CN100371300C - Method of thermo press preparing high purity aluminium titanium carbide block material - Google Patents
Method of thermo press preparing high purity aluminium titanium carbide block material Download PDFInfo
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- CN100371300C CN100371300C CNB2006101147780A CN200610114778A CN100371300C CN 100371300 C CN100371300 C CN 100371300C CN B2006101147780 A CNB2006101147780 A CN B2006101147780A CN 200610114778 A CN200610114778 A CN 200610114778A CN 100371300 C CN100371300 C CN 100371300C
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Abstract
The present invention relates to a method for preparing high-purity aluminium titanium carbide block material by utilizing hot-pressing process. Said method includes the following steps: using Ti powder, Al powder and TiC powder as raw material, using proper quantity of Sn as reaction adjuvant, mixing materials according to the mole ratio of Ti:Al:TiC:Sn=1:(0.9-1):1:(0-0.2), placing the mixed material and agate ball into a ball-grinding tank according to the ball material ratio of 2:1, dry mixing them for 5-10 h in ball-grinding machine, placing the uniformly-mixed material into a graphite mould, placing said graphite mould into a hot-pressing furnace, heating to 1350-1550 deg.C under the protection of argon atmosphere, at the same time applying pressure of 10-30 MPa then heat-insulating for 30-60 min so as to obtain the invented high-purity large-size Ti3AlC2 block material.
Description
Technical field
The present invention relates to the preparation method of ceramic block, particularly a kind of high conductive carbonized aluminium titanium Ti
3AlC
2Ceramic block and hot pressing method for preparing thereof.
Background technology
Aluminium-titanium carbonate Ti
3AlC
2Belong to the novel tertiary lamellar compound.It integrates the advantage of metal and pottery, structure set and function integration, as have high conductivity, anti-oxidant, corrosion-resistant, self-lubricating, easy premium properties such as processing.This new ceramics can be used as the 26S Proteasome Structure and Function material and is widely used in fields such as aerospace, petrochemical complex, communications and transportation, new forms of energy, electronic information, the preferred material of thermal structure spare is motor brush material of new generation and heat exchange material, bullet train Material for Pantograph Slide, various anti-friction wear-resistant parts, corrosion resistant member, solid self-lubricant material, fuel cell double polar plate material etc. in this way.
In the Ti-Al-C ternary phase diagrams, because Ti
3AlC
2Phase region very narrow, so synthesis of high purity Ti
3AlC
2Very there are impurity phases such as TiC usually in difficulty in the product, and this is to Ti
3AlC
2Performance impacts such as the conduction of material, easily processing, self-lubricating are bigger, therefore limited Ti
3AlC
2Pottery is in the application in engineering field.At present, synthesis of densified Ti
3AlC
2Block mainly adopts hot pressing and hot isostatic pressing technique.Document 1 (J.Am.Ceram.Soc., 2000; 83[4]: 825) report, with Ti powder, Al
4C
3Powder and Graphite Powder 99 are raw material, and at 1400 ℃, hot isostatic pressing is 16 hours under the 70MPa pressure, prepares Ti
3AlC
2Block materials, but because Al
4C
3Water absorbability, have Al in the final product
2O
3The impurity phase.Chinese invention patent ZL00123203.7 discloses and has a kind ofly prepared Ti with in-situ hot pressing/solid-liquid reaction method
3AlC
2The method of block materials.With Ti powder, Al powder and C powder is raw material, presses Ti: Al: C=3: 1: 2 molar ratio ingredient, hot pressing is 0.5～4 hour under 1200～1500 ℃, 25MPa pressure, obtains Ti
3AlC
2Block materials.Document 2 (Rare Metals Materials and engineering, 2005,34 (1): 132) report, utilize plasma discharging Fast Sintering method, press Ti: Al: C=3: 1.1: 1.8 molar ratio ingredient, at 1500 ℃, synthesized Ti under the pressure of 20MPa
3AlC
2Block materials, but contain TiC impurity phase.
