CN104909757A - Method for preparing Ta2AlC monolithic ceramics by mechanical activating and hot-pressing - Google Patents
Method for preparing Ta2AlC monolithic ceramics by mechanical activating and hot-pressing Download PDFInfo
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- CN104909757A CN104909757A CN201510268208.6A CN201510268208A CN104909757A CN 104909757 A CN104909757 A CN 104909757A CN 201510268208 A CN201510268208 A CN 201510268208A CN 104909757 A CN104909757 A CN 104909757A
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Abstract
The invention provides a method for preparing Ta2AlC monolithic ceramics by mechanical activating and hot-pressing. The method comprises the following steps: putting tantalum powder, aluminum powder and carbon powder in a ball-milling tank, and carrying out high-energy ball-milling mechanical activating in a planetary ball mill in a vacuum condition to obtain an activated mixed powder material; putting the sieved activated mixed powder material into graphite dies to be pre-pressed and moulded obtain preformed blanks; putting the preformed blanks and the graphite dies in a high-temperature hot-pressing sintering furnace and insulating and sintering the preformed blanks and the graphite dies for 30-60 minutes after raising the temperature to 1300-1500 DEG C; and cooling the preformed blanks and the graphite dies to room temperature to obtain the Ta2AlC monolithic ceramics. The method provided by the invention has the advantages of low synthetic temperature, fast reaction speed, short preparation time and low cost, and the prepared Ta2AlC monolithic ceramics have the characteristics of high purity, high compactness, fine crystalline grain and excellent mechanical property.
Description
Technical field
The invention belongs to material science, particularly a kind of mechanical activation hot pressing Ta
2the method of AlC block ceramic.
Background technology
Ta
2alC is a kind of novel tertiary nano lamellar pottery, by the people such as Jeitschko (W.Jeitschko, H.Nowotny, F.Benesovsky.Monatsch.Chem.1963; 94:672) find the earliest in the sixties, its crystalline structure belongs to hexagonal system, spacer is P63/mmc, and lattice parameter is
ta
2alC pottery integrates the advantage of metal and pottery, both as metal, had good electroconductibility, thermal conductivity, machinability, heat-shock resistance and higher damage tolerance, the same with pottery again have the performances such as higher fusing point, Young's modulus and fracture toughness property.Ta
2the over-all properties of AlC excellence makes it have broad application prospects in fields such as space flight and aviation, nuclear industry, machinery, electronic information.
Current research shows, Ta
2alC block is mainly prepared from by the technique such as hot isostatic pressing method and pressure sintering, as (American Ceramic Society such as Gupta, J.Am.Ceram.Soc.89 (2006) 2974) adopt hot isostatic pressing method at 1600 DEG C, under 100MPa, hot isostatic pressing 8h obtains highly purified Ta
2alC block ceramic.(the investigation of materials magazine such as Hu Chunfeng, Int.J.Mater.Res.99 (2008) 8) adopt reaction in－situ/pressure sintering, with Ta, Al and C powder for raw material, at 1550 DEG C, under 30MPa pressure after hot pressing 30min, obtain single-phase Ta at 1400 DEG C of thermal treatment 60min
2alC block ceramic.But this two classes technique not only apparatus expensive, and synthesis temperature is high, long reaction time, production efficiency are low; Through heating for a long time, material structure alligatoring, causes its mechanical property to reduce.
Summary of the invention
Goal of the invention: in order to solve prior art Ta
2the Ta that the synthesis temperature of AlC block ceramic is high, preparation time is long, production efficiency is low, cost is high and obtain
2the problem of AlC block materials microstructure coarsening, the object of the present invention is to provide a kind of mechanical activation hot-pressing technique to prepare Ta
2the method of AlC block ceramic, the method, in conjunction with the advantage of mechanical alloying and hot pressed sintering, adopts the Ta that the method is obtained
2alC block ceramic purity is high, densification good.
Technical scheme: a kind of mechanical activation hot pressing Ta provided by the invention
2the method of AlC block ceramic, comprises the following steps:
(1) tantalum powder, aluminium powder and carbon dust are inserted in ball grinder, under vacuum condition, in planetary ball mill, carry out the activation of high-energy ball milling machinery, obtain the mixed powder of activation;
(2), after sieving, the mixed powder of activation is inserted pre-molding in graphite jig, obtains precast billet;
(3) precast billet and graphite jig are placed in high temperature hot pressing sintering oven, heat preservation sintering 30 ~ 60min be warming up to 1300 ~ 1500 DEG C under argon shield after; Be cooled to room temperature, obtain Ta
2alC block ceramic.
