CN102181765B - A (Ti, cr)3AlC2/Al2O3composite material and its preparation method - Google Patents

A (Ti, cr)3AlC2/Al2O3composite material and its preparation method Download PDF

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CN102181765B
CN102181765B CN 201010623870 CN201010623870A CN102181765B CN 102181765 B CN102181765 B CN 102181765B CN 201010623870 CN201010623870 CN 201010623870 CN 201010623870 A CN201010623870 A CN 201010623870A CN 102181765 B CN102181765 B CN 102181765B
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朱建锋
韩娜
杨海波
林营
王芬
王莉丽
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Shaanxi Xinhui New Energy Technology Development Co Ltd
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Shaanxi University of Science and Technology
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Abstract

A (Ti, Cr)3AlC2/Al2O3 composite material and a preparation method thereof. The method comprises a hot-press sintering process according to ratios of 43.06-72.82% by weight of Ti powder, 14.03-19.19% by weight of Al powder, 9.67-12.26% by weight of C powder, and 0.89-28.08% by weight of Cr2O3 powder, and a fine crystalline composite material with an Al2O3 dispersed phase strengthening a matrix phase Ti3AlC2 is prepared by a thermite reaction which allows the autogeny of a particle reinforcing phase during the generation of the matrix phase, and the matrix phase is treated by solid solution strengthening by Cr generated in the reaction; the material has highly-adjustable components, low sintering temperature, a uniform and compact structure, low cost, excellent mechanical properties, which widens the application scope of the composite material; additionally, the invention reduces the sintering temperature and the hot-pressing pressure, and the microcrystallization of crystal grains is realized during rapid sintering.

