CN101716680A - Method for preparing Ti2AlN/TiAl compound material by regulating and controlling components accurately - Google Patents
Method for preparing Ti2AlN/TiAl compound material by regulating and controlling components accurately Download PDFInfo
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- CN101716680A CN101716680A CN200910073422A CN200910073422A CN101716680A CN 101716680 A CN101716680 A CN 101716680A CN 200910073422 A CN200910073422 A CN 200910073422A CN 200910073422 A CN200910073422 A CN 200910073422A CN 101716680 A CN101716680 A CN 101716680A
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Abstract
The invention discloses a method for preparing a Ti2AlN/TiAl compound material by regulating and controlling components accurately, and relates to the method for preparing a compound material. The method for preparing the Ti2AlN/TiAl compound material by regulating and controlling the components accurately solves the problems that the prior method for preparing the Ti2AlN/TiAl compound material is easy to introduce impurities and is difficult to control the volume fraction of the Ti2AlN/TiAl on large scale. The method comprises the following steps: firstly, putting Ti powder, Al powder and TiN powder into a liquid dispersant according to certain percentage, ball-milling the mixture, and drying the mixture to obtain mixed powder; and secondly, putting the mixed powder into a graphite mold, preserving heat and pressure of the mixed powder at 700 DEG C, 900 DEG C and 1,300 DEG C respectively, and cooling the mixed powder to a room temperature in a furnace so as to obtain the Ti2AlN/TiAl compound material. The method for preparing the Ti2AlN/TiAl compound material of the invention cannot introduce the impurities, and can control the volume fraction of the Ti2AlN/TiAl on a large scale by regulating the addition of the TiN powder.
Description
Technical field
The present invention relates to a kind of preparation method of composite.
Background technology
The Ti of present report
2The preparation method of AlN/TiAl composite mainly contains following two kinds:
Spray deposition: with Ti, Al is injecting substances, injection atmosphere is mist (nitrogen+hydrogen), Ti drop, Al drop surface carburization in flight course, Fei Hang drop drops on the substrate of preheating subsequently, forms the target composite behind the enterprising single step reaction of substrate.The shortcoming of the method is: therefore the limited amount of Ti, Al drop surface absorption N element is difficult to control Ti on a large scale
2The volume fraction of AlN; Also contain the nitride and the Ti-Al based compound of a small amount of other kinds in the material that obtains, cause material impure; Ti in the gained material
2AlN is wavy distribution, causes the material anisotropy; The hole that contains some in the composite.
Mechanical alloying method: with Ti powder, Al powder is raw material, mechanical ball milling mixed powder under air, make the N element of Ti, Al particle surface absorption some in the knockout process, also inevitably adsorb simultaneously the O element of some, finally obtain the target composite behind mixed powder process vacuum of mechanical ball milling or the argon gas atmosphere hot pressed sintering.The shortcoming of the method is: introduced the O element because mix in the powder process early stage, so contain Al in the final material
2O
3The impurity phase; Introduce the N element by surface absorption, reaction, the content of N element is less, is difficult to realize controlling Ti on a large scale
2The volume fraction of AlN.
Summary of the invention
Technical problem to be solved by this invention is in order to solve existing preparation Ti
2The method of AlN/TiAl composite is easily introduced impurity, is difficult to realize controlling Ti on a large scale
2The problem of AlN volume fraction provides a kind of Ti
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately.
A kind of Ti of the present invention
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is as follows: one, Ti powder, Al powder, TiN powder and alloying element powder are put into liquid dispersant, be that 1: 5, rotating speed are ball milling 3 hours～24 hours under 300 rev/mins the condition in Ti powder, Al powder, TiN powder and alloying element powder gross weight and abrading-ball weight ratio then, be to dry under 50 ℃～100 ℃ conditions in temperature then, get mixed powder; Two, mixed powder being put into graphite jig, rise to 700 ℃ with 10 ℃/minute heating rates from room temperature, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 700 ℃, pressure then; Three, the graphite jig of putting into mixed powder that will handle through step 2 rises to 900 ℃ with 10 ℃/minute heating rate from 700 ℃, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 900 ℃, pressure then; Four, the graphite jig of putting into mixed powder that will handle through step 3 rises to 1300 ℃ with 10 ℃/minute heating rate from 900 ℃, be heat-insulation pressure keeping 0.5 hour～2 hours under the condition of 20MPa～60MPa at 1300 ℃, pressure then, cool to room temperature again with the furnace, promptly get Ti
2The AlN/TiAl composite; The addition of alloying element is 1%～5% of Ti powder, Al powder, TiN powder and an alloying element powder gross weight in the step 1, the mass ratio of Ti powder and Al powder is 62.74～95.22: 34.78～48.17, and the mass ratio of Ti powder and TiN powder is 62.74～95.22: 7.58～68.26; Liquid dispersant described in the step 1 is alcohol, acetone or distilled water; Alloying element described in the step 1 is a kind of or wherein several combination among Nb, Cr, Mn, Si and the B.