In step (1), the mol ratio of described tantalum powder, aluminium powder and carbon dust is 2:(1 ~ 1.4): (0.7 ~ 1).
In step (1), Ta powder, aluminium powder and Graphite Powder 99 all adopt highly purified simple substance powder, and in tantalum powder, the massfraction of tantalum is more than 99%, and in aluminium powder, the massfraction of aluminium is more than 99%, and the massfraction of the graphite in Graphite Powder 99 is more than 99%.
In step (1), in planetary ball mill, ratio of grinding media to material is 5:1 ~ 50:1; Rotational speed of ball-mill is 500 ~ 1000r/min, and Ball-milling Time is 1 ~ 8h.The preparation method of vacuum condition: ball grinder is carried out vacuumizing-applying argon gas-vacuumize, above operation is in triplicate.
In step (2), pre-molding again after the mixed powder of activation sieves; Screen cloth is 300-400 mesh sieve, preferably 325 mesh sieves; To ensure even particle size.
In step (2), preload pressure is 10 ~ 30MPa; Graphite jig is the graphite jig scribbling BN.
In step (3), temperature rise rate is 10 ~ 30 DEG C/min; During heat preservation sintering, system pressure is 30 ~ 50MPa.
Beneficial effect: the inventive method has the advantage that synthesis temperature is low, speed of response is fast, preparation time is short, cost is low, obtained Ta
2alC block ceramic has that purity is high, density is high, crystal grain is tiny and the feature of excellent in mechanical performance.
Specifically, the present invention compared with prior art has following outstanding advantage:
1. raw material powder is carried out the activation of high-energy ball milling machinery by the present invention, and powder refinement within a short period of time also mixes, and decrease ball grinder and high energy ball-milling to the pollution of raw material, the raw material mixed powder obtained is comparatively pure.
2. the present invention is in high-energy ball milling machinery reactivation process, and raw material powder inside produces stress, strain, defect and a large amount of nanometer crystal boundary, phase boundary, makes system stored energy very high, greatly improves powder activity, and improve particle distribution uniformity.
3. the powder activity after high-energy ball milling machinery of the present invention activation is higher, not only can reduce later stage synthesis temperature, and also reduces the reaction times.
Accompanying drawing explanation
Fig. 1 is the Ta that mechanical activation hot pressing of the present invention obtains
2the SEM photo of AlC block ceramic fracture.
Embodiment
The Ta powder that the present invention uses, aluminium powder and Graphite Powder 99 all adopt highly purified simple substance powder, and in tantalum powder, the massfraction of tantalum is more than 99%, and in aluminium powder, the massfraction of aluminium is more than 99%, and the massfraction of the graphite in Graphite Powder 99 is more than 99%.
Embodiment 1
Mechanical activation hot pressing Ta
2alC block ceramic, comprises the following steps:
(1) with tantalum powder, aluminium powder and Graphite Powder 99 for raw material, by the molar ratio ingredient of Ta:Al:C=2:1.2:1;
(2) above-mentioned batching is inserted in ball grinder, ratio of grinding media to material 5:1, ball grinder is carried out vacuumizing-applying argon gas-vacuumize, more than operate in triplicate, then on planetary ball mill, carry out the activation of high energy ball mill tool, rotational speed of ball-mill is 500r/min, and Ball-milling Time is 4h; Cross 325 mesh sieves;
(3) after mixed powder mechanical activation, insert pre-molding in the graphite jig scribbling BN, preload pressure is 10MPa;
(4) precast billet of coldmoulding and mould are placed in high temperature hot pressing sintering oven, under Ar gas shielded, are warming up to 1500 DEG C with 20 DEG C/min, heat preservation sintering 60min under 30MPa pressure.Cool to room temperature with the furnace after insulation terminates, obtain Ta
2alC block ceramic.
