevent the oxidation of carbon in the material, and the method for employing interpolation metallic aluminium powder is improved the hot properties of refractory materials usually, but this method also exists some problems.Synthetic aluminium carbide (the Al of the reaction of the carbon in metallic aluminium and the refractory materials at high temperature for example
4C
3), in process of cooling, the easy and airborne moisture generation hydration reaction of aluminium carbide when heating up again, will cause the cracking of refractory materials.Because hydration reaction takes place in aluminium carbide easily, thus the method for adding metallic aluminium in the indefinite form carbon refractory of water combination, just can not be adopted, and the tiny metallic aluminium powder of granularity is easy the burning more, brings danger to operating process.Therefore need a kind of better additive to replace the aluminium powder additive.
According to Al
2O
3-Al
4C
3Phasor as can be known, in room temperature to 1890 ℃ temperature range, Al
4O
4C can stable existence.As at P
COUnder=0.101325MPa(=1atm) the CO atmospheric condition, since 800 ℃ of Al
4O
4C and CO gas reaction are without generating Al
4C
3Reaction process, direct reaction generates Al
2O
3And carbon, have the advantages that hydration reaction does not take place, so Al
4O
4C is considered to than the better refractory materials additive of metallic aluminium powder.
Most of vacuum oven, resistance furnace of adopting prepares Al at present
4O
4C, these method sintering temperature height, sintering time is long, and the present invention has adopted discharge plasma sintering (SPS) technology to be prepared.This preparation technology's advantage is fairly obvious: homogeneous heating, and heat-up rate is fast, and sintering temperature is low, and sintering time is short, and production efficiency height, product are organized tiny even, can keep raw-material state of nature, can obtain the material of high-compactness.
Summary of the invention
The object of the present invention is to provide the carbon containing refractory antioxidant Al that a kind of technical process is short, cost is low
4O
4The preparation method of C.
Discharge plasma sintering of the present invention (SPS) legal system is equipped with carbon containing refractory Al
4O
4The method of C.
The present invention adopts the method for discharge plasma sintering (SPS) to prepare carbon containing refractory Al
4O
4C, concrete steps are as follows:
1) with Al
2O
3Powder, Al powder, Graphite Powder 99 are raw material, according to mol ratio n (Al
2O
3): n(Al): n(C)=a:b:3 weighs, 1.0≤a≤6.0,1.0≤b≤6.0 wherein.The raw material for preparing is put into ball grinder carry out ball milling, ball milling time 4 ~ 12h, rotating speed are 200 ~ 600r/min.
2) powder behind the ball milling is packed in graphite or the sintered-carbide die, mould is placed the SPS sintering cavity, apply the axle pressure of 10 ~ 50MPa, be lower than sintering under the vacuum condition of 5Pa at total gas pressure, temperature rise rate with 100～150 ℃/min heats up, and sintering temperature is 1000 ~ 1500 ℃, insulation 5 ~ 15min, cool to room temperature with the furnace, obtain containing the Al of micro-C
2O
3And Al
4O
4The block of C.
Compared with prior art, the present invention has following beneficial effect:
(1) the inventive method technology is simple, and cost is low, and heat-up rate is fast during sintering, and sintering temperature is low, and sintering time is short, and can obtain Al
4O
4C is the single-phase block materials of crystalline phase, and does not have Al
4C
3Dephasign generates.
(2) can obtain single-phase Al by changing proportion of raw materials
4O
4The block materials of C.
Description of drawings
Fig. 1 is the carbon containing refractory Al by present method preparation
4O
4The XRD diffractogram of C block, thing phase composite are single Al
4O
4The C crystalline phase.
The invention will be further described below in conjunction with the drawings and specific embodiments, but protection scope of the present invention is not limited to following embodiment.
Embodiment
Embodiment 1
1) adopts ball mill, with Al
2O
3Powder, Al powder, Graphite Powder 99 are raw material, according to mol ratio n (Al
2O
3): n(Al): n(C)=4:4:3 weighs, and the raw material for preparing put into ball grinder carry out ball milling, and ball milling time 6h, rotating speed are 450r/min.
2) powder behind the ball milling is packed in graphite or the sintered-carbide die, mould is placed the SPS sintering cavity, apply the axle pressure of 10MPa, be lower than sintering under the vacuum condition of 5Pa at total gas pressure, temperature rise rate with 100 ℃/min heats up, and sintering temperature is 1200 ℃, insulation 5min, cool to room temperature with the furnace, obtaining the thing phase composite is Al
4O
4The single-phase block materials of C crystalline phase.
Embodiment 2
1) adopts ball mill, with Al
2O
3Powder, Al powder, Graphite Powder 99 are raw material, according to mol ratio n (Al
2O
3): n(Al): n(C)=2:2:3 weighs, and the raw material for preparing put into ball grinder carry out ball milling, and ball milling time 7h, rotating speed are 500r/min.
2) powder behind the ball milling is packed in graphite or the sintered-carbide die, mould is placed the SPS sintering cavity, apply the axle pressure of 20MPa, be lower than sintering under the vacuum condition of 5Pa at total gas pressure, temperature rise rate with 110 ℃/min heats up, and sintering temperature is 1300 ℃, insulation 8min, cool to room temperature with the furnace, obtaining the thing phase composite is Al
4O
4The single-phase block materials of C crystalline phase.
Embodiment 3
1) adopts ball mill, with Al
2O
3Powder, Al powder, Graphite Powder 99 are raw material, according to mol ratio n (Al
2O
3): n(Al): n(C)=2:2:3 weighs, and the raw material for preparing put into ball grinder carry out ball milling, and ball milling time 8h, rotating speed are 550r/min.
