CN102373358A - Preparation method of TiC dispersion-strengthened molybdenum alloy - Google Patents
Preparation method of TiC dispersion-strengthened molybdenum alloy Download PDFInfo
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- CN102373358A CN102373358A CN201010251588XA CN201010251588A CN102373358A CN 102373358 A CN102373358 A CN 102373358A CN 201010251588X A CN201010251588X A CN 201010251588XA CN 201010251588 A CN201010251588 A CN 201010251588A CN 102373358 A CN102373358 A CN 102373358A
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Abstract
The invention discloses a preparation method of a TiC dispersion-strengthened molybdenum alloy. The preparation method comprises the following steps that 1, TiO2 is utilized as a Ti carrier in a molybdenum matrix; and excessive C and TiO2 undergo a reduction reaction to produce TiC; 2, the obtained TiC is fully dissolved in the molybdenum matrix to form Ti atoms and C atoms; 3, the Ti atoms and the C atoms are diffused in the molybdenum matrix through an atom concentration gradient so that the Ti atoms and the C atoms are uniformly distributed in the molybdenum matrix; 4, the solution obtained by the step 2 is cooled so that solubility of the Ti atoms and the C atoms in the molybdenum matrix is reduced with cooling; and the Ti atoms and the C atoms are re-separated out from the molybdenum matrix and re-react with each other to produce fine TiC phases so thay good dispersion strengthening effects; and 5, the TiC powder and the molybdenum powder obtained by the step 4 are subjected to compression, sintering, extrusion and stretching to form the desired TiC dispersion-strengthened molybdenum alloy. A sample rod obtained by the preparation method has high tensile strength and high elongation.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of preparation method of TiC dispersion-strengthened molybdenum alloy.
Background technology
Molybdenum powder has excellent hot strength, and high thermal conductivity and low thermal coefficient of expansion are widely used in electronics, aviation and heating field.Pure molybdenum is because the shortcoming of high temperature oxidation and low temperature brittleness has limited the further expansion of its use range; On the other hand, along with the scientific-technical progress in fields such as inventionthe semiconductor industry, military affairs, to the molybdenum performance of products, become to grade to propose increasingly high requirement.
The development forward of molybdenum is high to be strengthened, and high-purity chemical combination green production direction develops.Continually develop the molybdenum alloy material of different use temperature scopes and different environments for use, increased range of product, enlarged molybdenum material use range, for example TZM alloy, Mo-la alloy and TiC dispersion-strengthened molybdenum alloy (Mo-TiC) etc.
The suitable recrystallization temperature of TZM alloy be (1300-1450) ℃, and temperature surpasses 1500 ℃, because worked structure generation recrystallize causes the strength of materials sharply to descend, and the material fragility raising.Though the Mo-la alloy has very high recrystallization temperature (1500-1700) ℃, the strength of materials reduces under the high temperature.Find that after deliberation TiC dispersion-strengthened molybdenum alloy (Mo-TiC) and TZM alloy, Mo-La alloy phase ratio have higher recrystallization temperature, higher hot strength and creep-resistant property.
Traditionally, Gu the preparation method of TZM alloy, Mo-la alloy and Mo-TiC alloy all adopts solid-batch mixing or solid-liquid batch mixing to mix mode.Because the strengthening phase in the molybdenum alloy accounts for to such an extent that ratio is considerably less in molybdenum; For example the total massfraction of strengthening phase is not higher than 0.7% in the TZM alloy; The massfraction of strengthening phase is not higher than 3% in the Mo-la alloy; Cause these two kinds to mix method can't realize that all strengthening phase is evenly distributed in the molybdenum matrix, material result has weakened.And the strengthening phase of reuniting, when material deformation, be prone to cause the generation of crackle, cause material property to worsen.
The Mo-TiC alloy directly adds the TiC powder in the molybdenum powder in the past, after mixing for some time, carries out compacting sintering, is prepared into the sintering blank.Though under the high temperature, most of TiC can dissolve and get in the molybdenum matrix, has the part titanyl compound among the TiC, and TiC is in the heat-agglomerating process, the water vapour reaction generation TiO in part TiC and the atmosphere
2Perhaps other oxide compounds of Ti; And the strengthening effect of the oxide compound of Ti well below the strengthening effect of TiC and, and because TiC skewness in the molybdenum matrix, dissolution process is too very long; Can't implement in the actual production, can cause existing part TiC to dissolve.
Summary of the invention
For overcoming deficiency of the prior art, the object of the present invention is to provide a kind of preparation method of TiC dispersion-strengthened molybdenum alloy.
For solving the problems of the technologies described above, the present invention has adopted following technical scheme:
Utilize TiO at a molybdenum matrix
2As the Ti carrier, with excessive C to TiO
2Reduce, reaction generates TiC, and reaction formula is TiO
2+ 3C=TiC+2CO (gas phase).
In 1700-1800 ℃ of TR, be incubated, TiC that reaction generates is dissolved in the said molybdenum matrix with the form of Ti and C atom fully.