Following reaction: Ti+Al → TiAl takes place in the step 2 to four of the present invention successively
3+ Ti
3Al; TiAl
3+ Ti
3Al → TiAl+TiAl
2TiAl in the process of diffusion homogenising
2All be converted into TiAl; TiAl+TiN → Ti
2AlN, the Ti of TiAl and generation then
2AlN forms Ti
2The AlN/TiAl composite.
The present invention prepares Ti
2The method of AlN/TiAl composite is not introduced impurity, can control Ti on a large scale by the addition of adjusting the TiN powder
2The volume fraction of AlN, gained Ti of the present invention
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 10%～90%, and the atomic percent of Ti is 45%～65% in the TiAl matrix.
Description of drawings
Fig. 1 is the photo of organizing of the specific embodiment 11 gained TiAl materials; Fig. 2 is the specific embodiment 12 gained Ti
2AlN strengthens the photo of organizing of TiAl based composites; Fig. 3 is the specific embodiment 13 gained Ti
2AlN strengthens the photo of organizing of TiAl based composites; Fig. 4 is the specific embodiment 11 gained TiAl materials, the specific embodiment 12 gained Ti
2AlN strengthens TiAl based composites and the specific embodiment 13 gained Ti
2AlN strengthens the XRD curve comparison diagram of TiAl based composites, and a represents the XRD curve of the specific embodiment 11 gained TiAl materials among the figure, and b represents the specific embodiment 12 gained Ti
2AlN strengthens the TiAl based composites, and c represents the specific embodiment 13 gained Ti
2AlN strengthens the TiAl based composites, ◆ expression TiAl, ■ represents Ti
3Al, ▲ expression Ti
2AlN.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: a kind of Ti in the present embodiment
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is as follows: one, Ti powder, Al powder, TiN powder and alloying element powder are put into liquid dispersant, be that 1: 5, rotating speed are ball milling 3 hours～24 hours under 300 rev/mins the condition in Ti powder, Al powder, TiN powder and alloying element powder gross weight and abrading-ball weight ratio then, be to dry under 50 ℃～100 ℃ conditions in temperature then, get mixed powder; Two, mixed powder being put into graphite jig, rise to 700 ℃ with 10 ℃/minute heating rates from room temperature, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 700 ℃, pressure then; Three, the graphite jig of putting into mixed powder that will handle through step 2 rises to 900 ℃ with 10 ℃/minute heating rate from 700 ℃, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 900 ℃, pressure then; Four, the graphite jig of putting into mixed powder that will handle through step 3 rises to 1300 ℃ with 10 ℃/minute heating rate from 900 ℃, be heat-insulation pressure keeping 0.5 hour～2 hours under the condition of 20MPa～60MPa at 1300 ℃, pressure then, cool to room temperature again with the furnace, promptly get Ti
2AlN strengthens the TiAl based composites; The addition of alloying element is 1%～5% of Ti powder, Al powder, TiN powder and an alloying element powder gross weight in the step 1, the mass ratio of Ti powder and Al powder is 62.74～95.22: 34.78～48.17, and the mass ratio of Ti powder and TiN powder is 62.74～95.22: 7.58～68.26.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 10%～90%, and the atomic percent of Ti is 45%～65% in the TiAl matrix.
The specific embodiment two: what present embodiment and the specific embodiment one were different is that the liquid dispersant described in the step 1 is alcohol, acetone or distilled water, and other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is that the alloying element described in the step 1 is a kind of or wherein several combination among Nb, Cr, Mn, Si and the B.Other is identical with the specific embodiment one or two.
The specific embodiment four: present embodiment and the specific embodiment one to three are different be in the step 1 ball milling time be 15 hours.Other is identical with the specific embodiment one to three.
The specific embodiment five: present embodiment and the specific embodiment one to four are different is to be heat-insulation pressure keeping under the condition of 40MPa at 700 ℃, pressure in the step 2.Other is identical with the specific embodiment one to four.
The specific embodiment six: present embodiment and the specific embodiment one to five are different be in the step 2 heat-insulation pressure keeping time be 3 hours.Other is identical with the specific embodiment one to five.
The specific embodiment seven: present embodiment and the specific embodiment one to six are different be the graphite jig of putting into mixed powder that will handle through step 2 in the step 3 at 900 ℃, pressure is heat-insulation pressure keeping under the condition of 50MPa.Other is identical with the specific embodiment one to six.
The specific embodiment eight: present embodiment and the specific embodiment one to seven are different be in the step 3 heat-insulation pressure keeping time be 3 hours.Other is identical with the specific embodiment one to seven.
