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: in present embodiment, molybdenum-wolframic acid scandium composite is made up of 35%~75% wolframic acid scandium, 1%~10% iron and 20%~60% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%.
The specific embodiment two: what present embodiment was different from the specific embodiment one is that molybdenum-wolframic acid scandium composite is made up of 40%~70% wolframic acid scandium, 3%~7% iron and 25%~55% molybdenum by quality percentage composition.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from one of specific embodiment one or two is that molybdenum-wolframic acid scandium composite is made up of 60% wolframic acid scandium, 5% iron and 35% molybdenum by quality percentage composition.Other is identical with one of specific embodiment one or two.
The specific embodiment four: what present embodiment was different from one of specific embodiment one to three is that described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.。Other is identical with one of specific embodiment one to three.
The specific embodiment five: the preparation method of present embodiment molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 35%~75% wolframic acid scandium, 1%~10% iron and 20%~60% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in dispersant, the consumption of dispersant is 1~2 times of raw material cumulative volume, obtains slurry, and described slurry is dried under vacuum condition, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be heat preservation sintering 1h~3h under 1200 ℃~1250 ℃, the pressure condition that is 30MPa~60MPa by mixed powder in temperature, obtain molybdenum-wolframic acid scandium composite.
The room temperature tensile strength of molybdenum-wolframic acid scandium composite prepared by present embodiment is 300MPa~400MPa, and 600 ℃ of tensile strength are 120MPa~160MPa, and 25 ℃~600 ℃ thermal coefficient of expansions are-1 × 10
-6k
-1~0.3 × 10
-6k
-1, elastic modelling quantity≤100GPa.
The specific embodiment six: what present embodiment was different from the specific embodiment five is that the dispersant described in step 2 is absolute ethyl alcohol.Other is identical with the specific embodiment five.
The specific embodiment seven: what present embodiment was different from the specific embodiment five or six is that ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 220rpm~400rpm, and ratio of grinding media to material is 5~8: 1, and Ball-milling Time is 20h~24h.Other is identical with the specific embodiment five or six.
The specific embodiment eight: what present embodiment was different from one of specific embodiment five to seven is that described in step 2, vacuum is not more than 1 × 10
-2pa.Other is identical with one of specific embodiment five to seven.
The specific embodiment nine: 80 ℃~90 ℃ of the temperature that what present embodiment was different from one of specific embodiment five to eight is dries described in step 2.Other is identical with one of specific embodiment five to eight.
The specific embodiment ten: what present embodiment was different from one of specific embodiment five to nine is in step 3 in temperature is heat preservation sintering 2h under 1230 ℃, the pressure condition that is 50MPa.Other is identical with one of specific embodiment five to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 60% wolframic acid scandium, 5% iron and 35% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 1 times of raw material cumulative volume, obtains slurry, and described slurry is dried under 80 ℃ of vacuum conditions, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-2pa, temperature are heat preservation sintering 3h under 1200 ℃, the pressure condition that is 30MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 400rpm, and ratio of grinding media to material is 5: 1, and Ball-milling Time is 20h.
Experiment two:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 35% wolframic acid scandium, 10% iron and 55% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 1 times of raw material cumulative volume, obtains slurry, and described slurry is dried under 80 ℃ of vacuum conditions, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-2pa, temperature are heat preservation sintering 3h under 1200 ℃, the pressure condition that is 30MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 400rpm, and ratio of grinding media to material is 5: 1, and Ball-milling Time is 20h.
Experiment three:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 75% wolframic acid scandium, 1% iron and 24% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 1 times of raw material cumulative volume, obtains slurry, and described slurry is dried under 80 ℃ of vacuum conditions, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-2pa, temperature are heat preservation sintering 3h under 1200 ℃, the pressure condition that is 30MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 400rpm, and ratio of grinding media to material is 5: 1, and Ball-milling Time is 20h.
Experiment four:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 35% wolframic acid scandium, 5% iron and 60% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 2 times of raw material cumulative volume, obtains slurry, and described slurry is dried under 90 ℃ of vacuum conditions, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-3pa, temperature are heat preservation sintering 1h under 1250 ℃, the pressure condition that is 60MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 220rpm, and ratio of grinding media to material is 8: 1, and Ball-milling Time is 24h.
Experiment five:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 70% wolframic acid scandium, 10% iron and 20% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 2 times of raw material cumulative volume, obtains slurry, and described slurry is dried under 90 ℃ of vacuum conditions, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-3pa, temperature are heat preservation sintering 1h under 1250 ℃, the pressure condition that is 60MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 220rpm, and ratio of grinding media to material is 8: 1, and Ball-milling Time is 24h.
Experiment six:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 40% wolframic acid scandium, 5% iron and 55% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 2 times of raw material cumulative volume, obtains slurry, and described slurry is dried under 90 ℃ of vacuum conditions, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-3pa, temperature are heat preservation sintering 1h under 1250 ℃, the pressure condition that is 60MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 220rpm, and ratio of grinding media to material is 8: 1, and Ball-milling Time is 24h.
Experiment seven:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 70% wolframic acid scandium, 3% iron and 27% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 1~2 times of raw material cumulative volume, obtains slurry, by the 85 ℃ of oven dry under vacuum condition of described slurry, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-2pa, temperature are heat preservation sintering 2h under 1220 ℃, the pressure condition that is 50MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 300rpm, and ratio of grinding media to material is 7: 1, and Ball-milling Time is 22h.
Experiment eight:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 68% wolframic acid scandium, 7% iron and 25% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 1~2 times of raw material cumulative volume, obtains slurry, by the 85 ℃ of oven dry under vacuum condition of described slurry, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-2pa, temperature are heat preservation sintering 2h under 1220 ℃, the pressure condition that is 50MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 300rpm, and ratio of grinding media to material is 7: 1, and Ball-milling Time is 22h.
Experiment nine:
The preparation method of molybdenum-wolframic acid scandium composite carries out according to following steps:
One, take 65% wolframic acid scandium, 6% iron and 29% molybdenum by quality percentage composition; The quality purity of described wolframic acid scandium is not less than 98%, and the quality purity of iron is not less than 99%;
Two, the raw material of step 1 is dispersed in absolute ethyl alcohol, the consumption of dispersant is 1~2 times of raw material cumulative volume, obtains slurry, by the 85 ℃ of oven dry under vacuum condition of described slurry, then the slurry ball milling after drying is ground, and obtains mixed powder;
Three, be 1 × 10 by mixed powder in vacuum
-2pa, temperature are heat preservation sintering 2h under 1220 ℃, the pressure condition that is 50MPa, obtain molybdenum-wolframic acid scandium composite.
Described wolframic acid scandium is the wolframic acid scandium powder that particle diameter is not more than 3 μ m, and iron is the iron powder that particle diameter is not more than 10 μ m, and molybdenum is the molybdenum powder that particle diameter is not more than 3 μ m.
Ball milling described in step 2 adopts planetary ball mill, and planetary ball mill rotating speed is 300rpm, and ratio of grinding media to material is 7: 1, and Ball-milling Time is 22h.
The performance test results of molybdenum-wolframic acid scandium composite prepared by experiment one to experiment nine is in table 1.
Cut into tensile sample and the Φ 3mm × 20mm thermal coefficient of expansion sample that gauge length is 40mm to testing one to experiment molybdenum-wolframic acid scandium composite of nine, and specimen surface is carried out to polishing, then the sample after polishing is carried out to mechanical property and thermal coefficient of expansion test, its test result sees the following form:
Table 1 is tested the performance test results of a molybdenum-wolframic acid scandium composite to experiment nine