Be incubated for some time again, utilize the concentration gradient diffusion of atom, Ti and C atom are spread in said molybdenum matrix, reach uniform distribution.
Cooling subsequently, Ti and the C solubility with temperature in said molybdenum matrix reduces and descends, and Ti atom and C atom are separated out from said molybdenum matrix again, and reaction generates tiny TiC phase again, has realized good dispersion-strengthened effect.
In theory, reaction generates the TiC of 1mol, TiO
2With the mol ratio of C be 3: 1.In the actual compacting sintering process,, therefore react completely TiO in order to guarantee because the existence of water vapour in the atmosphere causes a C meeting scaling loss part
2With the mol ratio of C be 1: (3.0-3.2), the best is 1: (3.10-3.15).
Through the solution after the dry above-mentioned steps, until the mixture that obtains TiC powder and molybdenum powder.
Advance compacting, sintering, extruding, drawing process step then and obtained required TiC dispersion-strengthened molybdenum alloy.
Preferably, 1600 ℃ of extruding of said sintered blank warp, extrusion ratio 3.5: 1,1400 ℃ of tensile strength of the lining bar of preparation are 167MPa, unit elongation 26.7%.
Compared with prior art, the Mo-TiC alloy of the present invention's preparation, strengthening phase is evenly distributed, and particle is tiny.The present invention adopts the Mo-TiC alloy of TiC powder and the preparation of molybdenum powder hybrid mode, and the tensile strength of the lining bar of the same deformation process preparation of warp is high, good percentage elongation.Therefore utilize TiO
2Gu the performance of the Mo-TiC alloy for preparing with the mode of C reaction is compared than traditional solid-mixing method, the high-temperature behavior of material is further enhanced.
Below in conjunction with specific embodiment the present invention is described in further detail.
Embodiment
A kind of preparation method of TiC dispersion-strengthened molybdenum alloy is according to TiO
2Dispose powdered alloy with 1: 3.1 mol ratio of carbon black:
Experimental procedure 1) takes by weighing the 10Kg molybdenum powder, molybdenum powder granularity 2.8um, 66.7g nano-TiO
2(granularity is less than 25nm), the 31g carbon black.
Experimental procedure 2) with TiO
2Pour in the flask with carbon black, add the 1000ml absolute ethyl alcohol, stir 10min, form an absolute ethyl alcohol suspension-s.
Experimental procedure 3) said molybdenum powder is poured in the mixing tank, said absolute ethyl alcohol suspension-s page or leaf is added in the said mixing tank, mix 4-6h.
Experimental procedure 4) solution that mixes is placed in the hopper of stainless steel making, and seasoning 30-60min makes the ethanol volatilization in the mixed solution clean, obtains a powdered alloy.
Experimental procedure 5) said powdered alloy is through the compacting of static pressure such as 200MPa, and in intermediate frequency sintering oven sintering, at 1800 ℃ of insulation 10h, furnace cooling obtains a sintered blank.
Experimental procedure 6) said sintered blank is behind 1600 ℃ of insulation 1h, is to push at 3.5: 1 with extrusion ratio, obtains an extruded bar stock.
Experimental procedure 7) said extruded bar stock is subsequently 1250 ℃ of insulation 30min, annealing then.
Experimental procedure 8) the annealing bar is heated to 1400 ℃ on the high temperature tension test machine, and insulation 15min stretches then, obtains TiC dispersion-strengthened molybdenum alloy material, and the tensile strength of said TiC dispersion-strengthened molybdenum alloy material is 167MPa, unit elongation 26.7%.
The foregoing description just is to let the one of ordinary skilled in the art can understand content of the present invention and enforcement according to this in order technical conceive of the present invention and characteristics to be described, to be its objective is, can not limit protection scope of the present invention with this.The variation or the modification of every equivalence that the essence of content has been done according to the present invention all should be encompassed in protection scope of the present invention.
Claims (10)
1. the preparation method of a TiC dispersion-strengthened molybdenum alloy may further comprise the steps:
Step 1) waits the mixture of a TiC powder and molybdenum powder for the static pressure compacting;
Step 2) with the mixture after the above-mentioned static pressure compacting, carry out sintering, heat tracing is after for some time, and cooling obtains a sintered blank;
Step 3) with said sintered blank heat tracing for some time after, push, obtain an extruded bar stock;
Step 4) with said extruded bar stock heat tracing for some time after, annealing;
The extruded bar stock of step 5) after with above-mentioned steps stretches after insulation for some time in Heating temperature on the high temperature tension test machine, obtains required TiC dispersion-strengthened molybdenum alloy;
It is characterized in that,
In powder of TiC described in the step 1 and molybdenum powder, be to get through the following steps preparation:
Step 101) in a molybdenum matrix, utilizes TiO
2As the Ti carrier with C to TiO
2Carry out reduction reaction and generate TiC, its reaction formula is TiO
2+ 3C=TiC+2CO;
Step 102) reacted solution is heated, TiC that reaction generates is dissolved in the said molybdenum matrix with the form of Ti and C atom fully;
Step 103) is incubated for some time again, utilizes the concentration gradient diffusion of atom, said Ti and C atom are spread in said molybdenum matrix, reach uniform distribution;
Step 104) cooling subsequently, said Ti and the C atom solubility with temperature in said molybdenum matrix reduces and descends, and said Ti atom and C atom are separated out from the molybdenum matrix again, and reaction generates tiny TiC phase again;
Step 105) solution after the dry above-mentioned steps is until the mixture that obtains described TiC powder and molybdenum powder.