The specific embodiment nine: present embodiment and the specific embodiment one to eight are different be the graphite jig of putting into mixed powder that will handle through step 3 in the step 4 at 1300 ℃, pressure is heat-insulation pressure keeping 1 hour under the condition of 30MPa.Other is identical with the specific embodiment one to eight.
The specific embodiment ten: present embodiment and the specific embodiment one to nine are different is that the addition of alloying element in the step 1 is 4% of Ti powder, Al powder, TiN powder and an alloying element powder gross weight.Other is identical with the specific embodiment one to nine.
The specific embodiment 11: the TiAl preparation methods is as follows in the present embodiment: one, Ti powder and Al powder are put into liquid dispersant, be that 1: 5, rotating speed are ball milling 3 hours～24 hours under 300 rev/mins the condition in Ti powder and Al powder gross weight and abrading-ball weight ratio then, be to dry under 50 ℃～100 ℃ conditions in temperature then, get mixed powder; Two, mixed powder being put into graphite jig, rise to 700 ℃ with 10 ℃/minute heating rates from room temperature, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 700 ℃, pressure then; Three, the graphite jig of putting into mixed powder that will handle through step 2 rises to 900 ℃ with 10 ℃/minute heating rate from 700 ℃, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 900 ℃, pressure then; Four, the graphite jig of putting into mixed powder that will handle through step 3 rises to 1300 ℃ with 10 ℃/minute heating rate from 900 ℃, be heat-insulation pressure keeping 0.5 hour～2 hours under the condition of 20MPa～60MPa at 1300 ℃, pressure then, cool to room temperature again with the furnace, promptly get the TiAl material; The mass ratio of Ti powder and Al powder is 62.74～95.22: 34.78～48.17 in the step 1.
The specific embodiment 12: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 91.16: 46.5: 15.17.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 20%.
The specific embodiment 13: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 79: 41.5: 38.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 50%.
In the present embodiment with TiAl material, the specific embodiment 12 gained Ti of the specific embodiment 11 gained
2AlN/TiAl composite, the specific embodiment 13 gained Ti
2The AlN/TiAl composite is that 900 ℃, strain rate are 10 in temperature respectively
-3Condition under carry out compression test, result of the test such as table 1:
The performance data of three kinds of materials of table 1
| Material category | Hardness MPa | Elastic modulus G Pa | Compressive strength MPa |
| The TiAl material of the specific embodiment 11 gained | ??471 | ??168 | ??515 |
| The specific embodiment 12 gained Ti 2The AlN/TiAl composite | ??509 | ??173 | ??565 |
| The specific embodiment 13 gained Ti 2The AlN/TiAl composite | ??604 | ??193 | ??671 |
The specific embodiment 12 gained Ti as shown in Table 1
2AlN/TiAl composite, the specific embodiment 13 gained Ti
2The hardness of AlN/TiAl composite, elastic modelling quantity and compressive strength be big than the specific embodiment 11 gained TiAl materials all.
The specific embodiment 12 gained Ti as shown in Figure 4
2AlN strengthens TiAl based composites and the specific embodiment 13 gained Ti
2Do not contain impurity in the AlN enhancing TiAl based composites.
The specific embodiment 14: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 95.22: 48.17: 7.58.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 10%.
The specific embodiment 15: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 87.1: 44.82: 22.75.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 30%.
The specific embodiment 16: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 83.04: 43.15: 30.34.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 40%.
The specific embodiment 17: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 74.92: 39.8: 53.1.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 60%.
The specific embodiment 18: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 70.86: 38.12: 53.1.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 70%.
The specific embodiment 19: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 66.8: 36.45: 60.68.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 80%.
The specific embodiment 20: what present embodiment and the specific embodiment one were different is Ti powder in the step 1: the Al powder: the mass ratio of TiN powder is 62.74: 34.78: 68.26.Other is identical with the specific embodiment one.
Present embodiment gained Ti
2AlN strengthens Ti in the TiAl based composites
2The volume fraction of AlN is 90%.
