CN102181768A - A (Ti, nb)2AlC solid solution composite material and its preparation method - Google Patents
A (Ti, nb)2AlC solid solution composite material and its preparation method Download PDFInfo
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- CN102181768A CN102181768A CN 201010623880 CN201010623880A CN102181768A CN 102181768 A CN102181768 A CN 102181768A CN 201010623880 CN201010623880 CN 201010623880 CN 201010623880 A CN201010623880 A CN 201010623880A CN 102181768 A CN102181768 A CN 102181768A
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Abstract
The invention discloses a (Ti, Nb)2AlC solid solution composite material and a preparation method thereof. The preparation method comprises the following steps of: performing a hot pressed sintering process on 43.82 to 70.23 weight percent of Ti powder, 20.14 to 23.70 weight percent of Al powder, 6.66 to 8.85 weight percent of C powder and 0.78 to 25.81 weight percent of Nb2O5 powder; automatically generating a particle reinforced phase in the process of generating a matrix phase through a thermit reaction to prepare a fine crystal composite material of Al2O3 dispersed phase reinforced matrix phase Ti2AlC; and performing solid solution strengthening on the matrix phase by using Nb generated by a reaction. The material has high component adjustability, a low firing temperature, a uniform and compact structure, relatively low cost and a high mechanical property, and the application range of the composite material is widened; in addition, the firing temperature and hot-pressing pressure are reduced and the sitallization of crystal grains is realized during fast firing by the method.
Description
Technical field
The invention belongs to matrix material and make the field, particularly a kind of (Ti, Nb)
2AlC sosoloid matrix material and preparation method thereof.
Background technology
The ceramic layered material Ti of novel tertiary
2AlC has attracted lot of domestic and foreign scholar's broad research with its excellent properties.Ti
2AlC has the performance of 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
2The performance of AlC 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, this research adopts the Nb element to carry out study on the modification, but directly adopt the metal simple-substance raw materials cost 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 to Ti
2AlC has the Ti of analog structure
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
2Sintering is carried out in two kinds of powders mixing of AlC, perhaps with Al, C, TiO
2For raw material high temperature generates Ti by reduction reaction
2AlC/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.Patent (200910219290.8) has been reported and has been utilized high-energy ball milling to synthesize Ti
2AlC/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
2The AlC matrix 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)
2AlC sosoloid 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
2AlC sosoloid matrix material; This method is utilized cheap oxide compound Nb
2O
5Rather than, reduced raw materials cost with expensive metal simple-substance Nb; 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)
2AlC sosoloid 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 and C powder and metal oxide Nb
2O
5Carry out proportioning by following reaction formula:
2(1-x)Ti+(1+10x/3)Al+C+xNb
2O
5→(Ti
1-xNb
x)
2AlC+5x/3Al
2O
3 (1)(x＝0.004～0.1750)
The result is: a kind of (Ti, Nb)
2AlC sosoloid matrix material, the raw material moiety is: the Ti powder accounts for 43.82～70.23% of gross weight, and the Al powder accounts for 20.14～23.70% of gross weight, and the C powder accounts for 6.66～8.85% and Nb of gross weight
2O
5Powder accounts for 0.78～25.81% of gross weight.
A kind of (Ti, Nb)
2The preparation technology of AlC 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 and metal oxide Nb
2O
5By following proportioning weighing, the Ti powder accounts for 43.82～70.23% of gross weight, and the Al powder accounts for 20.14～23.70%, and the C powder accounts for 6.66～8.85% 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)
2AlC sosoloid matrix material.
Institute of the present invention synthetic (Ti, Nb)
2AlC sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for the 99.5-81.5% 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)
2AlC, wherein x gets 0.004～0.1750, and wild phase is Al
2O
3
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
2AlC carries out solution strengthening.Thereby prepared Al
2O
3The thin brilliant Ti of dispersion consolidatedization
2AlC 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.
Description of drawings
Accompanying drawing is the material phase analysis result of example one gained sample; X-coordinate is a diffraction angle, and ordinate zou is a diffraction peak intensity, and wherein matrix is (Ti mutually
0.9662Nb
0.0338)
2AlC; Wild phase is Al
2O
3As seen from the figure, this material purity is very high, except matrix phase and Al
2O
3Almost there is not other impurity phase outward.
Embodiment
Embodiment one
A kind of (Ti, Nb)
2AlC sosoloid matrix material, its raw material weight moiety is: 20.57%, the 1200 purpose C powder that 64.39%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 8.85% and Nb of gross weight
2O
5Powder accounts for 6.19% 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, 64.39%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for 20.57%, 1200 purpose C powder and account for 8.85% and Nb
2O
5Powder accounts for 6.19%;
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 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)
2AlC sosoloid matrix material.