2. the preparation method of TiC dispersion-strengthened molybdenum alloy according to claim 1 is characterized in that, in said step 1, the said pressure that waits static pressure to suppress is 200MPa.
3. the preparation method of TiC dispersion-strengthened molybdenum alloy according to claim 1 is characterized in that, in said step 2, said agglomerating temperature is 1800 ℃, and soaking time is 10h.
4. the preparation method of TiC dispersion-strengthened molybdenum alloy according to claim 1 is characterized in that, in said step 3, the Heating temperature of said sintered blank is 1600 ℃, and soaking time is 1h, and extrusion ratio is 3.5: 1.
5. the preparation method of TiC dispersion-strengthened molybdenum alloy according to claim 1 is characterized in that, in said step 4, the Heating temperature of said extruded bar stock is 1250 ℃, and soaking time is 30min.
6. the preparation method of TiC dispersion-strengthened molybdenum alloy according to claim 1 is characterized in that, in said step 5, said draft temperature is 1400 ℃, and soaking time is 15min.
7. according to the preparation method of any described TiC dispersion-strengthened molybdenum alloy in the claim 1 to 6, it is characterized in that, in step 101, said TiO
2With the mol ratio of the add-on of C be 1: (3-3.2).
8. according to the preparation method of any described TiC dispersion-strengthened molybdenum alloy in the claim 1 to 6, it is characterized in that, in step 101, said TiO
2With the mol ratio of the add-on of C be 1: (3.1-3.15).
9. the preparation method of TiC dispersion-strengthened molybdenum alloy according to claim 7 is characterized in that, in step 101, said C is a carbon black.
10. the preparation method of TiC dispersion-strengthened molybdenum alloy according to claim 8 is characterized in that, in step 101, said C is a carbon black.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103386487A (en) * | 2013-08-16 | 2013-11-13 | 苏州艾默特材料技术有限公司 | Preparation method for carbide-enhanced molybdenum alloy |
| CN103421969A (en) * | 2013-09-06 | 2013-12-04 | 金堆城钼业股份有限公司 | Preparation method of molybdenum alloys for isothermal forging die |
| CN104651696A (en) * | 2015-03-13 | 2015-05-27 | 潍坊学院 | TiC dispersion-strengthened molybdenum alloy and preparation method thereof |
| CN112281041A (en) * | 2020-10-16 | 2021-01-29 | 内蒙金属材料研究所 | Lutetium oxide particle reinforced molybdenum-based composite material and preparation method thereof |
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|---|---|---|---|---|
| US5194237A (en) * | 1990-04-23 | 1993-03-16 | National Research Council Of Canada | TiC based materials and process for producing same |
| CN1348919A (en) * | 2001-11-29 | 2002-05-15 | 华南理工大学 | Microwave synthesis process for nanometer level titaniuym carbide |
| CN1962910A (en) * | 2006-12-08 | 2007-05-16 | 金堆城钼业集团有限公司 | Method for preparing reinforced molybdenum alloy |
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2010
- 2010-08-12 CN CN 201010251588 patent/CN102373358B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5194237A (en) * | 1990-04-23 | 1993-03-16 | National Research Council Of Canada | TiC based materials and process for producing same |
| CN1348919A (en) * | 2001-11-29 | 2002-05-15 | 华南理工大学 | Microwave synthesis process for nanometer level titaniuym carbide |
| CN1962910A (en) * | 2006-12-08 | 2007-05-16 | 金堆城钼业集团有限公司 | Method for preparing reinforced molybdenum alloy |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103386487A (en) * | 2013-08-16 | 2013-11-13 | 苏州艾默特材料技术有限公司 | Preparation method for carbide-enhanced molybdenum alloy |
| CN103386487B (en) * | 2013-08-16 | 2016-07-06 | 苏州艾默特材料技术有限公司 | A kind of preparation method of carbide reinforced molybdenum alloy |
| CN103421969A (en) * | 2013-09-06 | 2013-12-04 | 金堆城钼业股份有限公司 | Preparation method of molybdenum alloys for isothermal forging die |
| CN104651696A (en) * | 2015-03-13 | 2015-05-27 | 潍坊学院 | TiC dispersion-strengthened molybdenum alloy and preparation method thereof |
| CN112281041A (en) * | 2020-10-16 | 2021-01-29 | 内蒙金属材料研究所 | Lutetium oxide particle reinforced molybdenum-based composite material and preparation method thereof |
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