CN105732040A - Synthesis method for preparing Ti3AlC2 by microwave self-propagating method - Google Patents
Synthesis method for preparing Ti3AlC2 by microwave self-propagating method Download PDFInfo
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Abstract
The invention relates to a synthesis method for preparing Ti3AlC2 by a microwave self-propagating method. The method comprises the steps: firstly, proportioning raw materials, i.e., Ti powder, TiC powder, Al powder, carbon powder, silicon powder and tin powder according to a mole ratio, adding ethanol, of which the mass is equal to that of the proportioned raw materials, into the proportioned raw materials, carrying out uniform stirring, then, adding agate balls, of which sizes are different and the mass is 2 to 5 times that of the mixture, into the mixture, and carrying out ball milling for 4 to 12 hours on a high-speed ball mill; centrifuging the ball-milled slurry, recovering a powder material, then, carrying out drying for 24 hours at room temperature, carrying out dry-pressing forming in an immobilized grinding tool at the pressure of 5MPa to 25MPa, and then, carrying out isostatic pressing treatment in the pressure intensity range of 120MPa to 200MPa; and putting blocks obtained after isostatic pressing into a self-made ceramic die, placing the sample containing die into a microwave reactor, carrying out a reaction, then, carrying out furnace cooling for 10 to 20 minutes, shifting the die to room temperature, carrying out cooling for 10 to 20 minutes, taking out a synthesized material, carrying out mechanical crushing, and then, carrying out recovery treatment. The method is simple in process, is energy-saving and efficient and is very applicable to industrial production.
Description
Technical field: the present invention relates to a kind of Ti3AlC2The preparation method of material, particularly relates to a kind of microwave self-propagating method and prepares Ti3AlC2Synthetic method.
Background technology: Ti3AlC2It is M3AX2A kind of new compound in system, belongs to the cermet material of a kind of stratiform.Ti3AlC2Having the hexagonal layered architectural feature that space octahedron connects, have metal and the double grading of pottery concurrently, it has the metalloid characteristic such as good electric conductivity and heat conductivity, higher elastic modelling quantity, thermal shock resistance, high temperature plasticity and machinability on the one hand；And on the other hand, it has high yield strength, high-melting-point, high heat stability, the typical ceramic characteristics such as highly oxidation resistant and corrosion.These excellent characteristics give its potential using value space in fields such as electromechanics, metallurgy, chemical industry, automobile, boats and ships, petrochemical industry, space flight and national defence.
Although Ti3AlC2Excellent properties attracted extensive concern both domestic and external.But due in Ti-Al-C ternary phase diagrams, single Ti3AlC2Phase stable range is narrow, therefore preparation technology relative complex.Preparation method conventional at present has hot pressing sintering method, HIP sintering method, discharge plasma sintering method, pulsed discharge plasma sintering process, machine-alloying, self-propagating high-temperature synthesis, vacuum non-pressure sintering method, lf method etc..Wherein hot pressing, high temperature insostatic pressing (HIP) or vacuum non-pressure sintering method these three method all need high temperature and longer temperature retention time to maintain the carrying out of reaction, so the actual consumption in course of reaction is very big.And discharge plasma sintering or pulsed discharge plasma sintering process need expensive Preparation equipment and high energy consumption.Although the lf method response time is shorter, but it requires height for Preparation equipment, and productivity is low, it is difficult to extensive use.Although and traditional self-propagating high-temperature energy consumption is relatively low, being swift in response, technique is simple, but reaction process is difficult to control to, and there is very big thermograde in course of reaction, and product purity is relatively low.Thus lack at present and really be able to be applied in batches produce the Ti that synthesis is high-purity3AlC2The technical method of material.
Summary of the invention: the invention aims to solve current Ti3AlC2Apparatus expensive in material synthesis processes, response time length, product purity are low, synthesis condition is harsh, uncontrollable especially for technique in current self-propagating method, the problem that material reaction yield is low, utilize microwave high-temperature self-propagating technology, it is provided that a kind of microwave self-propagating method prepares Ti3AlC2Synthetic method.
For achieving the above object, the technical solution used in the present invention is: a kind of microwave self-propagating method prepares Ti3AlC2Synthetic method, detailed process is as follows:
(1) dispensing and ball milling: by raw material Ti powder (or TiH2Powder), TiC powder, Al powder, carbon dust, silica flour, glass putty is according to mol ratio (1.9-3.2): (0-1.3): (1-1.3): (1-2.2): (0-0.2): (0-0.1) carries out dispensing, after the ethanol of addition equal quality stirs, add the agate ball that 2-5 times of quality varies in size, ball milling 4-12h on high speed ball mill.
(2) dry and molding: by the pulp centrifuged process after ball milling, reclaims drying at room temperature 24h after powder, and in FIxed abrasive article, 5-25MPa is dry-pressing formed, then carries out isostatic cool pressing process in the pressure range of 120-200MPa.
