CN100357179C - Titanium aluminium carbide powder and synthesis method using tin as reactive adjuvant therefor - Google Patents
Titanium aluminium carbide powder and synthesis method using tin as reactive adjuvant therefor Download PDFInfo
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- CN100357179C CN100357179C CNB2005100116507A CN200510011650A CN100357179C CN 100357179 C CN100357179 C CN 100357179C CN B2005100116507 A CNB2005100116507 A CN B2005100116507A CN 200510011650 A CN200510011650 A CN 200510011650A CN 100357179 C CN100357179 C CN 100357179C
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Abstract
The present invention discloses a titanium aluminium carbide (Ti3AlC2) powder and a synthesis method thereof by using tin as a reactive auxiliary agent. The powder is characterized in that titanium (Ti), aluminum (Al) and graphite (C) powder are used as raw material; stannum (Sn) is used as a reactive auxiliary agent; the raw material and the reactive auxiliary agent are mixed in the molar ratio (Ti: Al: C: Sn) of 3.0:1.0: (1.8 to 2.0): (0.1 to 0.2); the mixture is mixed for 2 to 6 hours in a ball milling mode; the mixture is dried in a drying oven at 60 to 70 DEG C; the dried raw material mixture is extruded into blocks at 10 to 20MPa; the blocks are placed in a high temperature furnace and is protected by argon; the furnace temperature is raised to 1300 to 1550 DEG C at the heating rate of 20 to 40 DEG C /min; the temperature is kept for 5 to 10 minutes; the blocks are cooled at the rate of 10 to 15 DEG C /min. Thus, the titanium aluminium carbide powder is prepared.
Description
Technical field
The present invention relates to a kind of titanium aluminium carbide (Ti
3AlC
2) powder and be the synthetic method of the titanium aluminium carbide powder of reaction promoter with tin (Sn).
Background technology
The titanium aluminium carbide powder is a kind of novel double carbide ceramic powder, available its is raw material, but titanium aluminium carbide block materials and various matrix material and the device that contains titanium aluminium carbide that preparation has performances such as high conductivity, high thermal conductivity, heat shock resistance, self-lubricating mechanical workout.
Titanium aluminium carbide as a kind of new material 1994 by Pietzka and Schuster (J.Phase Equilib, 1994[15]: 392) find first.People such as Tzenov in 2000 (J.Am Ceram.Soc, 2000[83]: 825) with Ti powder, Al
4C
3Powder and Graphite Powder 99 are raw material, and with hot isostatic pressing (HIP) method, 1400 ℃ of following 70MPa hot isostatic pressings 16 hours, original position was synthesized the Ti that contains 4% aluminum oxide
3AlC
2The block materials sample.People such as distribution spring in 2003 (on May 14th, 2003, [21] the ZL patent No.: be raw material 00123203.7) with Ti powder, Al powder and C powder, with in-situ hot pressing/solid-liquid reaction method, hot pressing is 0.5～4 hour under 1200～1500 ℃, 10～50MPa, and original position has been synthesized Ti
3AlC
2The block materials sample.Zhai Hong in 2004 is auspicious to be waited the people (Mater.Sci.Forum, (2004) [475-479]: be raw material with titanium valve, aluminium powder and Graphite Powder 99 1251), use pressing methods, hot pressing is 0.5 hour under 1450 ℃, 20MPa, and original position has been synthesized Ti
3AlC
2Volume content is greater than 98% high purity Ti
3AlC
2The block materials sample.But various original position synthetic methods can not be widely used in preparation and contain Ti
3AlC
2Diphase ceramic material and the various Ti that contains
3AlC
2Matrix material, on engineering is used, significant limitation is arranged.The Ti that usually, prepare various practicalities
3AlC
2Material and matrix material thereof and device need to use highly purified Ti
3AlC
2Powder is that raw material carries out the secondary preparation.Therefore, highly purified Ti
3AlC
2Powder and synthetic method thereof are for Ti
3AlC
2The practical application of material has crucial meaning.
With the synthetic Ti of the method for high-temperature calcination
3AlC
2Powder is economical and practical, is fit to industrial-scale production.With the method for high-temperature calcination, not only need to improve the Ti that once synthesizes in the powder to greatest extent by formulating of recipe and technological design
3AlC
2Content needs simultaneously to solve in the synthetic reaction process and concentrates the thermal explosion problem that takes place because of reaction heat.The generation of thermal explosion has very big harm to used High Temperature Furnaces Heating Apparatus, and causes the generation of a large amount of titanium carbides dephasigns such as (TiC).People such as Peng (Mater.Sci.Forum, (2004) [475-479]: 1247) once attempted in raw material, adding boron oxide (B
2O
3) method suppress the generation of thermal explosion.But the B of these interpolations
2O
3Final residue is in the synthetic powder, and is harmful to the performance of powder.And, B
2O
3Existence be unfavorable for Ti in the synthetic reaction process
3AlC
2Generation, thereby be difficult to improve Ti in the synthetic powder
3AlC
2Content.