The characteristics of aforesaid method are, are not that sintering time is long, and pressure is big, and the purity that is exactly synthetic materials is low.And discover, when adopting above-mentioned batching, because of the volatilization loss of Al, be the major cause that causes impurity such as TiC to exist mutually in the high-temperature reaction process.And the volatilization loss of Al is relevant with appearance " thermal explosion " phenomenon in the Ti/Al/C reactive system." thermal explosion " phenomenon mainly is because the vigorous reaction of Ti and C is emitted a large amount of heat causes.The appearance of " thermal explosion " reaction sharply raises system temperature, causes Al volatilization loss serious, has changed the reaction ratio of each element in the system, influences the purity of resultant." thermal explosion " reaction causes temperature big ups and downs in the stove, the heating member of infringement body of heater.Even add B
2O
3, low melting components such as NaF reduce the thermal explosion level of response, but because the volatilization of low melting point constituent element causes the corrosion and the environmental pollution of body of heater and heating member.Especially prepare large size Ti
3AlC
2During block materials, the problem that the thermal explosion reaction is caused is more outstanding.
Summary of the invention
Key technical problem to be solved by this invention is, changes tradition with Ti, and Al and C be initial batching, solves by traditional proportioning and synthesizes Ti
3AlC
2The time problem that exists, directly adopt Ti, Al and TiC are raw material, or to add an amount of Sn be reaction promoter, under stable processing parameter, with hot-pressing technique in wide temperature range, in the short period of time, preparation high purity and low-cost Ti
3AlC
2Block materials.
Technical scheme of the present invention is:
The thermo press preparing high purity aluminium titanium carbide block material method:
(1) be raw material with Ti powder, Al powder and TiC powder, Sn is a reaction promoter, presses Ti: Al: TiC: Sn=1: (0.9～1): 1: the molar ratio ingredient of (0～0.2);
(2) above-mentioned batching and agate ball are put into ball grinder by ratio of grinding media to material at 2: 1, on ball mill, do and mixed 5～10 hours;
(3) above-mentioned mixed batching is put into graphite jig; graphite jig is placed hot pressing furnace; under argon shield atmosphere; with 20～50 ℃/minute temperature rise rates furnace temperature is risen to 1350～1550 ℃; simultaneously the powder in the mould is applied the pressure of 10～30MPa; be incubated 30～60 minutes, obtain high purity large size Ti
3AlC
2Block materials.
The present invention compares the beneficial effect that is had with prior art and is:
(1) the present invention is according to Ti: Al: TiC=1: 1: 1 molar ratio ingredient, or to add an amount of Sn be reaction promoter, the Ti of synthetic equal in quality
3AlC
2Block materials is compared (Ti: Al: C=3: 1: 2 mol ratio), reduced the content of raw material powder, reduced cost with traditional proportioning.
(2) technical process of the present invention is simple, and processing parameter is stable, and in the hot pressing furnace of routine, under argon gas (or vacuum) protective atmosphere, the short period of time, lower pressure in the wide temperature range, makes high purity Ti
3AlC
2The compact block material.
(3) with Ti, Al and C traditional proportioning synthesize Ti
3AlC
2Process in, at first be Ti and Al reaction forming Ti-Al compound, be that Ti and C reaction generates TiC then.TiC that generates and the reaction of Ti-Al compound generate Ti
3AlC
2But with respect to Ti
3AlC
2Formation speed, the generation of TiC has hysteresis quality in the system, has reduced Ti
3AlC
2Resultant velocity.Directly adopt TiC in the Ti-Al-TiC batching, reduced process and step that Ti and C reaction generates TiC, as long as reach temperature, TiC and Ti-Al compound direct reaction generate Ti
3AlC
2, make Ti
3AlC
2Resultant velocity accelerate.