(3) microwave self-propagating synthesis: the block after isostatic cool pressing is put in self-control ceramic die, mould is through strict design, there is three layers composite-like structures, mould meets the short time and bears internal-external temperature difference up to more than 600 DEG C, the mould filling sample is put in microwave reactor, reaction power 200-2000W, response time 3-10min.Described self-control ceramic die is stepped up pin, reaction module chamber, thermal insulation layer and ceramic backing formed by inorganic housing, pottery cushion, location.Pottery cushion is in inorganic housing.Thermal insulation layer is fixed in pottery cushion by positioning clamping pin, and reaction module chamber is in thermal insulation layer.Ceramic backing is in the lower end of inorganic housing.Described pottery cushion includes porous ceramics.
(4) material recovery: the cold 10-20min of stove after reaction, moves to mould room temperature cooling 10-20min, takes out the material of synthesis, recycle after carrying out mechanical activation comminution.
The technology of the present invention advantage:
(1) reaction uniform, controllable: adopt microwave self-propagating synthesis technology, overcome traditional resistor silk to ignite or outside self-propagating technique of igniting causes local temperature too high, the shortcoming that reaction exists thermograde, reaction is uniformly synthesized powder purity height, can indirectly control synthesis temperature and time by control microwave power, isostatic pressed module size, process time, it is suppressed that the generation of other dephasigns in reaction simultaneously.
(2) efficient energy-saving: adopt the ceramic abrasive tool of simple three-layer composite structure and an easy microwave generator, react without heating, utilize the feature of self deoxygenation self-expanding simultaneously, react whole process and process without passing into noble gas or evacuation, being swift in response, equipment is cheap.
(3) high reaction activity and compactness: tradition self-propagating technology is a large amount of volatilizations along with aluminum melts, producing a large amount of cavity makes reactivity reduce, this technology is reacted internal layer at mould and is arranged thermal insulation layer, due to reaction heat expansion, internal-response keeps significantly high temperature to produce certain expansion, owing to the effect of thermal insulation layer makes internal generation certain pressure, indirectly play the effect of hot pressing synthesis, make reaction have high activity and compactness.
(4) environmental friendliness, pollutes low: self-propagating reaction inevitably produces a large amount of dust, and air, water body etc. can be caused severe contamination by this.This technology is nested porous wave transparent pottery in reaction mould second layer transition zone, it is possible to the dust produced in adsorption reaction, in whole course of reaction, the flue dust of more than 99% can be absorbed by the excessive layer of mould, pollutes low, environmental friendliness.
Accompanying drawing illustrates:
Fig. 1 is the structural representation of self-control ceramic die.
Detailed description of the invention:
As shown in Figure 1: self-control ceramic die is stepped up pin 3, reaction module chamber 4, thermal insulation layer 2 and ceramic backing 5 formed by inorganic housing 6, pottery cushion 1, location.Pottery cushion 1 is in inorganic housing 6.Thermal insulation layer 2 is fixed in pottery cushion 1 by positioning clamping pin 3, and reaction module chamber 4 is in thermal insulation layer 2.Ceramic backing 5 is in the lower end of inorganic housing 6.
Embodiment 1
Weigh 73g titanium valve, 20g aluminium powder, 14g carbon dust, 1.8g silica flour, add 108.8g ethanol, 217.6g agate ball.Put into the speed ball milling 6h with 300r/min in ball grinder.The pulp centrifuged removal supernatant,
At drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 5MPa after, sample block is fine and close in isostatic pressing machine 120MPa compacting.Then sample block is put in homemade ceramic die, moves in microwave reactor, microwave treatment 3min, and after the cold 15min of stove, room temperature cools down 15min again, takes out reaction sample block mechanical activation comminution and obtains sample.
Embodiment 2
Weigh 80g hydride powder, 16g aluminium powder, 14g carbon dust, 1.2g silica flour, 0.8g glass putty, add 112g ethanol, 224g agate ball.Put into the speed ball milling 4h with 400r/min in ball grinder.The pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 10MPa after, sample block is fine and close in isostatic pressing machine 160MPa compacting.Then sample block is put in homemade ceramic die, moves in microwave reactor, microwave treatment 5min, and after the cold 15min of stove, room temperature cools down 20min again, takes out reaction sample block mechanical activation comminution and obtains sample.
Embodiment 3
Weigh 52g titanium valve, 14g aluminium powder, 7g carbon dust, 30g carbonized titanium powder, 1.5g silica flour, 1g glass putty, add 105.5g ethanol, 250g agate ball.Put into the speed ball milling 6h with 600r/min in ball grinder.The pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 15MPa after, sample block is fine and close in isostatic pressing machine 150MPa compacting.Then sample block is put in homemade ceramic die, moves in microwave reactor, microwave treatment 5min, and after the cold 20min of stove, room temperature cools down 20min again, takes out reaction sample block mechanical activation comminution and obtains sample.