Summary of the invention
The object of the present invention is to provide a kind of highly purified titanium aluminium carbide powder to reach with tin is the synthetic method of the titanium aluminium carbide powder of reaction promoter.
Titanium aluminium carbide powder of the present invention, its composition is as follows:
Ti
3AlC
2Volume content＞98vol.%;
Volume content＜the 2vol.% of dephasigns such as TiC.
Of the present invention is the titanium aluminium carbide powder synthetic method of reaction promoter with tin, comprises following each step:
(1) batching: with titanium (Ti) powder, aluminium (Al) powder, graphite (C) powder and tin (Sn) powder Ti: Al: C: Sn=3.0 in molar ratio: (0.9～1.1): (1.8～2.0): the ratio batching of (0.05～0.2);
(2) batch mixing: add 70 milliliters dehydrated alcohol, the agate ball or the alumina balls of 200～250 grams in the above-mentioned batching of per 100 grams, ball milling 2～6 hours, 60～70 ℃ of oven dry in baking oven with the mixing raw material grinding of oven dry, are crossed 70～100 mesh sieves;
(3) precompressed: the block that the dried feed behind the above-mentioned batch mixing is pressed into Any shape with the pressure of 10～20MPa;
(4) calcining: the mixing raw material of above-mentioned precompressed is put into the graphite jar and placed High Temperature Furnaces Heating Apparatus; under argon shield; temperature rise rate by 10～40 ℃/min; furnace temperature is risen to 1300 ℃～1550 ℃; insulation 5～10min; speed cooling with 10～15 ℃/min promptly obtains titanium aluminium carbide powder of the present invention.
The Ti that obtains with synthetic method of the present invention
3AlC
2Do not contain or only contain the dephasigns such as TiC of minute quantity in the powder.The Sn that adds as reaction promoter is solid-solubilized in Ti
3AlC
2Intragranular is to Ti
3AlC
2The performance of powder does not have substantial effect;
Make reaction promoter with Sn, can suppress the generation of dephasigns such as TiC effectively, and in the synthetic powder, do not have or have only the reaction promoter residuals of minute quantity, thereby do not need aftertreatment just can obtain highly purified Ti
3AlC
2Powder;
Make reaction promoter with Sn, can prevent the generation of thermal explosion phenomenon in the building-up process effectively, thereby can a heat obtain the high purity Ti of kg level
3AlC
2Powder is fit to plant-scale production;
Make reaction promoter with Sn, can make synthesis temperature be reduced to 1300 ℃, the range extension to 1300 of synthesis temperature～1500 ℃, thereby significantly relaxed technical qualification and temperature controlled requirement to High Temperature Furnaces Heating Apparatus, help industrial-scale production.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum with the inventive method synthetic titanium aluminium carbide powder.
Embodiment
Embodiment 1
A gross weight is the small sample of 9.0 grams.Take by weighing Ti powder 5.98 grams, Al powder 1.12 grams, Graphite Powder 99 0.91 gram, Sn powder 0.99 gram, mix the back and add 6 milliliters of dehydrated alcohols and 20 gram agate balls, ball mill mixing 2 hours, dry, grind, cross 100 mesh sieves then, compacting under 15MPa pressure, put into the graphite jig of High Temperature Furnaces Heating Apparatus, argon shield, speed with 38 ℃/min is warming up to 1500 ℃, insulation 5min, speed with 10～15 ℃/min is reduced to 60 ℃ with furnace temperature, and the loose shape block that reaction is generated takes out, grinds, and promptly obtains titanium aluminium carbide powder of the present invention; Wherein the volume content of titanium aluminium carbide is greater than 99%.This embodiment has showed at ceiling temperature of the present invention and has synthesized the operational details of titanium aluminium carbide powder under near upper limit temperature rise rate situation.
Embodiment 2
A gross weight of the present invention is the small sample of 44.3 grams.Take by weighing Ti powder 30.0 grams, Al powder 6.0 grams, Graphite Powder 99 4.6 grams, Sn powder 3.7 grams, mix the back and add 31 milliliters of dehydrated alcohols and 100 gram agate balls, ball mill mixing 3 hours, dry, grind, cross 100 mesh sieves then, compacting under 20MPa pressure, put into the graphite jig of High Temperature Furnaces Heating Apparatus, argon shield, speed with 30 ℃/min is warming up to 1450 ℃, insulation 5min, speed with 10～15 ℃/min is reduced to 60 ℃ with furnace temperature, and the loose shape block that reaction is generated takes out, grinds, and promptly obtains titanium aluminium carbide powder of the present invention; Wherein the volume content of titanium aluminium carbide is greater than 98.5%.This embodiment has showed the operational details of synthetic titanium aluminium carbide powder under the situation of optional parameter in prescription of the present invention, synthesis temperature, temperature rise rate and blank forming pressure range.
