CN101723670B - Ti(CxN1-x)/Al2O3 composite material and preparation method thereof - Google Patents

Ti(CxN1-x)/Al2O3 composite material and preparation method thereof Download PDF

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CN101723670B
CN101723670B CN 200910219302 CN200910219302A CN101723670B CN 101723670 B CN101723670 B CN 101723670B CN 200910219302 CN200910219302 CN 200910219302 CN 200910219302 A CN200910219302 A CN 200910219302A CN 101723670 B CN101723670 B CN 101723670B
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ball milling
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CN101723670A (en
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朱建锋
林营
王芬
杨海波
马晓伟
齐国权
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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(CxN1-x)/Al2O3 composite material and a preparation method thereof. The preparation method comprises: fully mixing Al powder accounting for 28.14 to 31.05 percent of the total weight of the composite, C powder accounting for 0 to 9.39 percent of the total weight of the composite and TiO2 accounting for 62.47 to 68.95 percent of the total weight of the composite; adding a sodium stearate dispersant accounting for 0.5 to 1 percent of the total mass into the mixture to pre-synthesize Ti(CxN1-x)/Al2O3/TiAlON composite powder by high-power ball milling process in an atmosphere of nitrogen; and generating the Ti(CxN1-x)/Al2O3 composite material in situ at a low temperature by a hot pressed sintering process under a vacuum or argon atmosphere condition. The method reduces the preparation temperature of the material, improves the performance of the material and greatly reduces the manufacturing cost of the material.