Description

A kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material and preparation method thereof
Technical field
The invention belongs to matrix material and make field, particularly a kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material and preparation method thereof.
Background technology
In recent years, _ 2 Ceramics material Ti 3AlC 2Attracted lot of domestic and foreign scholar's broad research with its excellent properties.Ti 3AlC 2Performance with metal as having at normal temperatures good thermal conductivity and electroconductibility, lower Vickers' hardness, higher Young's modulus and shearing modulus, at room temperature can be carried out traditional mechanical workout, can produce viscous deformation under comparatively high temps; This material has again the performance of pottery, such as high-melting-point, high high-temp stability and good antioxidant property.But this material also exists sintering temperature high, and temperature range is little, and the shortcoming such as hardness is low, intensity is smaller and limited its further application.
For improving Ti 3AlC 2The performance of material, people utilize the means of solid solution highly malleablized and Composite that it has been carried out study on the modification, have obtained preferably effect.Such as bibliographical information (Surface ﹠amp; Coatings Technology 203 (2009) 3595-3609) utilize simple substance Cr element to carry out the solid solution study on the modification, material mechanical performance is greatly improved, but the method raw materials cost is higher, and synthesis temperature is higher simultaneously, is unfavorable for its industrialization production; Also there is document (ScriptaMaterialia 50 (2004) 897-901) report to utilize Al 2O 3Particle can be to Ti 3AlC 2Material property carries out modification.But currently used method is all more single, simultaneously, on the preparation method mainly with Al 2O 3And Ti 3AlC 2Sintering is carried out in two kinds of powders mixing, perhaps with Al, C, TiO 2For raw material high temperature generates Ti by reduction reaction 3AlC 2/ Al 2O 3Matrix material, but no matter all there is the temperature of reaction height in the sort of technique and the relatively low deficiency that waits of intensity, can't large-scale industrialized production.Document (Advanced Powder Technology 03 (2010) 1-4) has been reported and has been utilized high-energy ball milling to synthesize Ti 3AlC 2/ Al 2O 3The novel method of matrix material, the material that the method is synthesized is greatly improved in performance, but high-energy ball milling is difficult to suitability for industrialized production, simultaneously, matrix phase is not carried out the solid solution modification.Therefore, how to take effective approach, utilize cheap material to synthesize Al 2O 3The solid-solution type Ti of particle highly malleablized 3AlC 2Matrix material will become research emphasis from now on.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material and preparation method thereof utilizes Ti-Al-C-Cr 2O 3System is raw material, prepares Al by thermite reaction reaction in-situ technique low temperature 2O 3The Ti that strengthens 3AlC 2Solid solution composite material; The method is utilized cheap oxide compound Cr 2O 3Substitute expensive metal simple-substance, reduced raw materials cost; Utilize the reaction heat of thermite reaction self, reduced the synthesis temperature of material, simultaneously generated in-situ Al 2O 3The wild phase particle is tiny, even, and the performance of material is greatly improved, and prepared material has high-strength, fine and close, high temperature resistant, machinable characteristics.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material, its initial feed be purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Cr 2O 3, carry out proportioning by following reaction formula:
3(1-x)Ti+(1+3x)Al+2C+3x/2Cr 2O 3→(Ti 1-xCr x) 3AlC 2+3x/2Al 2O 3 (1)(x=0.0064~0.2555),
The result is: a kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material, the raw material moiety is: the Ti powder accounts for 43.06~72.82% of gross weight, and the Al powder accounts for 14.03~19.19% of gross weight, and the C powder accounts for 9.67~12.26% and Cr of gross weight 2O 3Powder accounts for 0.89~28.08% of gross weight.
A kind of (Ti, Cr) 3AlC 2/ Al 2O 3The composite manufacture method, step is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, carbon dust and metal oxide Cr 2O 3By following proportioning weighing, the Ti powder accounts for 43.06~72.82% of gross weight, and the Al powder accounts for 14.03~19.19% of gross weight, and the C powder accounts for 9.67~12.26% and Cr of gross weight 2O 3Powder accounts for 0.89~28.08% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 600~900 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 0.5~1.5 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 4~8 hours at 40~50 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, 1100 ℃~1400 ℃, the pressure hot pressed sintering of 5.0~30MPa 1~2 hour;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material.
(Ti, the Cr) that the present invention synthesized 3AlC 2/ Al 2O 3Matrix material is characterized in that: it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for 81.5~99.5%% of matrix material gross weight, and wild phase accounts for the 0.5-18.5% of gross weight, and matrix phase is (Ti 1-x, Cr x) 3AlC 2, wherein x gets 0.0064~0.2555, and wild phase is Al 2O 3If Al in the matrix material that generates 2O 3Growing amount does not have enhancing, toughness reinforcing Ti less than 0.5% of product quality 3AlC 2The effect of matrix, otherwise, if Al in the product 2O 3Phasor surpasses Ti 3AlC 2The content of matrix phase can not be referred to as Ti 3AlC 2Based composites, simultaneously, Al 2O 3Growing amount will be above 18.5%, excessive Al 2O 3Not only do not have and improve Ti 3AlC 2Effect, can worsen its performance on the contrary.Therefore determined above compositional range.
The present invention utilizes Ti powder, Al powder, C powder and Cr 2O 3Powder is raw material, by thermite reaction spontaneous particulates reinforcements Al in the process that matrix phase generates 2O 3The metal simple-substance Cr that restores simultaneously is to Ti 3AlC 2Carry out solution strengthening.Thereby prepared Al 2O 3The thin brilliant Ti of dispersion consolidatedization 3AlC 2Solid solution composite material.Because the material composition adjustability that this technique is synthesized is large, firing temperature is low, and even structure is fine and close, and cost is lower, and mechanical property is excellent, has widened the range of application of this matrix material.
Description of drawings
Fig. 1 is the material phase analysis result of example one gained sample; X-coordinate is diffraction angle, and ordinate zou is diffraction peak intensity, and wherein matrix phase is (Ti 0.9468Cr 0.0532) 3AlC 2Wild phase is Al 2O 3
Fig. 2 is the material phase analysis result of example two gained samples; X-coordinate is diffraction angle, and ordinate zou is diffraction peak intensity, and wherein matrix phase is (Ti 0.9740Cr 0.0260) 3AlC 2Wild phase is Al 2O 3
Embodiment
Embodiment one
A kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material, the raw material moiety is: 16.66%, the 1200 purpose C powder that 65.84%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.47%, Cr 2O 3Powder accounts for 7.03% of gross weight.
The step of preparation process of present embodiment is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, carbon dust and metal oxide Cr 2O 3By following proportioning weighing, 16.66%, the 1200 purpose C powder that 65.84%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.47%, Cr 2O 3Powder accounts for 7.03% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum condition, 1360 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material.
(Ti, the Cr) that present embodiment synthesized 3AlC 2/ Al 2O 3Matrix material with reference to Fig. 1, is characterized in that, it is comprised of matrix phase and wild phase two portions, wherein matrix phase (Ti 0.9477, Cr 0.0523) 3AlC 2Account for 96% of gross weight, Al 2O 3Account for mutually 4% of product total mass.
Embodiment two
A kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material, the raw material moiety is: 15.95%, the 1200 purpose C powder that 69.73%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.78%, Cr 2O 3Powder accounts for 3.54% of gross weight.
The step of preparation process of present embodiment is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, carbon dust and metal oxide Cr 2O 3By following proportioning weighing, 15.95%, the 1200 purpose C powder that 69.73%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.78%, Cr 2O 3Powder accounts for 3.54% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum condition, 1250 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material.
(Ti, the Cr) that present embodiment synthesized 3AlC 2/ Al 2O 3Matrix material is characterized in that, it is comprised of matrix phase and wild phase two portions, wherein matrix phase (Ti 0.9740, Cr 0.0260) 3AlC 2Account for 98% of gross weight, Al 2O 3Account for mutually product total mass 2%.
With reference to Fig. 2, show that this material matrix is by (Ti, Cr) 3AlC 2Phase contains a small amount of impurity TiC phase, and wild phase is Al 2O 3Phase.
Embodiment three
A kind of (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material, the raw material moiety is: 17.96%, the 1200 purpose C powder that 57.89%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.35%, Cr 2O 3Powder accounts for 13.80% of gross weight.
The manufacture method of present embodiment may further comprise the steps:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, carbon dust and metal oxide Cr 2O 3By following proportioning weighing, 17.96%, the 1200 purpose C powder that 57.89%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.35%, Cr 2O 3Powder accounts for 13.80% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio of ethanol=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum condition, 1360 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature can obtain (Ti, Cr) 3AlC 2/ Al 2O 3Matrix material.
(Ti, the Cr) that present embodiment synthesized 3AlC 2/ Al 2O 3Matrix material is characterized in that, it is comprised of matrix phase and wild phase two portions, wherein matrix phase (Ti 0.8886, Cr 0.1114) 3AlC 2Account for 92% of gross weight, Al 2O 3Account for mutually product total mass 8%.