Embodiment 2
Mechanical activation hot pressing Ta
2alC block ceramic, comprises the following steps:
(1) with tantalum powder, aluminium powder and Graphite Powder 99 for raw material, by the molar ratio ingredient of Ta:Al:C=2:1.4:1;
(2) above-mentioned batching is inserted in ball grinder, ratio of grinding media to material 10:1, ball grinder is carried out vacuumizing-applying argon gas-vacuumize, more than operate in triplicate, then on planetary ball mill, carry out the activation of high energy ball mill tool, rotational speed of ball-mill is 600r/min, and Ball-milling Time is 3h; Cross 325 mesh sieves;
(3) after mixed powder mechanical activation, insert pre-molding in the graphite jig scribbling BN, preload pressure is 20MPa;
(4) precast billet of coldmoulding and mould are placed in high temperature hot pressing sintering oven, under Ar gas shielded, are warming up to 1400 DEG C with 10 DEG C/min, heat preservation sintering 60min under 30MPa pressure.Cool to room temperature with the furnace after insulation terminates, obtain Ta
2alC block ceramic.
Embodiment 3
Mechanical activation hot pressing Ta
2alC block ceramic, comprises the following steps:
(1) with tantalum powder, aluminium powder and Graphite Powder 99 for raw material, by the molar ratio ingredient of Ta:Al:C=2:1.2:0.9;
(2) above-mentioned batching is inserted in ball grinder, ratio of grinding media to material 10:1, ball grinder is carried out vacuumizing-applying argon gas-vacuumize, more than operate in triplicate, then on planetary ball mill, carry out the activation of high energy ball mill tool, rotational speed of ball-mill is 1000r/min, and Ball-milling Time is 5h; Cross 325 mesh sieves;
(3) after mixed powder mechanical activation, insert pre-molding in the graphite jig scribbling BN, preload pressure is 20MPa;
(4) precast billet of coldmoulding and mould are placed in high temperature hot pressing sintering oven, under Ar gas shielded, are warming up to 1450 DEG C with 30 DEG C/min, heat preservation sintering 30min under 50MPa pressure.Cool to room temperature with the furnace after insulation terminates, obtain Ta
2alC block ceramic.
Embodiment 4
Mechanical activation hot pressing Ta
2alC block ceramic, comprises the following steps:
(1) with tantalum powder, aluminium powder and Graphite Powder 99 for raw material, by the molar ratio ingredient of Ta:Al:C=2:1:0.7;
(2) above-mentioned batching is inserted in ball grinder, ratio of grinding media to material 50:1, ball grinder is carried out vacuumizing-applying argon gas-vacuumize, more than operate in triplicate, then on planetary ball mill, carry out the activation of high energy ball mill tool, rotational speed of ball-mill is 800r/min, and Ball-milling Time is 1h; Cross 300 mesh sieves;
(3) after mixed powder mechanical activation, insert pre-molding in the graphite jig scribbling BN, preload pressure is 30MPa;
(4) precast billet of coldmoulding and mould are placed in high temperature hot pressing sintering oven, under Ar gas shielded, are warming up to 1300 DEG C with 20 DEG C/min, heat preservation sintering 40min under 40MPa pressure.Cool to room temperature with the furnace after insulation terminates, obtain Ta
2alC block ceramic.
Embodiment 5
Mechanical activation hot pressing Ta
2alC block ceramic, comprises the following steps:
(1) with tantalum powder, aluminium powder and Graphite Powder 99 for raw material, by the molar ratio ingredient of Ta:Al:C=2:1.2:0.8;
(2) above-mentioned batching is inserted in ball grinder, ratio of grinding media to material 30:1, ball grinder is carried out vacuumizing-applying argon gas-vacuumize, more than operate in triplicate, then on planetary ball mill, carry out the activation of high energy ball mill tool, rotational speed of ball-mill is 800r/min, and Ball-milling Time is 8h; Cross 400 mesh sieves;
(3) after mixed powder mechanical activation, insert pre-molding in the graphite jig scribbling BN, preload pressure is 20MPa;
(4) precast billet of coldmoulding and mould are placed in high temperature hot pressing sintering oven, under Ar gas shielded, are warming up to 1350 DEG C with 20 DEG C/min, heat preservation sintering 50min under 40MPa pressure.Cool to room temperature with the furnace after insulation terminates, obtain Ta
2alC block ceramic.