Description

A kind of Ti (C xN 1-x)/Al 2O 3Matrix material and preparation method thereof
Technical field
The invention belongs to material science, particularly a kind of Ti (C xN 1-x)/Al 2O 3Matrix material and preparation method thereof.
Background technology
TiC/Al 2O 3And TiN/Al 2O 3Matrix material is widely used because it has excellent mechanical property, is regarded as especially for a long time good cutter preferred material always.Along with the development of science and technology, the performance of material is also required more and more higher, compare Ti (C with the TiN material with traditional TiC xN 1-x) have higher mechanical property and less frictional coefficient, therefore, its research in cutter material is used and is more and more paid attention to.At present, the basic skills of synthetic this material is with TiC, TiN and Al 2O 3Carry out hot isostatic pressing or hot pressed sintering after mixing, form Ti (C by High temperature diffusion xN 1-x)/Al 2O 3Matrix material.Because the method needs temperature high, pressure is large, so production cost is higher, simultaneously, because primary particle is thicker, makes the Ti (C of formation xN 1-x)/Al 2O 3Matrix material crystal grain is also thicker, and its mechanical property is limited by very large, thereby has limited the application of this material.
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 (C xN 1-x)/Al 2O 3Matrix material and preparation method thereof utilizes Al-C-TiO 2Be raw material, under nitrogen protection through high-energy-milling pre-synthesis Ti (C xN 1-x), Al 2O 3With the TiAlON composite granule, by hot-pressing sintering technique under vacuum or the argon shield condition, original position generates Ti (C under lower temperature afterwards xN 1-x)/Al 2O 3Matrix material has not only reduced the material preparation temperature, has improved the performance of material, also so that the manufacturing cost decrease of this material.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of Ti (C xN 1-x)/Al 2O 3Matrix material, its raw material weight moiety is: 28.14-31.05%, C powder that the Al powder accounts for gross weight account for 0-9.39% and TiO 2Account for 62.47-68.95%.
Above feed composition designs by following reaction equation:
8Al+6xC+6TiO 2+3(1-x)N 2→6Ti(C xN 1-x)+4Al 2O 3 (1)
Just can synthesize different content Ti (C by changing the x value xN 1-x) Al 2O 3Matrix material, x=0-1.
A kind of Ti (C xN 1-x)/Al 2O 3The preparation method of ceramic composite may further comprise the steps:
One, at first by mass percentage with 28.14-31.05%100-200 purpose Al powder, 0-9.39%1200 purpose C powder and 62.47-68.95%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 0.5-1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 700-800 rpm, and the pellet mass ratio is 1: 10, and ball milling 12-24 hour, forming principal crystalline phase was Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 at 50-80 ℃ of lower vacuum-drying 4-5 hour;
Four, dried powder is packed in the graphite grinding tool, with 1300-1400 ℃, the pressure hot pressed sintering of 10-35MPa can obtain Ti (C in 1-2 hour under argon gas or vacuum condition xN 1-x)/Al 2O 3Matrix material.
The present invention utilizes Al powder, C powder, TiO 2And a small amount of additive reaches hot pressed sintering, reaction in－situ generation super-refinement Ti (C behind high-energy ball milling xN 1-x)/Al 2O 3Matrix material, because this material firing temperature is low, even structure, tiny, fine and close, cost is lower, has widened this composite manufacture method and range of application.
Description of drawings
Fig. 1 is the material phase analysis result of embodiment one Process During High Energy Ball Milling.
Fig. 2 is the material phase analysis result of one 1300 ℃ of sintered specimens of embodiment.
Embodiment
Embodiment one
A kind of Ti (C xN 1-x)/Al 2O 3Matrix material, its raw material weight moiety is: 29.52%, the 1200 order C powder that 120 order Al powder account for gross weight account for 4.93% and 325 order TiO 2Account for 65.55%.
The preparation method of the present embodiment may further comprise the steps:
One, at first by mass percentage with 29.52% 120 order Al powder, 4.93%1200 purpose C powder and 65.55%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 750 rpms, and the pellet mass ratio is 1: 10, ball milling 20 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 75 ℃ of lower vacuum-dryings 5 hours;
Four, dried powder is packed in the graphite grinding tool, with 1300 ℃, the pressure hot pressed sintering of 25MPa can obtain Ti (C in 1.5 hours under the argon gas condition xN 1-x)/Al 2O 3Matrix material.
Ti (the C that the present embodiment is prepared 0.5N 0.5)/Al 2O 3Matrix material, wherein Ti (C 0.5N 0.5) account for 92.85% of gross weight, Al 2O 3Account for mutually product total mass 7.15%.Phase behind this material high-energy ball milling and the hot pressed sintering forms as depicted in figs. 1 and 2, and Fig. 1 is the material phase analysis of powder before and after the high-energy ball milling, can find out, before the ball milling mainly by Al powder TiO 2Form, because the C powder is oil coke non-crystalline state, can't see its diffraction peak; Principal crystalline phase is (N behind the ball milling 0.5C 0.5), Al 2O 3And TiAlNO; Fig. 2 is the material phase analysis result of 1300 ℃ of sintered specimens, and as seen from the figure, this material is by (N 0.5C 0.5) and Al 2O 3Form, without any impurity.
Embodiment two
A kind of Ti (C xN 1-x)/Al 2O 3Matrix material, its raw material weight moiety is: 100 order Al powder account for 31.05% and 325 order TiO of gross weight 2Account for 68.95%.
The preparation method of the present embodiment may further comprise the steps:
One, at first by mass percentage with 31.05%100 purpose Al powder and 68.95%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 800 rpms, and the pellet mass ratio is 1: 10, ball milling 24 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 80 ℃ of lower vacuum-dryings 4 hours;
Four, dried powder is packed in the graphite grinding tool, with 1350 ℃, the pressure hot pressed sintering of 20MPa can obtain Ti (C in 1 hour under vacuum condition xN 1-x)/Al 2O 3Matrix material.
The TiN/Al that the present embodiment is prepared 2O 3Matrix material, wherein TiN accounts for 93.32% of gross weight, Al 2O 3Account for mutually product total mass 6.68%.
Embodiment three
A kind of Ti (C xN 1-x)/Al 2O 3Matrix material, its raw material weight moiety is: 30.11%, the 1200 order C powder that 150 order Al powder account for gross weight account for 3.02% and 325 order TiO 2Account for 66.87%.
The preparation method of the present embodiment may further comprise the steps:
One, at first by mass percentage with 30.12%150 purpose Al powder, 3.02%1200 purpose C powder and 66.87%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 0.6% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 780 rpms, and the pellet mass ratio is 1: 10, ball milling 18 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 80 ℃ of lower vacuum-dryings 4 hours;
Four, dried powder is packed in the graphite grinding tool, with 1320 ℃, the pressure hot pressed sintering of 15MPa can obtain Ti (C in 1.8 hours under vacuum condition xN 1-x)/Al 2O 3Matrix material.
Ti (the C that the present embodiment is prepared 0.3N 0.7)/Al 2O 3Matrix material, wherein Ti (C 0.3N 0.7) account for 93.05% of gross weight, Al 2O 3Account for mutually product total mass 6.95%.
Embodiment four
A kind of Ti (C xN 1-x)/Al 2O 3Matrix material, its raw material weight moiety is: 28.95%, the 1200 order C powder that 180 order Al powder account for gross weight account for 6.77% and 325 order TiO 2Account for 64.28%.
The preparation method of the present embodiment may further comprise the steps:
One, at first by mass percentage with 28.95%180 purpose Al powder, 6.77%1200 purpose C powder and 64.28%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 0.5% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 800 rpms, and the pellet mass ratio is 1: 10, ball milling 15 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 80 ℃ of lower vacuum-dryings 4.5 hours;
Four, dried powder is packed in the graphite grinding tool, with 1120 ℃, the pressure hot pressed sintering of 20MPa can obtain Ti (C in 1.8 hours under vacuum condition xN 1-x)/Al 2O 3Matrix material.
Ti (the C that the present embodiment is prepared 0.7N 0.3)/Al 2O 3Matrix material, wherein Ti (C 0.7N 0.3) account for 92.64% of gross weight, Al 2O 3Account for mutually product total mass 7.36%.
Embodiment five
A kind of Ti (C xN 1-x)/Al 2O 3Matrix material, its raw material weight moiety is: 28.14%, the 1200 order C powder that 200 order Al powder account for gross weight account for 9.39% and 325 order TiO 2Account for 62.47%.
The preparation method of the present embodiment may further comprise the steps:
One, at first by mass percentage with 28.14%200 purpose Al powder, 9.39%1200 purpose C powder and 62.47%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 800 rpms, and the pellet mass ratio is 1: 10, ball milling 12 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 70 ℃ of lower vacuum-dryings 5 hours;
Four, dried powder is packed in the graphite grinding tool, with 1300 ℃, the pressure hot pressed sintering of 25MPa can obtain Ti (C in 2 hours under the argon gas condition xN 1-x)/Al 2O 3Matrix material.
The TiC/Al that the present embodiment is prepared 2O 3Compound composite material, wherein TiC accounts for 92.30% of gross weight, Al 2O 3Account for mutually product total mass 7.7%.