Claims (6)

1. one kind (Ti, Cr) 3AlC 2/ Al 2O 3The composite manufacture method is characterized in that, step is as follows: step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, carbon dust and metal oxide Cr 2O 3By following proportioning weighing, the Ti powder accounts for 43.06~72.82% of gross weight, and the Al powder accounts for 14.03~19.19% of gross weight, and the C powder accounts for 9.67~12.26% and Cr of gross weight 2O 3Powder accounts for 0.89~28.08% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 600~900 rpms, material: ball: the mass ratio=1:3:1 of ethanol, ball milling 0.5~1.5 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 4~8 hours at 40~50 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, 1100 ℃~1400 ℃, the pressure hot pressed sintering of 5.0~30MPa 1~2 hour;
Step 5, the step 4 resulting materials is naturally cooled to room temperature get final product.
2. a kind of (Ti, Cr) according to claim 1 3AlC 2/ Al 2O 3The composite manufacture method is characterized in that, step is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, carbon dust and metal oxide Cr 2O 3By following proportioning weighing, 16.66%, the 1200 purpose C powder that 65. 84%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.47%, Cr 2O 3Powder accounts for 7.03% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio=1:3:1 of ethanol, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum condition, 1360 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature get final product.
3. a kind of (Ti, Cr) according to claim 1 3AlC 2/ Al 2O 3The composite manufacture method is characterized in that, step is as follows:
Step 1, at first with purity more than or equal to 99%, fineness is less than or equal to 200 purpose metal Ti powder, Al powder, carbon dust and metal oxide Cr 2O 3By following proportioning weighing, 15.95%, the 1200 purpose C powder that 69.73%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.78%, Cr 2O 3Powder accounts for 3.54% of gross weight;
Step 2, the batching in the step 1 is put into the alumina balls grinding jar carry out mixing and ball milling at planetary ball mill, take dehydrated alcohol as ball-milling medium, the rotating speed of ball mill is 800 rpms, material: ball: the mass ratio=1:3:1 of ethanol, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is lower dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum condition, 1250 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, the step 4 resulting materials is naturally cooled to room temperature get final product.
4. one kind (Ti, Cr) 3AlC 2/ Al 2O 3Solid solution composite material is characterized in that, it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for 81.5~99.5% of matrix material gross weight, and wild phase accounts for the 0.5-18.5% of gross weight, and matrix phase is (Ti 1-x, Cr x) 3AlC 2, wherein x gets 0.0064~0.2555, and wild phase is Al 2O 3
5. a kind of (Ti, Cr) according to claim 4 3AlC 2/ Al 2O 3Solid solution composite material is characterized in that, it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for 96% of matrix material gross weight, and wild phase accounts for 4% of gross weight, and matrix phase is (Ti 0.9477, Cr 0.0523) 3AlC 2, wild phase is Al 2O 3
6. a kind of (Ti, Cr) according to claim 4 3AlC 2/ Al 2O 3Solid solution composite material is characterized in that, it is comprised of matrix phase and wild phase two portions, and matrix phase accounts for 98% of matrix material gross weight, and wild phase accounts for 2% of gross weight, and matrix phase is (Ti 0.9740, Cr 0.0260) 3AlC 2, wild phase is Al 2O 3
CN 201010623870 2010-12-31 2010-12-31 A (Ti, cr)3AlC2/Al2O3composite material and its preparation method Expired - Fee Related CN102181765B (en)

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CN107042315A (en) * 2017-05-03 2017-08-15 济南大学 A kind of preparation method of titanium aluminum oxide cermet material
CN110116213B (en) * 2019-06-06 2022-04-01 陕西科技大学 One kind (Cr, Mo)2AlC solid solution material and preparation method thereof

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