Embodiment 3
Gross weight be 432.3 grams than large sample.Take by weighing Ti powder 287.5 grams, Al powder 54.0 grams, Graphite Powder 99 43.3 grams, Sn powder 47.5 grams, mix the back and add 303 milliliters of dehydrated alcohols and 1080 gram agate balls, ball mill mixing 6 hours, dry, grind, cross 100 mesh sieves then, compacting under 10 MPa pressure, put into the graphite jig of High Temperature Furnaces Heating Apparatus, argon shield, speed with 20 ℃/min is warming up to 1350 ℃, insulation 5min, speed with 10-15 ℃/min is reduced to 60 ℃ with furnace temperature, and the loose shape block that reaction is generated takes out, grinds, and promptly obtains titanium aluminium carbide powder of the present invention; Wherein the volume content of titanium aluminium carbide is greater than 98.0%.This embodiment has showed the operational details of synthetic titanium aluminium carbide powder under approaching lower limit temperature of the present invention and lower limit temperature rise rate situation.
Fig. 1 is the X-ray diffracting spectrum of the inventive method synthetic titanium aluminium carbide powder.This collection of illustrative plates shows uses the inventive method synthetic titanium aluminium carbide powder by the single phase composite of titanium aluminium carbide, does not have or have only few dephasign to exist.
Claims (2)
1. one kind is the titanium aluminium carbide powder preparation method of reaction promoter with tin, it is characterized in that: may further comprise the steps:
(1) batching: titanium (Ti) powder, aluminium (Al) powder, graphite (C) powder and tin (Sn) powder are massaged than Ti: Al: C: Sn=3.0: (0.9～1.1): (1.8～2.0): the ratio batching of (0.05～0.2);
(2) batch mixing: will prepare burden adds anhydrous ethanol medium, ball milling 2～6 hours, and 60～70 ℃ of oven dry down in baking oven afterwards, the mixing raw material with oven dry grinds again, crosses 70～100 mesh sieves;
(3) precompressed: the block that the dried feed behind the above-mentioned batch mixing is pressed into Any shape with the pressure of 10～20MPa;
(4) calcining: the mixing raw material of above-mentioned precompressed is put into the graphite jar and placed High Temperature Furnaces Heating Apparatus, under argon shield, temperature rise rate by 10～40 ℃/min, furnace temperature is risen to 1300 ℃～1550 ℃, insulation 5～10min, with the speed cooling of 10～15 ℃/min, obtain the loose shape block that generates by the mixing raw material reaction then;
(5) will react the loose shape block that generates and grind, can obtain titanium aluminium carbide powder.
2. titanium aluminium carbide powder with the preparation of the method for claim 1, it is characterized in that: its composition is as follows:
(1) Ti
3AlC
2The volume content of phase＞98%;
(2) volume content＜2% of titanium carbide (TiC) dephasign;
(3) Sn that adds as reaction promoter is solid-solubilized in Ti
3AlC
2Intragranular.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100465134C (en) * | 2007-02-09 | 2009-03-04 | 上海大学 | Method of preparing compact Ti3AlC2 ceramic by low-temperature non-pressure sintering |
| CN103922374A (en) * | 2014-04-29 | 2014-07-16 | 江苏大学 | Aluminium fluoride nano material as well as preparation method and application thereof |
| 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 |
| CN106396683B (en) * | 2016-08-29 | 2019-03-01 | 华北电力大学（保定） | A kind of titanium aluminium carbon and titanium carbide composite hydrogen storage material and preparation method thereof |
| CN107522202A (en) * | 2017-08-07 | 2017-12-29 | 四川大学 | A kind of stratiform two-dimensional material MXene preparation method and applications |
| CN108083278A (en) * | 2017-12-26 | 2018-05-29 | 佛山科学技术学院 | A kind of titanium aluminium tin carbon-coating shape solid solution powder 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 |
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| CN1460660A (en) * | 2003-06-20 | 2003-12-10 | 武汉理工大学 | Method for preparing single-phase compact titanium aluminium carbon block body material by using si as adjurant through hot pressing process |
| CN1460659A (en) * | 2003-06-20 | 2003-12-10 | 武汉理工大学 | Method for preparing single-phase compact titanium aluminium carbon block material by using Al as adjuvant through discharge plasma agglomeration process |
| CN1477080A (en) * | 2003-07-11 | 2004-02-25 | 清华大学 | Titanium aluminium carbon powder material and its high-temp, synthesis method |
| CN1594213A (en) * | 2004-06-23 | 2005-03-16 | 北京交通大学 | Titanium silicon carbon block material using aluminium as additive and its preparing method |
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|---|---|---|---|---|
| CN1460660A (en) * | 2003-06-20 | 2003-12-10 | 武汉理工大学 | Method for preparing single-phase compact titanium aluminium carbon block body material by using si as adjurant through hot pressing process |
| CN1460659A (en) * | 2003-06-20 | 2003-12-10 | 武汉理工大学 | Method for preparing single-phase compact titanium aluminium carbon block material by using Al as adjuvant through discharge plasma agglomeration process |
| CN1477080A (en) * | 2003-07-11 | 2004-02-25 | 清华大学 | Titanium aluminium carbon powder material and its high-temp, synthesis method |
| CN1594213A (en) * | 2004-06-23 | 2005-03-16 | 北京交通大学 | Titanium silicon carbon block material using aluminium as additive and its preparing method |
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