(4) in batching, adopt TiC to replace whole C and part Ti, avoided the generation of thermal explosion reaction in the traditional proportioning Ti-Al-C system, can not cause the fluctuation of temperature, reduced the high temperature loss problem of Al, sintering process parameter is easy to stablize, help system components and generate by design proportion, impurity such as no TiC exist mutually, synthetic Ti
3AlC
2The purity height of material.
(5) the used prescription of the present invention, therefore the high temperature loss problem owing to thermal explosion reaction of having avoided occurring in the traditional proportioning and Al can prepare large-diameter high-purity Ti
3AlC
2Block materials.
(5) the present invention adopts Sn as auxiliary agent, because the fusing point low (232 ℃) of Sn, liquid phase begins to occur at low temperatures, makes that each component is tending towards homogenizing in the batching, helps reaction and carries out.After reaction was finished, the Sn atom entered Ti
3AlC
2Form sosoloid in the lattice, can not be present in mutually in the product, therefore to Ti with impurity
3AlC
2The purity and the characteristic of material do not have substantial effect.
Description of drawings
Fig. 1 is the Ti of hot pressing preparation of the present invention
3AlC
2The X-ray diffraction of ceramic block material (XRD) collection of illustrative plates.
Embodiment
Embodiment one:
1) press Ti: Al: TiC: Sn=1: 1: 1: 0.1 molar ratio ingredient takes by weighing Ti powder 14.68 grams, Al powder 8.29 grams, TiC powder 18.38 grams, Sn powder 3.64 grams.2) above-mentioned batching and agate ball are put into ball grinder by ratio of grinding media to material at 2: 1, batch mixing 5 hours.3) batching that will mix is put into graphite jig, and graphite jig is placed hot pressing furnace, under the argon shield atmosphere; with 30 ℃/minute temperature rise rates furnace temperature is risen to 1350 ℃; simultaneously the powder in the mould is applied the pressure of 20MPa, soaking time 40 minutes obtains high purity Ti
3AlC
2The compact block material.This material X-ray diffraction (XRD) collection of illustrative plates is seen accompanying drawing 1.As seen from the figure, the product purity height, impurity such as no TiC exists mutually in XRD figure spectrum.
Embodiment two:
1) press Ti: Al: TiC: Sn=1: 1: 1: 0.15 molar ratio ingredient takes by weighing Ti powder 14.12 grams, Al powder 7.97 grams, TiC powder 17.66 grams, Sn powder 5.25 grams.2) above-mentioned batching and agate ball are put into ball grinder by ratio of grinding media to material at 2: 1, batch mixing 5 hours.3) batching that will mix is put into graphite jig, and graphite jig is placed hot pressing furnace, under the argon shield atmosphere; with 40 ℃/minute speed furnace temperature is risen to 1400 ℃; simultaneously the powder in the mould is applied the pressure of 20MPa, soaking time 30 minutes obtains high purity Ti
3AlC
2The compact block material.Its XRD result is identical with embodiment one.
Embodiment three:
1) press Ti: Al: TiC=1: 0.9: 1 molar ratio ingredient takes by weighing Ti powder 16.29 grams, Al powder 8.26 grams, TiC powder 20.37 grams.2) above-mentioned batching and agate ball are put into ball grinder by ratio of grinding media to material at 2: 1, batch mixing 8 hours.3) batching that will mix is put into graphite jig, and graphite jig is placed hot pressing furnace, under the argon shield atmosphere; with 40 ℃/minute speed furnace temperature is risen to 1500 ℃; simultaneously the powder in the mould is applied the pressure of 30MPa, soaking time 60 minutes obtains high purity Ti
3AlC
2The compact block material.Its XRD result is identical with embodiment one.
