CN102041425A - (Ti, Nb) 3AlC2/Al2O3 solid solution composite material and preparation method thereof - Google Patents

(Ti, Nb) 3AlC2/Al2O3 solid solution composite material and preparation method thereof Download PDF

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CN102041425A
CN102041425A CN2010106238890A CN201010623889A CN102041425A CN 102041425 A CN102041425 A CN 102041425A CN 2010106238890 A CN2010106238890 A CN 2010106238890A CN 201010623889 A CN201010623889 A CN 201010623889A CN 102041425 A CN102041425 A CN 102041425A
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朱建锋
韩娜
林营
杨海波
陈平
杨文文
叶兰
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Phenom Innovations Xi''an Co ltd
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a (Ti, Nb) 3AlC2/Al2O3 solid solution composite material and a preparation method thereof. The preparation method comprises the following steps: hot pressing and sintering the following materials in percentage by weight: 45.87-72.95% of Ti powder, 14.02-19.10% of Al powder, 9.23-12.25% of C powder and 0.78-25.81% of Nb2O5 powder, wherein a particle wild phase grows in the matrix phase generating process via thermit reaction, a fine crystal composite material of Al2O3 dispersed phase strengthened matrix phase Ti3AlC2 is prepared, and Nb generated by the reaction is used for carrying out solid solution strengthening on the matrix. Because the material ingredients have big adjustability, low firing temperature, even and compact structure, lower cost and excellent mechanical property, the application range of the composite material is expanded. In addition, the method lowers the firing temperature and the hot-press pressure and realizes crystalline grain micritization in the quick firing process.