Present embodiment prepared (Ti, Nb)
2AlC 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
0.9662, Nb
0.0338)
2AlC, wild phase are Al
2O
3
With reference to accompanying drawing, show that this material matrix has (Ti mutually
0.9662, Nb
0.0338)
2AlC contains the TiC phase of small amount of impurities, and wild phase is Al
2O
3Phase.
Embodiment two
A kind of (Ti, Nb)
2AlC sosoloid matrix material, its raw material weight moiety is: 20.15%, the 1200 purpose C powder that 68.27%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 8.50%, Nb
2O
5Powder accounts for 3.08% 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, 68.27%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for that 20.15%, 1200 purpose C powder account for 8.50%, Nb
2O
5Powder accounts for 3.08%;
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 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)
2AlC sosoloid matrix material.
Present embodiment prepared (Ti, Nb)
2AlC 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
0.9836, Nb
0.0164)
2AlC, wild phase are Al
2O
3
Embodiment three
A kind of (Ti, Nb)
2AlC sosoloid matrix material, its raw material weight moiety is: 21.43%, the 1200 purpose C powder that 56.83%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 7.69%, Nb
2O
5Powder accounts for 14.05% 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 and metal oxide Nb
2O
5By following proportioning weighing, 21.43%, the 1200 purpose C powder that 56.83%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 7.69%, Nb
2O
5Powder accounts for 14.05% 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 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)
2AlC sosoloid matrix material.
Present embodiment prepared (Ti, Nb)
2AlC 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
0.9277, Nb
0.0723)
2AlC, wild phase are Al
2O
3
Claims (9)
1. one kind (Ti, Nb)
2AlC sosoloid matrix material is characterized in that, the raw material moiety is: the Ti powder accounts for 43.82～70.23% of gross weight, and the Al powder accounts for 20.14～23.70% of gross weight, and the C powder accounts for 6.66～8.85% 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)
2AlC sosoloid matrix material is characterized in that, the raw material moiety is: 20.57%, the 1200 purpose C powder that 64.39%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 8.85% and Nb of gross weight
2O
5Powder accounts for 6.19% of gross weight.
3. according to claim 1 a kind of (Ti, Nb)
2AlC sosoloid matrix material is characterized in that, the raw material moiety is: 68.27%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for that 20.15%, 1200 purpose C powder account for 8.50%, Nb
2O
5Powder accounts for 3.08%.
4. one kind (Ti, Nb)
2The preparation technology of AlC 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 and C powder and and metal oxide Nb
2O
5By following proportioning weighing, the Ti powder accounts for 43.82～70.23% of gross weight, and the Al powder accounts for 20.14～23.70% of gross weight, and the C powder accounts for 6.66～8.85% 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, step 4 gained material is naturally cooled to room temperature get final product.
5. according to claim 5 a kind of (Ti, Nb)
2The preparation technology of AlC 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 and C powder and and metal oxide Nb
2O
5By following proportioning weighing, 20.57%, the 1200 purpose C powder that 64.39%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 8.85% and Nb of gross weight
2O
5Powder accounts for 6.19% 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 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, step 4 gained material is naturally cooled to room temperature get final product.
6. according to claim 5 a kind of (Ti, Nb)
2The preparation technology of AlC 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 and metal oxide Nb
2O
5By following proportioning weighing, 20.15%, the 1200 purpose C powder that 68.27%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 8.50%, Nb
2O
5Powder accounts for 3.08% 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 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, step 4 gained material is naturally cooled to room temperature get final product.
7. one kind (Ti, Nb)
2AlC sosoloid matrix material is characterized in that, it is made up of matrix phase and wild phase two portions, and matrix accounts for the 99.5-81.5% 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)
2AlC, wherein x gets 0.004～0.1750, and wild phase is Al
2O
3
8. according to claim 9 a kind of (Ti, Nb)
2AlC 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
0.9662, Nb
0.0338)
2AlC, wild phase are Al
2O
3
9. according to claim 9 a kind of (Ti, Nb)
2AlC 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
0.9836, Nb
0.0164)
2AlC, wild phase are Al
2O
3
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|---|---|---|---|
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576380A (en) * | 2003-06-30 | 2005-02-09 | 希尔蒂股份公司 | Hot press tool |
| CN101717253A (en) * | 2009-12-03 | 2010-06-02 | 陕西科技大学 | Al2O3/Ti2AlC ceramic composite material and preparation method thereof |
-
2010
- 2010-12-31 CN CN 201010623880 patent/CN102181768A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576380A (en) * | 2003-06-30 | 2005-02-09 | 希尔蒂股份公司 | Hot press tool |
| CN101717253A (en) * | 2009-12-03 | 2010-06-02 | 陕西科技大学 | Al2O3/Ti2AlC ceramic composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of the American Ceramic Society》 20100630 De-Tian Wan等 A New Method to Improve the High-Temperature Mechanical Properties of Ti3SiC2 by Substituting Ti with Zr, Hf, or Nb 第1749～1752页 1-9 第93卷, 第6期 * |
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Application publication date: 20110914 |