CN100404465C - Method for preparing TiN/Al2O3 composite materials - Google Patents
Method for preparing TiN/Al2O3 composite materials Download PDFInfo
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- CN100404465C CN100404465C CNB2006101048145A CN200610104814A CN100404465C CN 100404465 C CN100404465 C CN 100404465C CN B2006101048145 A CNB2006101048145 A CN B2006101048145A CN 200610104814 A CN200610104814 A CN 200610104814A CN 100404465 C CN100404465 C CN 100404465C
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Abstract
This invention discloses a method for preparing TiN/Al2O3 composite material. The method comprises: preparing a mixture of Ti, Al and TiO2, adding sodium stearate dispersant into the mixture, performing dry ball-milling for mechanically alloying and obtaining alloyed amorphous powder with TiAl as the major crystalline, drying, loading into a graphite mold, and hot-pressing sintering in Ar or vacuum. The method adopts inexpensive Ti, Al and TiO2 as the raw materials, and utilizes high energy ball-milling to synthesize ultra-fine TiAl(NO) composite powder without protective atmosphere, which is then hot-pressing sintered in vacuum at a relatively low temperature to form TiN-particle-reinforced Al2O3 composite material. The method has such advantages as reduced preparation temperature, and improved material performance.
Description
Technical field
The invention belongs to material science, particularly a kind of TiN/Al
2O
3The preparation method of matrix material.
Background technology
The corundum porcelain has advantages such as the big and chemical stability of high temperature resistant, corrosion-resistant, wear-resisting, hardness, insulativity, dielectricity excellence because of it, in the application in fields such as electronics, electric power, oil, chemical industry, weaving more and more widely.But higher firing temperature not only makes cost increase but also technology difficulty is strengthened in preparation process.Simultaneously the same with other stupaliths, owing to lack slip system, its essential fragility has limited Al
2O
3The application of pottery.Toughness reinforcing Al
2O
3The method of pottery is a lot, and wherein particle dispersion is toughness reinforcing is one of effective toughness reinforcing mode, promptly passes through at Al
2O
3The middle second phase particle that adds significantly improves its toughness.
TiN has excellent physics, chemical property, can be used as the refractory high-abrasive material, also can be used as electrode and contact material.Recently, TiN particle REINFORCED Al
2O
3Composite study also day by day increases, at Al
2O
3The TiN that induces one in the matrix can utilize its advantage separately, prepares high performance high-temperature structural material, not only can improve its intensity, toughness and wear resistance, can also improve its conductivity, makes it be used to make the high-temperature wearable structure unit.In addition, this class electro-conductive material also has the ceramic component that can utilize the spark technology manufacturing complex shapes, reduces the advantage of processing charges significantly.TiN-Al
2O
3More traditional complex method is with Al
2O
3Powder and TiN powder mechanically mixing, sintering again after the moulding, this method makes the manufacturing cost raising on the one hand because the TiN price is higher, on the other hand, easily cause the reunion of adding phase, or cause local component deviation, finally cause descending of matrix material for learning performance and conductivity.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of and can effectively reduce microstructural ununiformity in the matrix material, it is tiny simultaneously can to synthesize crystal grain, even nano level matrix material, fundamentally solves the TiN/Al of the fragility problem of stupalith
2O
3The preparation method of matrix material.
For achieving the above object, the technical solution used in the present invention is: at first by mass percentage with the Al of Ti, the 36-58% of 0-64% and the TiO of 0-44%
2Make mixture; Add the sodium stearate dispersion agent of mixture quality 0.2-0.5% in mixture, adopt dry ball milling, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder was descended dry 4-5 hour at 70-80 ℃; Dried powder is packed in the graphite jig, and with 1200-1300 ℃, the pressure hot pressed sintering of 10-35MPa got final product in 1-2 hour under argon gas or vacuum condition.
The present invention adopts cheap raw material Ti, Al and TiO
2, utilize high-energy ball milling technology, be the alloying amorphous powder of TiAl (NO) not having to have synthesized principal phase under the atmosphere protection condition, the back is by hot-pressing sintering technique under the vacuum atmosphere, and original position generates TiN particle strengthening Al under lower temperature
2O
3Matrix material has not only reduced the preparation temperature of material, has improved the performance of material, also makes the manufacturing cost of this material reduce significantly.