Embodiment 4
Weigh 80g titanium valve, 24g aluminium powder, 18g carbon dust, 9g carbonized titanium powder, 2g glass putty, add 133g ethanol, 300g agate ball.Put into the speed ball milling 8h with 600r/min in ball grinder.The pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 20MPa after, sample block is fine and close in isostatic pressing machine 180MPa compacting.Then sample block is put in homemade ceramic die, moves in microwave reactor, microwave treatment 8min, and after the cold 20min of stove, room temperature cools down 20min again, takes out reaction sample block mechanical activation comminution and obtains sample.
Embodiment 5
Weigh 55g hydride powder, 18g aluminium powder, 6g carbon dust, carbonized titanium powder 30g silica flour, 2g silica flour, 1g glass putty, add 112g ethanol, 400g agate ball.Put into the speed ball milling 10h with 600r/min in ball grinder.The pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 20MPa after, sample block is fine and close in isostatic pressing machine 200MPa compacting.Then sample block is put in homemade ceramic die, moves in microwave reactor, microwave treatment 10min, and after the cold 20min of stove, room temperature cools down 20min again, takes out reaction sample block mechanical activation comminution and obtains sample.
Claims (8)
1. a microwave self-propagating method prepares Ti3AlC2Synthetic method, detailed process is as follows:
(1) dispensing and ball milling: by raw material Ti powder, TiC powder, Al powder, carbon dust, silica flour, glass putty according to mol ratio (1.9-3.2): (0-1.3): (1-1.3): (1-2.2): (0-0.2): (0-0.1) carries out dispensing, after the ethanol of addition equal quality stirs, add the agate ball that 2-5 times of quality varies in size, ball milling 4-12h on high speed ball mill；
(2) dry and molding: by the pulp centrifuged process after ball milling, reclaims drying at room temperature 24h after powder, and in FIxed abrasive article, 5-25MPa is dry-pressing formed, then carries out isostatic cool pressing process in the pressure range of 120-200MPa；
(3) microwave self-propagating synthesis: the block after isostatic cool pressing is put in self-control ceramic die, mould is through strict design, there is three layers composite-like structures, mould meets the short time and bears internal-external temperature difference up to more than 600 DEG C, the mould filling sample is put in microwave reactor, reaction power 200-2000W, response time 3-10min；Described self-control ceramic die is stepped up pin, reaction module chamber, thermal insulation layer and ceramic backing formed by inorganic housing, pottery cushion, location, pottery cushion is in inorganic housing, thermal insulation layer is fixed in pottery cushion by positioning clamping pin, reaction module chamber is in thermal insulation layer, and ceramic backing is in the lower end of inorganic housing；
(4) material recovery: the cold 10-20min of stove after reaction, moves to mould room temperature cooling 10-20min, takes out the material of synthesis, recycle after carrying out mechanical activation comminution.
2. a kind of microwave self-propagating method as claimed in claim 1 prepares Ti3AlC2Synthetic method, it is characterised in that: in described step (1), by raw material TiH2Powder, TiC powder, Al powder, carbon dust, silica flour, glass putty are according to mol ratio (1.9-3.2): (0-1.3): (1-1.3): (1-2.2): (0-0.2): (0-0.1) carries out dispensing.
3. a kind of microwave self-propagating method as claimed in claim 1 prepares Ti3AlC2Synthetic method, it is characterised in that: described ceramic cushion includes porous ceramics.
4. a kind of microwave self-propagating method as described in claim 1 or 2 or 3 prepares Ti3AlC2Synthetic method, it is characterised in that detailed process is as follows: weigh 73g titanium valve, 20g aluminium powder, 14g carbon dust, 1.8g silica flour, adds 108.8g ethanol, 217.6g agate ball, puts into the speed ball milling 6h with 300r/min in ball grinder.The pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 5MPa after, sample block is suppressed densification at isostatic pressing machine 120MPa, then sample block is put in homemade ceramic die, move in microwave reactor, microwave treatment 3min, after the cold 15min of stove, room temperature cools down 15min again, takes out reaction sample block mechanical activation comminution and obtains sample.
5. a kind of microwave self-propagating method as described in claim 1 or 2 or 3 prepares Ti3AlC2Synthetic method, it is characterized in that, detailed process is as follows: weigh 80g hydride powder, 16g aluminum powder, 14g carbon dust, 1.2g silica flour, 0.8g glass putty, add 112g ethanol, 224g agate ball, put into the speed ball milling 4h with 400r/min in ball grinder, the pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 10MPa after, sample block is suppressed densification at isostatic pressing machine 160MPa, then sample block is put in homemade ceramic die, move in microwave reactor, microwave treatment 5min, after the cold 15min of stove, room temperature cools down 20min again, take out reaction sample block mechanical activation comminution and obtain sample.