Description

A kind of (Ti, Nb) 3AlC 2/ Al 2O 3Sosoloid matrix material and preparation method thereof
Technical field
The invention belongs to matrix material and make the field, particularly a kind of (Ti, Nb) 3AlC 2/ Al 2O 3Sosoloid matrix material and preparation method thereof.
Background technology
Novel lamellar stupalith Ti 3AlC 2Attracted lot of domestic and foreign scholar's broad research with its excellent properties.Ti 3AlC 2Performance with metal as having good thermal conductivity and electroconductibility, lower Vickers' hardness, higher modulus of elasticity and shearing modulus at normal temperatures, can carrying out traditional mechanical workout, has plasticity under comparatively high temps; This material has the performance of pottery again, as high-melting-point, high thermal stability and good antioxidant property.But also there is the sintering temperature height in this material, and temperature range is little, and shortcoming such as hardness is low, strength ratio is less and limited its further application.
In recent years, for improving Ti 3AlC 2The performance of material, people utilize the means of solid solution highly malleablized and compoundization that it has been carried out study on the modification, have obtained effect preferably.(Scripta Materialia 53 (2005) 1369-1372) utilize the simple substance V element to carry out the solid solution study on the modification as bibliographical information, its mechanical property is greatly improved, same principle we can utilize the Nb element that it is carried out molten admittedly modification, but this method raw materials cost is higher, synthesis temperature is higher simultaneously, is unfavorable for its industrialization production; Also there is document (Scripta Materialia 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 technology, and undercapacity, can't large-scale industrialized production.Document (AdvancedPowder 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, this method institute synthetic material is greatly improved on performance, but high-energy ball milling is difficult to suitability for industrialized production, simultaneously, matrix is not carried out the solid solution modification mutually.Therefore, how to take valid approach, utilize cheap material to synthesize Al 2O 3The solid solution type Ti of particle highly malleablized 3AlC 2Matrix material is a 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, Nb) 3AlC 2/ Al 2O 3Sosoloid matrix material and preparation method thereof utilizes Ti-Al-C-Nb 2O 5System is a raw material, prepares Al by thermite reaction reaction in technology low temperature 2O 3The Ti that strengthens 3AlC 2The sosoloid matrix material; This method is utilized cheap oxide compound Nb 2O 5Substitute expensive metal simple-substance, reduced raw materials cost; Utilize the reaction heat of thermite reduction 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; The material of preparation 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, Nb) 3AlC 2/ Al 2O 3Sosoloid matrix material, its initial feed be purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb 2O 5Carry out proportioning by following reaction formula:
3(1-x)Ti+(1+5x)Al+2C+3x/2Nb 2O 5→(Ti 1-xNb x) 3AlC 2+5x/2Al 2O 3 (1)(x=0.0039~0.1685),
The result is: a kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material, the raw material moiety is: the Ti powder accounts for 45.87~72.95% of gross weight, and the Al powder accounts for 14.02~19.10% of gross weight, and the C powder accounts for 9.23~12.25% and Nb of gross weight 2O 5Powder accounts for 0.78~25.81% of gross weight.
A kind of (Ti, Nb) 3AlC 2/ Al 2O 3The preparation technology of sosoloid matrix material the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb 2O 5By following proportioning weighing, the Ti powder accounts for 45.87~72.95% of gross weight, and the Al powder accounts for 14.02~19.10%, and the C powder accounts for 9.23~12.25% and Nb 2O 5Powder accounts for 0.78~25.81%;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar on planetary ball mill, carry out mixing and ball milling, with the dehydrated alcohol is ball-milling medium, the rotating speed of ball mill is 600~900 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 0.5~1.5 hour;
Step 3, the ball milling powder of step 2 gained is following 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, at 1100 ℃~1400 ℃, the pressure hot pressed sintering of 5.0~30MPa 1~2 hour;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material.
Institute of the present invention synthetic (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for the 81.5-99.5% of matrix material gross weight mutually, and wild phase accounts for the 0.5-18.5% of gross weight, and matrix is (Ti mutually 1-x, Nb x) 3AlC 2, wherein x gets 0.0039~0.1685, 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 Nb 2O 5Powder is a raw material, by thermite reaction spontaneous particle wild phase Al in the process that matrix generates mutually 2O 3The metal simple-substance Nb that restores simultaneously is to Ti 3AlC 2Carry out solution strengthening.Thereby prepared Al 2O 3The thin brilliant Ti of dispersion consolidatedization 3AlC 2The sosoloid matrix material.Because this technology institute synthetic material composition adjustability is big, firing temperature is low, the even structure densification, and cost is lower, and the mechanical property excellence has been widened the range of application of this matrix material.
Embodiment
Embodiment one
A kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material, its raw material weight moiety is: 15.08%, the 1200 purpose C powder that 66.79%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.55% and Nb of gross weight 2O 5Powder accounts for 6.58% 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 smaller or equal to 200 purpose metal Ti powder, Al powder and C powder and metal oxide Nb 2O 5By following proportioning weighing, 15.08%, the 1200 purpose C powder that 66.79%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.55% and Nb of gross weight 2O 5Powder accounts for 6.58% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar carrying out mixing and ball milling on planetary ball mill, is ball-milling medium with the dehydrated alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material.
Present embodiment institute synthetic (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for 96% of matrix material gross weight mutually, and wild phase accounts for 4% of gross weight, and matrix is (Ti mutually 0.9675, Nb 0.0325) 3AlC 2, wild phase is Al 2O 3
Embodiment two
A kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material, its raw material weight moiety is: 14.46%, the 1200 purpose C powder that 70.23%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.93% and Nb of gross weight 2O 5Powder accounts for 3.38% 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 smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb 2O 5By following proportioning weighing, 14.46%, the 1200 purpose C powder that 70.23%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 11.93%, Nb 2O 5Powder accounts for 3.38% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar carrying out mixing and ball milling on planetary ball mill, is ball-milling medium with the dehydrated alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 47 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material.
Present embodiment institute synthetic (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for 98% of matrix material gross weight mutually, and wild phase accounts for 2% of gross weight, and matrix is (Ti mutually 0.9842, Nb 0.0158) 3AlC 2, wild phase is Al 2O 3
Embodiment three
A kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material, its raw material weight moiety is: 59.92%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for 16.31%, 1200 purpose C powder and account for 10.77% and Nb 2O 5Powder accounts for 13.00%.
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 smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb 2O 5By following proportioning weighing, 16.31%, the 1200 purpose C powder that 59.92%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 10.77%, Nb 2O 5Powder accounts for 13.00% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar carrying out mixing and ball milling on planetary ball mill, is ball-milling medium with the dehydrated alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material.
Present embodiment institute synthetic (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for 92% of matrix material gross weight mutually, and wild phase accounts for 8% of gross weight, and matrix is (Ti mutually 0.9304, Nb 0.0696) 3AlC 2, wild phase is Al 2O 3