Embodiment four:
1) press Ti: Al: TiC: Sn=1: 1: 1: 0.1 molar ratio ingredient takes by weighing Ti powder 83.29 grams, Al powder 46.98 grams, TiC powder 104.20 grams, Sn powder 20.65 grams.2) above-mentioned batching and agate ball are put into ball grinder by the weight ratio of ball and material at 2: 1, batch mixing 10 hours.3) batching that will mix is put into graphite jig; graphite jig is placed hot pressing furnace; under the argon shield atmosphere; with 30 ℃/minute speed furnace temperature is risen to 1450 ℃; simultaneously the powder in the mould is applied the pressure of 30MPa; soaking time 30 minutes obtains high purity, diameter is the large size Ti of Φ 120mm
3AlC
2The compact block material.Its XRD result is identical with embodiment one.
Embodiment five:
1) press Ti: Al: TiC=1: 0.9: 1 molar ratio ingredient takes by weighing Ti powder 92.45 grams, Al powder 46.9 grams, TiC powder 115.61 grams.2) above-mentioned batching and agate ball are put into ball grinder by ratio of grinding media to material at 2: 1, batch mixing 10 hours.3) batching that will mix is put into graphite jig; graphite jig is placed hot pressing furnace; under the argon shield atmosphere; with 30 ℃/minute speed furnace temperature is risen to 1500 ℃; simultaneously the powder in the mould is applied the pressure of 30MPa; soaking time 60 minutes obtains high purity, diameter is the large size Ti of Φ 120mm
3AlC
2The compact block material.Its XRD result is identical with embodiment one.
Claims (1)
1. the method for thermo press preparing high purity aluminium titanium carbide block material steps of the method are:
(1) be raw material with Ti powder, Al powder and TiC powder, Sn is a reaction promoter, presses Ti: Al: TiC: Sn=1: (0.9～1): 1: the molar ratio ingredient of (0～0.2);
(2) above-mentioned batching and agate ball are put into ball grinder by ratio of grinding media to material at 2: 1, on ball mill, do and mixed 5～10 hours;
(3) the above-mentioned batching that mixes is put into graphite jig; graphite jig is placed hot pressing furnace; under the argon shield atmosphere; with 20～50 ℃/minute temperature rise rates furnace temperature is risen to 1350～1550 ℃; simultaneously the powder in the mould is applied the pressure of 10～30MPa; be incubated 30～60 minutes, obtain high purity large size Ti
3AlC
2Block materials.
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|---|---|---|---|
| CNB2006101147780A CN100371300C (en) | 2006-11-23 | 2006-11-23 | Method of thermo press preparing high purity aluminium titanium carbide block material |
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|---|---|---|---|
| CNB2006101147780A CN100371300C (en) | 2006-11-23 | 2006-11-23 | Method of thermo press preparing high purity aluminium titanium carbide block material |
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| CN1948220A CN1948220A (en) | 2007-04-18 |
| CN100371300C true CN100371300C (en) | 2008-02-27 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102206079B (en) * | 2011-03-29 | 2013-01-02 | 西北有色金属研究院 | Method for preparing large-size Ti3SiC2 ceramic material |
| CN104805326B (en) * | 2015-04-02 | 2017-12-08 | 北京交通大学 | A kind of adjustable Ti of coefficient of friction3Al1‑xSnxC2Solid-solution material and preparation method thereof |
| CN110156018B (en) * | 2019-06-03 | 2020-11-06 | 蚌埠学院 | Preparation method of high-purity titanium silicon carbon material |
| CN113044842B (en) * | 2021-01-12 | 2022-05-17 | 辽宁中色新材科技有限公司 | Production process of high-purity aluminum titanium carbide |
| CN112935250A (en) * | 2021-01-28 | 2021-06-11 | 北京大学 | Cu and Ti for pantograph slide plate3AlC2Functionally graded material and preparation method thereof |
| CN113233464A (en) * | 2021-06-03 | 2021-08-10 | 北京理工大学前沿技术研究院 | High-purity titanium aluminum carbide and preparation method and application thereof |
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Non-Patent Citations (1)
| Title |
|---|
| 原位热压TiC/Ti/Al合成Ti2AlC的研究. 周卫兵等.佛山陶瓷，第3期. 2005 * |
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