Description of drawings
The powder that Fig. 1 obtains for alloying is through the XRD analysis result of 1300 ℃ of sintered specimens, and wherein X-coordinate is that XRD tests 2 θ angles, and ordinate zou is a diffraction peak intensity;
Fig. 2 is the cross-section morphology figure of 1300 ℃ of sintered specimens.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1, at first by mass percentage 64% Ti and 36% Al made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.3%, adopting dry ball milling is 760 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 30 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4 hours at 80 ℃; Dried powder is packed in the graphite jig, and with 1200 ℃, the pressure hot pressed sintering of 35MPa got final product in 1 hour under the argon gas condition.
Embodiment 2, at first by mass percentage with 58% Al and 42% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.5%, adopting dry ball milling is 710 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 34 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.3 hours at 75 ℃; Dried powder is packed in the graphite jig, and with 1250 ℃, the pressure hot pressed sintering of 28MPa got final product in 1.3 hours under vacuum condition.
Embodiment 3, at first by mass percentage with 16% Ti, 40% Al and 44% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.2%, adopting dry ball milling is 750 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 32 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.5 hours at 73 ℃; Dried powder is packed in the graphite jig, and with 1210 ℃, the pressure hot pressed sintering of 16MPa got final product in 1.5 hours under the argon gas condition.
Embodiment 4, at first by mass percentage with 30% Ti, 50% Al and 20% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.4%, adopting dry ball milling is 780 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 35 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 5 hours at 77 ℃; Dried powder is packed in the graphite jig, and with 1270 ℃, the pressure hot pressed sintering of 30MPa got final product in 1.8 hours under vacuum condition.
Embodiment 5, at first by mass percentage with 45% Ti, 45% Al and 10% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.2%, adopting dry ball milling is 700 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 31 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.7 hours at 79 ℃; Dried powder is packed in the graphite jig, and with 1290 ℃, the pressure hot pressed sintering of 25MPa got final product in 1.4 hours under the argon gas condition.
Embodiment 6, at first by mass percentage with 9% Ti, 55% Al and 36% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.5%, adopting dry ball milling is 800 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 33 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.1 hours at 70 ℃; Dried powder is packed in the graphite jig, and with 1300 ℃, the pressure hot pressed sintering of 10MPa got final product in 2 hours under vacuum condition.
Embodiment 7, at first by mass percentage with 55% Ti, 40% Al and 5% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.3%, adopting dry ball milling is 730 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 35 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.8 hours at 71 ℃; Dried powder is packed in the graphite jig, and with 1260 ℃, the pressure hot pressed sintering of 20MPa got final product in 1.7 hours under vacuum condition.
Referring to Fig. 1, as seen from Figure 1 according to preparation method of the present invention in the XRD analysis result of 1300 ℃ of sintered specimens, the principal crystalline phase that obtains is TiN and Al
2O
3Phase.
Referring to Fig. 2, this material grains that makes according to preparation method of the present invention is tiny as seen from Figure 2, compact structure, pore-free.
The present invention utilizes Ti powder, Al powder TiO
2And a small amount of additive is after high-energy ball milling is decrystallized, and reaction in generates super-refinement TiN/Al
2O
3Matrix material, because this material composition adjustability is big, firing temperature is low, the even structure densification, cost is lower.Widened the range of application of this matrix material.
Claims (9)
1. TiN/Al
2O
3The preparation method of matrix material is characterized in that:
1) at first by mass percentage with the Al of Ti, the 36-58% of 0-64% and the TiO of 0-44%
2Make mixture;
2) the sodium stearate dispersion agent of adding mixture quality 0.2-0.5% in mixture adopts dry ball milling, makes its mechanical alloying, and the formation principal phase is the alloying amorphous powder of TiAl (NO);
3) the alloying amorphous powder was descended dry 4-5 hour at 70-80 ℃;
4) dried powder is packed in the graphite jig, with 1200-1300 ℃, the pressure hot pressed sintering of 10-35MPa got final product in 1-2 hour under argon gas or vacuum condition.
2. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: said dry ball milling employing rotating speed is 700-800 rpm a planetary ball mill, and the pellet mass ratio is 1: 10, and the ball milling time is 30-35 hour.
3. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: at first by mass percentage 64% Ti and 36% Al are made mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.3%, adopting dry ball milling is 760 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 30 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4 hours at 80 ℃; Dried powder is packed in the graphite jig, and with 1200 ℃, the pressure hot pressed sintering of 35MPa got final product in 1 hour under the argon gas condition.
4. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: at first by mass percentage with 58% Al and 42% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.5%, adopting dry ball milling is 710 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 34 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.3 hours at 75 ℃; Dried powder is packed in the graphite jig, and with 1250 ℃, the pressure hot pressed sintering of 28MPa got final product in 1.3 hours under vacuum condition.
5. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: at first by mass percentage with 16% Ti, 40% Al and 44% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.2%, adopting dry ball milling is 750 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 32 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.5 hours at 73 ℃; Dried powder is packed in the graphite jig, and with 1210 ℃, the pressure hot pressed sintering of 16MPa got final product in 1.5 hours under the argon gas condition.
6. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: at first by mass percentage with 30% Ti, 50% Al and 20% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.4%, adopting dry ball milling is 780 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 35 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 5 hours at 77 ℃; Dried powder is packed in the graphite jig, and with 1270 ℃, the pressure hot pressed sintering of 30MPa got final product in 1.8 hours under vacuum condition.
7. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: at first by mass percentage with 45% Ti, 45% Al and 10% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.2%, adopting dry ball milling is 700 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 31 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.7 hours at 79 ℃; Dried powder is packed in the graphite jig, and with 1290 ℃, the pressure hot pressed sintering of 25MPa got final product in 1.4 hours under the argon gas condition.
8. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: at first by mass percentage with 9% Ti, 55% Al and 36% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.5%, adopting dry ball milling is 800 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 33 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.1 hours at 70 ℃; Dried powder is packed in the graphite jig, and with 1300 ℃, the pressure hot pressed sintering of 10MPa got final product in 2 hours under vacuum condition.
9. TiN/Al according to claim 1
2O
3The preparation method of matrix material is characterized in that: at first by mass percentage with 55% Ti, 40% Al and 5% TiO
2Make mixture; The sodium stearate dispersion agent that in mixture, adds mixture quality 0.3%, adopting dry ball milling is 730 rpms planetary ball mill with rotating speed, and the pellet mass ratio is 1: 10, ball milling 35 hours, make its mechanical alloying, the formation principal phase is the alloying amorphous powder of TiAl (NO); The alloying amorphous powder is following dry 4.8 hours at 71 ℃; Dried powder is packed in the graphite jig, and with 1260 ℃, the pressure hot pressed sintering of 20MPa got final product in 1.7 hours under vacuum condition.
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|---|---|---|---|
| CNB2006101048145A CN100404465C (en) | 2006-10-30 | 2006-10-30 | Method for preparing TiN/Al2O3 composite materials |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553630A (en) * | 2013-10-22 | 2014-02-05 | 湖北工业大学 | Preparation method of Ti2AlN/TiN functionally gradient material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101716680B (en) * | 2009-12-15 | 2011-05-18 | 哈尔滨工业大学 | Method for preparing Ti2AlN/TiAl compound material by regulating and controlling components accurately |
| CN102826852B (en) * | 2012-08-31 | 2016-01-13 | 中国地质大学（北京） | A kind of preparation method of titanium nitride-alumina multi-phase wear-resistant high temperature ceramic material |
| RU2524061C1 (en) * | 2013-04-04 | 2014-07-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Национальный исследовательский Томский политехнический университет" | Method of producing composite ceramic material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349950A (en) * | 2001-11-30 | 2002-05-22 | 中国科学院上海硅酸盐研究所 | Prepn of conductive composite nanometer titanium nitride-alumina material |
| CN1422827A (en) * | 2002-12-24 | 2003-06-11 | 山东大学 | Nitride/alumina based composite ceramic material and process of preparing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349950A (en) * | 2001-11-30 | 2002-05-22 | 中国科学院上海硅酸盐研究所 | Prepn of conductive composite nanometer titanium nitride-alumina material |
| CN1422827A (en) * | 2002-12-24 | 2003-06-11 | 山东大学 | Nitride/alumina based composite ceramic material and process of preparing the same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553630A (en) * | 2013-10-22 | 2014-02-05 | 湖北工业大学 | Preparation method of Ti2AlN/TiN functionally gradient material |
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