Claims (9)

1. one kind (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that, the raw material moiety is: the Ti powder accounts for 45.87~72.95% of gross weight, and the Al powder accounts for 14.02~19.10% of gross weight, and the C powder accounts for 9.23~12.25% and Nb of gross weight 2O 5Powder accounts for 0.78~25.81% of gross weight.
2. according to claim 1 a kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that, the raw material moiety is: 15.08%, the 1200 purpose C powder that 66.79%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.55% and Nb of gross weight 2O 5Powder accounts for 6.58% of gross weight.
3. according to claim 1 a kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that, the raw material moiety is: 14.46%, the 1200 purpose C powder that 70.23%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.93% and Nb of gross weight 2O 5Powder accounts for 3.38% of gross weight.
4. one kind (Ti, Nb) 3AlC 2/ Al 2O 3The preparation technology of sosoloid matrix material is characterized in that, the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb 2O 5By following proportioning weighing, the Ti powder accounts for 45.87~72.95% of gross weight, and the Al powder accounts for 14.02~19.10% of gross weight, and the C powder accounts for 9.23~12.25% and Nb of gross weight 2O 5Powder accounts for 0.78~25.81% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar on planetary ball mill, carry out mixing and ball milling, with the dehydrated alcohol is ball-milling medium, the rotating speed of ball mill is 600~900 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 0.5~1.5 hour;
Step 3, the ball milling powder of step 2 gained is following 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, at 1100 ℃~1400 ℃, the pressure hot pressed sintering of 5.0~30MPa 1~2 hour;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material.
5. according to claim 4 a kind of (Ti, Nb) 3AlC 2/ Al 2O 3The preparation technology of sosoloid matrix material is characterized in that, the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb 2O 5By following proportioning weighing, 15.08%, the 1200 purpose C powder that 66.79%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 11.55% and Nb of gross weight 2O 5Powder accounts for 6.53% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar carrying out mixing and ball milling on planetary ball mill, is ball-milling medium with the dehydrated alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material.
6. according to claim 4 a kind of (Ti, Nb) 3AlC 2/ Al 2O 3The preparation technology of sosoloid matrix material is characterized in that, the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and metal oxide Nb 2O 5By following proportioning weighing, 14.46%, the 1200 purpose C powder that 70.23%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 11.93%, Nb 2O 5Powder accounts for 3.38% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar carrying out mixing and ball milling on planetary ball mill, is ball-milling medium with the dehydrated alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 47 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material.
7. one kind (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that, it is made up of matrix phase and wild phase two portions, and matrix accounts for the 81.5-99.5% of matrix material gross weight mutually, and wild phase accounts for the 0.5-18.5% of gross weight, and matrix is (Ti mutually 1-x, Nb x) 3AlC 2, wherein x gets 0.0039~0.1685, and wild phase is Al 2O 3
According to claim 7 described a kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that, it is made up of matrix phase and wild phase two portions, and matrix accounts for 96% of matrix material gross weight mutually, and wild phase accounts for 4% of gross weight, and matrix is (Ti mutually 0.9675, Nb 0.0325) 3AlC 2, wild phase is Al 2O 3
According to claim 7 described a kind of (Ti, Nb) 3AlC 2/ Al 2O 3The sosoloid matrix material is characterized in that, it is made up of matrix phase and wild phase two portions, and matrix accounts for 98% of matrix material gross weight mutually, and wild phase accounts for 2% of gross weight, and matrix is (Ti mutually 0.9842, Nb 0.0158) 3AlC 2, wild phase is Al 2O 3
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