6. a kind of microwave self-propagating method as described in claim 1 or 2 or 3 prepares Ti3AlC2Synthetic method, it is characterized in that, detailed process is as follows: weigh 52g titanium valve, 14g aluminum powder, 7g carbon dust, 30g carbonized titanium powder, 1.5g silica flour, 1g glass putty, add 105.5g ethanol, 250g agate ball, put into the speed ball milling 6h with 600r/min in ball grinder, the pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 15MPa after, sample block is suppressed densification at isostatic pressing machine 150MPa, then sample block is put in homemade ceramic die, move in microwave reactor, microwave treatment 5min, after the cold 20min of stove, room temperature cools down 20min again, take out reaction sample block mechanical activation comminution and obtain sample.
7. a kind of microwave self-propagating method as described in claim 1 or 2 or 3 prepares Ti3AlC2Synthetic method, it is characterized in that, detailed process is as follows: weigh 80g titanium valve, 24g aluminum powder, 18g carbon dust, 9g carbonized titanium powder, 2g glass putty, add 133g ethanol, 300g agate ball, put into the speed ball milling 8h with 600r/min in ball grinder, the pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 20MPa after, sample block is suppressed densification at isostatic pressing machine 180MPa, then sample block is put in homemade ceramic die, move in microwave reactor, microwave treatment 8min, after the cold 20min of stove, room temperature cools down 20min again, take out reaction sample block mechanical activation comminution and obtain sample.
8. a kind of microwave self-propagating method as described in claim 1 or 2 or 3 prepares Ti3AlC2Synthetic method, it is characterized in that, detailed process is as follows: weigh 55g hydride powder, 18g aluminum powder, 6g carbon dust, carbonized titanium powder 30g silica flour, 2g silica flour, 1g glass putty, add 112g ethanol, 400g agate ball, put into the speed ball milling 10h with 600r/min in ball grinder, the pulp centrifuged removal supernatant, at drying at room temperature 24h, be pressed into the shape of requirement by small pressure forming machine 20MPa after, sample block is suppressed densification at isostatic pressing machine 200MPa, then sample block is put in homemade ceramic die, move in microwave reactor, microwave treatment 10min, after the cold 20min of stove, room temperature cools down 20min again, take out reaction sample block mechanical activation comminution and obtain sample.
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| CN108298541A (en) * | 2018-02-05 | 2018-07-20 | 中国科学院电工研究所 | A kind of preparation method of two-dimensional layer MXene nanometer sheets |
| CN108585869A (en) * | 2018-05-10 | 2018-09-28 | 西北工业大学 | A kind of preparation method of in-situ authigenic MAX phase modified composite materials |
| CN109231989A (en) * | 2018-11-01 | 2019-01-18 | 燕山大学 | A kind of alloy with high activity intercalation Ti3AlMC2The preparation method of ceramic material |
| CN109867515A (en) * | 2017-12-05 | 2019-06-11 | 辽宁法库陶瓷工程技术研究中心 | A kind of Al2O3-Ti3AlC2Graded ceramics and preparation method thereof |
| CN110078511A (en) * | 2019-03-11 | 2019-08-02 | 昆明理工大学 | A kind of Ti3AlC2The preparation method of base ceramic bond diamond boring means cutter head |
| CN110395733A (en) * | 2019-08-22 | 2019-11-01 | 陕西科技大学 | A kind of preparation method of titanium alumina-carbon material that can be etched in water and preparation method thereof and organ shape material |
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| CN110078511A (en) * | 2019-03-11 | 2019-08-02 | 昆明理工大学 | A kind of Ti3AlC2The preparation method of base ceramic bond diamond boring means cutter head |
| CN110078511B (en) * | 2019-03-11 | 2021-10-12 | 昆明理工大学 | Ti3AlC2Method for preparing diamond drilling tool bit based on ceramic bond |
| CN110395733A (en) * | 2019-08-22 | 2019-11-01 | 陕西科技大学 | A kind of preparation method of titanium alumina-carbon material that can be etched in water and preparation method thereof and organ shape material |
| CN111477875A (en) * | 2020-04-27 | 2020-07-31 | 成都新柯力化工科技有限公司 | Method for preparing lithium battery double-layer anchoring coated silicon-carbon negative electrode material by mechanical force |
| CN111477875B (en) * | 2020-04-27 | 2020-12-15 | 成都新柯力化工科技有限公司 | Method for preparing lithium battery double-layer anchoring coated silicon-carbon negative electrode material by mechanical force |
| CN115583839A (en) * | 2022-11-09 | 2023-01-10 | 山东科技大学 | Three-dimensional integrated double-layer porous ceramic material and preparation method and application thereof |
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