2) powder behind the ball milling is packed in graphite or the sintered-carbide die, mould is placed the SPS sintering cavity, apply the axle pressure of 30MPa, be lower than sintering under the vacuum condition of 5Pa at total gas pressure, temperature rise rate with 120 ℃/min heats up, and sintering temperature is 1400 ℃, insulation 10min, cool to room temperature with the furnace, obtaining the thing phase composite is Al
4O
4The single-phase block materials of C crystalline phase.
Embodiment 4
1) adopts ball mill, with Al
2O
3Powder, Al powder, Graphite Powder 99 are raw material, according to mol ratio n (Al
2O
3): n(Al): n(C)=4:4:3 weighs, and the raw material for preparing put into ball grinder carry out ball milling, and ball milling time 9h, rotating speed are 600r/min.
2) powder behind the ball milling is packed in graphite or the sintered-carbide die, mould is placed the SPS sintering cavity, apply the axle pressure of 40MPa, be lower than sintering under the vacuum condition of 5Pa at total gas pressure, temperature rise rate with 150 ℃/min heats up, and sintering temperature is 1500 ℃, insulation 15min, cool to room temperature with the furnace, obtaining the thing phase composite is Al
4O
4The single-phase block materials of C crystalline phase.
Claims (1)
1. carbon containing refractory antioxidant Al
4O
4The preparation method of C is characterized in that, may further comprise the steps:
1) with Al
2O
3Powder, Al powder, Graphite Powder 99 are raw material, according to mol ratio n (Al
2O
3): n(Al): n(C)=a:b:3 weighs, 1.0≤a≤6.0,1.0≤b≤6.0 wherein; The raw material for preparing is put into ball grinder carry out ball milling, ball milling time 4 ~ 12h, rotating speed are 200 ~ 600r/min; 2) powder behind the ball milling is packed in graphite or the sintered-carbide die, mould is placed the SPS sintering cavity, apply the axle pressure of 10 ~ 50MPa, be lower than sintering under the vacuum condition of 10Pa at sintering atmosphere pressure, temperature rise rate with 60～150 ℃/min heats up, 1000 ~ 1500 ℃ of sintering temperatures, insulation 5 ~ 15min, cool to room temperature with the furnace, obtaining the thing phase composite is Al
4O
4C is the single-phase block materials of crystalline phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101850460A CN103274701A (en) | 2013-05-19 | 2013-05-19 | Preparation method of carbonous refractory material antioxidant Al4O4C |
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|---|---|---|---|
| CN2013101850460A CN103274701A (en) | 2013-05-19 | 2013-05-19 | Preparation method of carbonous refractory material antioxidant Al4O4C |
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| CN103274701A true CN103274701A (en) | 2013-09-04 |
Family
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| CN2013101850460A Pending CN103274701A (en) | 2013-05-19 | 2013-05-19 | Preparation method of carbonous refractory material antioxidant Al4O4C |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896315A (en) * | 2014-03-25 | 2014-07-02 | 中国科学院金属研究所 | Al2OC nanowire material 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 |
| CN110317061A (en) * | 2018-03-28 | 2019-10-11 | 山东理工大学 | It is a kind of to prepare Al4O4The method of C nano fiber |
| CN111635248A (en) * | 2020-06-09 | 2020-09-08 | 武汉科技大学 | AlN-AlON composite material and preparation method thereof |
| CN114315490A (en) * | 2021-12-20 | 2022-04-12 | 江苏润驰防务装备有限公司 | PTFE-Al-Ce energetic structural material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102361836A (en) * | 2009-03-30 | 2012-02-22 | 黑崎播磨株式会社 | Aluminum oxycarbide composition and process for producing same |
-
2013
- 2013-05-19 CN CN2013101850460A patent/CN103274701A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102361836A (en) * | 2009-03-30 | 2012-02-22 | 黑崎播磨株式会社 | Aluminum oxycarbide composition and process for producing same |
Non-Patent Citations (2)
| Title |
|---|
| SHAOWEI ZHANG, ET AL.: "Hydration resistances and reactions with CO of Al4O4C and Al2OC formed in carbon-containing refractions with Al", 《JOURNAL OF THE CERAMIC SOCIETY OF JAPAN》 * |
| 乔英杰主编: "《材料合成与制备》", 30 April 2010, 国防工业出版社 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896315A (en) * | 2014-03-25 | 2014-07-02 | 中国科学院金属研究所 | Al2OC nanowire material and preparation method thereof |
| CN103896315B (en) * | 2014-03-25 | 2016-01-20 | 中国科学院金属研究所 | A kind of Al 2oC nano-material 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 |
| CN107814583B (en) * | 2017-11-03 | 2020-10-02 | 江苏高淳陶瓷股份有限公司 | Al (aluminum)4O4C-reinforced silicon carbide honeycomb ceramic and preparation method thereof |
| CN110317061A (en) * | 2018-03-28 | 2019-10-11 | 山东理工大学 | It is a kind of to prepare Al4O4The method of C nano fiber |
| CN110317061B (en) * | 2018-03-28 | 2021-06-15 | 山东理工大学 | Preparation of Al4O4Method for producing C nanofibers |
| CN111635248A (en) * | 2020-06-09 | 2020-09-08 | 武汉科技大学 | AlN-AlON composite material and preparation method thereof |
| CN114315490A (en) * | 2021-12-20 | 2022-04-12 | 江苏润驰防务装备有限公司 | PTFE-Al-Ce energetic structural material and preparation method thereof |
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Application publication date: 20130904 |