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.
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%.