The above is only present pre-ferred embodiments, not does any restriction to the present invention, and every any simple modification done above embodiment according to the technology of the present invention essence, all still belongs in the protection domain of technical solution of the present invention.
Claims (7)
1. a mechanical activation hot pressing Ta
2the method of AlC block ceramic, is characterized in that: comprise the following steps:
(1) tantalum powder, aluminium powder and carbon dust are inserted in ball grinder, under vacuum condition, in planetary ball mill, carry out the activation of high-energy ball milling machinery, obtain the mixed powder of activation;
(2) mixed powder of activation is inserted pre-molding in graphite jig, obtain precast billet;
(3) precast billet and graphite jig are placed in high temperature hot pressing sintering oven, heat preservation sintering 30 ~ 60min be warming up to 1300 ~ 1500 DEG C under argon shield after; Be cooled to room temperature, obtain Ta
2alC block ceramic.
2. a kind of mechanical activation hot pressing Ta according to claim 1
2the method of AlC block ceramic, is characterized in that: in step (1), and the mol ratio of described tantalum powder, aluminium powder and carbon dust is 2:(1 ~ 1.4): (0.7 ~ 1).
3. a kind of mechanical activation hot pressing Ta according to claim 1
2the method of AlC block ceramic, is characterized in that: in step (1), in tantalum powder, the massfraction of tantalum is more than 99%, and in aluminium powder, the massfraction of aluminium is more than 99%, and the massfraction of the graphite in Graphite Powder 99 is more than 99%.
4. a kind of mechanical activation hot pressing Ta according to claim 1
2the method of AlC block ceramic, is characterized in that: in step (1), and in planetary ball mill, ratio of grinding media to material is 5:1 ~ 50:1; Rotational speed of ball-mill is 500 ~ 1000r/min, and Ball-milling Time is 1 ~ 8h.
5. a kind of mechanical activation hot pressing Ta according to claim 1
2the method of AlC block ceramic, is characterized in that: in step (2), pre-molding again after the mixed powder of activation sieves; Screen cloth is 300-400 mesh sieve, preferably 325 mesh sieves.
6. a kind of mechanical activation hot pressing Ta according to claim 1
2the method of AlC block ceramic, is characterized in that: in step (2), and preload pressure is 10 ~ 30MPa; Graphite jig is the graphite jig scribbling BN.
7. a kind of mechanical activation hot pressing Ta according to claim 1
2the method of AlC block ceramic, is characterized in that: in step (3), and temperature rise rate is 10 ~ 30 DEG C/min; During heat preservation sintering, system pressure is 30 ~ 50MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294106A (en) * | 2015-10-15 | 2016-02-03 | 河海大学 | Ta2AlC block ceramic prepared through spark plasma sintering process and preparing method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024575A (en) * | 2006-02-17 | 2007-08-29 | 中国科学院金属研究所 | Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction |
| JP2008143769A (en) * | 2006-12-07 | 2008-06-26 | Korea Inst Of Machinery & Materials | Nano-size lead-free piezoceramic powder and method of synthesizing the same |
| CN102174681A (en) * | 2010-12-31 | 2011-09-07 | 陕西科技大学 | High-purity Ti2AlNxC1-x solid solution material and preparation method thereof |
| CN104628386A (en) * | 2015-02-05 | 2015-05-20 | 河海大学 | Preparation method of Ta2AlC block ceramic |
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- 2015-05-22 CN CN201510268208.6A patent/CN104909757A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024575A (en) * | 2006-02-17 | 2007-08-29 | 中国科学院金属研究所 | Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction |
| JP2008143769A (en) * | 2006-12-07 | 2008-06-26 | Korea Inst Of Machinery & Materials | Nano-size lead-free piezoceramic powder and method of synthesizing the same |
| CN102174681A (en) * | 2010-12-31 | 2011-09-07 | 陕西科技大学 | High-purity Ti2AlNxC1-x solid solution material and preparation method thereof |
| CN104628386A (en) * | 2015-02-05 | 2015-05-20 | 河海大学 | Preparation method of Ta2AlC block ceramic |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294106A (en) * | 2015-10-15 | 2016-02-03 | 河海大学 | Ta2AlC block ceramic prepared through spark plasma sintering process and preparing method thereof |
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Application publication date: 20150916 |