Claims (5)

1. Ti (C xN 1-x)/Al 2O 3The composite manufacture method is characterized in that, may further comprise the steps: one, at first by mass percentage with 28.14-31.05%100-200 purpose Al powder, 0-9.39%1200 purpose C powder and 62.47-68.95%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 0.5-1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 700-800 rpm, and the pellet mass ratio is 1:10, and ball milling 12-24 hour, forming principal crystalline phase was Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 at 50-80 ℃ of lower vacuum-drying 4-5 hour;
Four, dried powder is packed in the graphite grinding tool, with 1300-1400 ℃, the pressure hot pressed sintering of 10-35MPa can obtain Ti (C in 1-2 hour under argon gas or vacuum condition xN 1-x)/Al 2O 3Matrix material.
2. preparation method according to claim 1 is characterized in that, may further comprise the steps: one, at first by mass percentage with 29.52% 120 order Al powder, 4.93%1200 purpose C powder and 65.55%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 750 rpms, and the pellet mass ratio is 1:10, ball milling 20 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 75 ℃ of lower vacuum-dryings 5 hours;
Four, dried powder is packed in the graphite grinding tool, with 1300 ℃, the pressure hot pressed sintering of 25MPa can obtain Ti (C in 1.5 hours under the argon gas condition xN 1-x)/Al 2O 3Matrix material.
3. preparation method according to claim 1 is characterized in that, may further comprise the steps: one, at first by mass percentage with 31.05%100 purpose Al powder and 68.95%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 800 rpms, and the pellet mass ratio is 1:10, ball milling 24 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 80 ℃ of lower vacuum-dryings 4 hours;
Four, dried powder is packed in the graphite grinding tool, with 1350 ℃, the pressure hot pressed sintering of 20MPa can obtain Ti (C in 1 hour under vacuum condition xN 1-x)/Al 2O 3Matrix material.
4. preparation method according to claim 1 is characterized in that, may further comprise the steps: one, at first by mass percentage with 30.12%150 purpose Al powder, 3.02%1200 purpose C powder and 66.87%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 0.6% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 780 rpms, and the pellet mass ratio is 1:10, ball milling 18 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 80 ℃ of lower vacuum-dryings 4 hours;
Four, dried powder is packed in the graphite grinding tool, with 1320 ℃, the pressure hot pressed sintering of 15MPa can obtain Ti (C in 1.8 hours under vacuum condition xN 1-x)/Al 2O 3Matrix material.
5. preparation method according to claim 1 is characterized in that, may further comprise the steps: one, at first by mass percentage with 28.14%200 purpose Al powder, 9.39%1200 purpose C powder and 62.47%325 purpose TiO 2Fully mix;
Two, add the sodium stearate dispersion agent of mixture quality 1% in mixture, carry out high-energy ball milling under nitrogen protection, the rotating speed of ball mill is 800 rpms, and the pellet mass ratio is 1:10, ball milling 12 hours, and forming principal crystalline phase is Ti (C xN 1-x), Al 2O 3With the tiny composite granule of TiAlON;
Three, with the powder behind the ball milling in the step 2 70 ℃ of lower vacuum-dryings 5 hours;
Four, dried powder is packed in the graphite grinding tool, with 1300 ℃, the pressure hot pressed sintering of 25MPa can obtain Ti (C in 2 hours under the argon gas condition xN 1-x)/Al 2O 3Matrix material.
CN 200910219302 2009-12-03 2009-12-03 Ti(CxN1-x)/Al2O3 composite material and preparation method thereof Active CN101723670B (en)

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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
CN103787407B (en) * 2013-12-25 2016-04-20 河北科技大学 Reaction ball milling legal system is for nano TiC N/Al 2o 3the method of composite powder
CN105132728B (en) * 2015-07-16 2017-08-29 攀枝花学院 The preparation method and applications of black ceramic composite
CN105002389B (en) * 2015-07-22 2017-05-24 内蒙古工业大学 Al-TiO2-C grain refiner, preparation method thereof and commercial-purity aluminum refining method
CN108546098A (en) * 2018-07-10 2018-09-18 武汉科技大学 A kind of in-situ carbon TiN phase toughened aluminum oxide base complex phase ceramic and preparation method thereof

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