Claims (10)
1. Ti
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that Ti
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is as follows: one, Ti powder, Al powder, TiN powder and alloying element powder are put into liquid dispersant, be that 1: 5, rotating speed are ball milling 3 hours～24 hours under 300 rev/mins the condition in Ti powder, Al powder, TiN powder and alloying element powder gross weight and abrading-ball weight ratio then, be to dry under 50 ℃～100 ℃ conditions in temperature then, get mixed powder; Two, mixed powder being put into graphite jig, rise to 700 ℃ with 10 ℃/minute heating rates from room temperature, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 700 ℃, pressure then; Three, the graphite jig of putting into mixed powder that will handle through step 2 rises to 900 ℃ with 10 ℃/minute heating rate from 700 ℃, is heat-insulation pressure keeping 1 hour～4 hours under the condition of 20MPa～60MPa at 900 ℃, pressure then; Four, the graphite jig of putting into mixed powder that will handle through step 3 rises to 1300 ℃ with 10 ℃/minute heating rate from 900 ℃, be heat-insulation pressure keeping 0.5 hour～2 hours under the condition of 20MPa～60MPa at 1300 ℃, pressure then, cool to room temperature again with the furnace, promptly get Ti
2The AlN/TiAl composite; The addition of alloying element is 1%～5% of Ti powder, Al powder, TiN powder and an alloying element powder gross weight in the step 1, the mass ratio of Ti powder and Al powder is 62.74～95.22: 34.78～48.17, and the mass ratio of Ti powder and TiN powder is 62.74～95.22: 7.58～68.26.
2. a kind of Ti according to claim 1
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that the liquid dispersant described in the step 1 is alcohol, acetone or distilled water.
3. a kind of Ti according to claim 1 and 2
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that the alloying element described in the step 1 is a kind of or wherein several combination among Nb, Cr, Mn, Si and the B.
4. a kind of Ti according to claim 3
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that the ball milling time is 15 hours in the step 1.
5. according to claim 1,2 or 4 described a kind of Ti
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that in the step 2 that at 700 ℃, pressure be heat-insulation pressure keeping under the condition of 40MPa.
6. a kind of Ti according to claim 5
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that the heat-insulation pressure keeping time is 3 hours in the step 2.
7. according to claim 1,2,4 or 6 described a kind of Ti
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that in the step 3 that the graphite jig of putting into mixed powder that will handle through step 2 is heat-insulation pressure keeping under the condition of 50MPa at 900 ℃, pressure.
8. a kind of Ti according to claim 7
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that the heat-insulation pressure keeping time is 3 hours in the step 3.
9. according to claim 1,2,4,6 or 8 described a kind of Ti
2The preparation method of AlN/TiAl compound material by regulating and controlling components accurately is characterized in that in the step 4 that the graphite jig of putting into mixed powder that will handle through step 3 is heat-insulation pressure keeping 1 hour under the condition of 40MPa at 1300 ℃, pressure.
10. the preparation method of a kind of Ti2AlN/TiAl compound material by regulating and controlling components accurately according to claim 9, the addition that it is characterized in that alloying element in the step 1 are 4% of Ti powder, Al powder, TiN powder and alloying element powder gross weight.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139370A (en) * | 2011-01-14 | 2011-08-03 | 广州有色金属研究院 | Method for preparing Ti2AlC self-lubricating and heat-resisting structural material |
| CN102418000A (en) * | 2011-12-14 | 2012-04-18 | 哈尔滨工业大学 | Three-dimensional network distributed Ti2AlN particle reinforced TiAl-based composite material and preparation method thereof |
| CN105779825A (en) * | 2016-03-21 | 2016-07-20 | 太原理工大学 | TiAl alloy self-lubricating material and preparation method thereof |
| CN106187199A (en) * | 2016-07-05 | 2016-12-07 | 陕西科技大学 | A kind of highly-textured Ti2the preparation method of AlN ceramic |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100488669C (en) * | 2006-03-06 | 2009-05-20 | 陕西科技大学 | TiAl/Ti2AlN intermetallic compound composite material and its preparing method |
| CN100404465C (en) * | 2006-10-30 | 2008-07-23 | 陕西科技大学 | Method for preparing TiN/Al2O3 composite materials |
-
2009
- 2009-12-15 CN CN2009100734220A patent/CN101716680B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139370A (en) * | 2011-01-14 | 2011-08-03 | 广州有色金属研究院 | Method for preparing Ti2AlC self-lubricating and heat-resisting structural material |
| CN102418000A (en) * | 2011-12-14 | 2012-04-18 | 哈尔滨工业大学 | Three-dimensional network distributed Ti2AlN particle reinforced TiAl-based composite material and preparation method thereof |
| CN102418000B (en) * | 2011-12-14 | 2013-03-13 | 哈尔滨工业大学 | Preparation method of three-dimensional network distributed Ti2AlN particle reinforced TiAl-based composite material |
| CN105779825A (en) * | 2016-03-21 | 2016-07-20 | 太原理工大学 | TiAl alloy self-lubricating material and preparation method thereof |
| CN105779825B (en) * | 2016-03-21 | 2017-08-22 | 太原理工大学 | A kind of TiAl alloy self-lubricating material and preparation method thereof |
| CN106187199A (en) * | 2016-07-05 | 2016-12-07 | 陕西科技大学 | A kind of highly-textured Ti2the preparation method of AlN ceramic |
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