CN104087772A - Powder metallurgy method for preparing high-density titanium and titanium alloy - Google Patents
Powder metallurgy method for preparing high-density titanium and titanium alloy Download PDFInfo
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- CN104087772A CN104087772A CN201410313474.1A CN201410313474A CN104087772A CN 104087772 A CN104087772 A CN 104087772A CN 201410313474 A CN201410313474 A CN 201410313474A CN 104087772 A CN104087772 A CN 104087772A
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Abstract
The invention discloses a powder metallurgy method for preparing high-density titanium and titanium alloy products. The method comprises the following steps: preparing raw materials and mixing; performing pressure forming; performing atmosphere purifying; performing atmosphere-vacuum sintering. According to the method, titanium powder or titanium alloy mixed powder is adopted as the raw material and is subjected to pressure forming and atmosphere-vacuum sintering in sequence; the atmosphere sintering is adopted at the temperature of 400-600 DEG C, mixed gas of hydrogen and argon is introduced, and heat is preserved for 2-3 hours, thus generating TiHx (x is more than 0 and not more than 2); the vacuum sintering is adopted at the temperature of 600-1350 DEG C, and heat is preserved at 1200-1350 DEG C for 4-6 hours; by virtue of the diffusion analysis effect and the interstitial solid solution of hydrogen, the vacancy concentration and dislocation in titanium are increased, the surface activity of titanium is improved, and the sintering free energy effect is reduced, thus obtaining dense titanium and titanium alloy. The titanium/ titanium alloy products prepared by adopting the method are high in density, the process route is short, a subsequent pressure processing process can be reduced or shortened, and the processing cost is lowered. The problems of high cost and low density of a conventional powder metallurgy method for preparing titanium and titanium alloy are solved.
Description
Technical field
The invention belongs to the processing technique field of titanium or titanium alloy goods, be specifically related to a kind of method that adopts powder metallurgical technique to prepare titanium or titanium alloy goods.
Background technology
Metal titanium and alloy thereof have that density is low, specific tenacity is high, solidity to corrosion is good, thermotolerance is high, without advantages such as magnetic, good welding performance, be widely used in the fields such as aerospace, automobile, chemical industry, electric power, wrist-watch, medical treatment, but because conventional melting and casting method operational path is long, the utilization ratio of material is low, and titanium machinability is poor, preparation cost is high, therefore the application of titanium or titanium alloy is restricted.Powder metallurgy becomes the novel process of a kind of applicable feasibility of producing titanium or titanium alloy; it is raw material that traditional powder metallurgy process be take the metal-powder of titanium valve and alloy; the density of titanium or titanium alloy prepared by employing vacuum sintering or inert atmosphere protection only can reach 95% left and right; cause the titanium or titanium alloy Mechanical Properties of Products of preparation poor; generally need follow-up hip treatment can improve material sintered density; thereby raising material property, has increased production cost.Therefore, develop a kind of method of the titanium or titanium alloy of preparing high-compactness particularly important.
Summary of the invention
Of the present inventionly be to provide a kind of powder metallurgy process of preparing high-compactness titanium or titanium alloy goods.
The realization of object of the present invention comprises the following steps: the mixed powder of batching, compression moulding, atmosphere purification, atmosphere-vacuum sintering, be specially:
(1) the mixed powder of batching: according to the titanium or titanium alloy component proportions of drawing up standby, titanium valve and other interpolation alloying element powders are mixed powder under argon gas atmosphere protection;
(2) compression moulding: pack the good powder of mixed preparing into mould and be pressed into needed article shape, compacting can adopt isostatic cool pressing or mold pressing compacting;
(3) atmosphere purification: pressed compact is packed into after atmosphere sintering furnace, be evacuated to vacuum tightness in stove and be less than 10
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is more than 3 times;
(4) atmosphere-vacuum sintering: complete after furnace atmosphere purification, start atmosphere sintering, pass into hydrogen and argon gas mixed gas, passing into the interior hydrogen of stove and argon gas must be high-purity gas, be warming up to 400 ~ 600 ℃, and be incubated 2～3h at this temperature, after insulation finishes, close gas, open vacuum system, start vacuum sintering, be warming up to 1200 ~ 1350 ℃, soaking time 4 ~ 6h, finally cool to 20 ℃ of room temperatures with the furnace, in vacuum sintering and process of cooling, vacuumize, in the sintered heat insulating stage, the vacuum tightness of sintering oven is answered < 10 always
-3pa.
It is raw material that titanium valve or titanium alloy mixed powder are take in the present invention, after press forming, adopt atmosphere-vacuum sintering, wherein at 400 ~ 600 ℃ of temperature sections, adopt atmosphere sintering, pass into the mixed gas of hydrogen and argon gas, be incubated 2 ~ 3 hours, generate TiHx (0 < x≤2), 600 ~ 1350 ℃ of temperature sections adopt vacuum sintering, and 1200 ~ 1350 ℃ of insulations 4 ~ 6 hours, vacancy concentration and the dislocation utilizing the diffusion analytic function of hydrogen and gap solid solution characteristic and cause in titanium increase, increased the surfactivity of titanium, reduce the effect of sintering free energy and prepared fine and close titanium or titanium alloy.Titanium or titanium alloy product density prepared by this method technique is high, and operational path is short, can reduce or shorten packing pressure manufacturing procedure, cuts down finished cost.The present invention has overcome prior powder metallurgy and has prepared the problem that titanium or titanium alloy cost is high, density is low.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, but must not to the present invention, be limited by any way, and any change or the improvement based on training centre of the present invention, done, all belong to protection scope of the present invention.
As shown in drawings and Examples: a kind of powder metallurgy process of preparing high-compactness titanium or titanium alloy goods of the present invention, comprises the following steps: the mixed powder of batching, compression moulding, atmosphere purification, atmosphere-vacuum sintering, be specially:
(1) the mixed powder of batching: according to the titanium or titanium alloy component proportions of drawing up standby, titanium valve and other interpolation alloying element powders are mixed powder under argon gas atmosphere protection;
(2) compression moulding: pack the good powder of mixed preparing into mould and be pressed into needed article shape, compacting can adopt isostatic cool pressing or mold pressing compacting;
(3) atmosphere purification: pressed compact is packed into after atmosphere sintering furnace, be evacuated to vacuum tightness in stove and be less than 10
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is more than 3 times;
(4) atmosphere-vacuum sintering: complete after furnace atmosphere purification, start atmosphere sintering, pass into hydrogen and argon gas mixed gas, passing into the interior hydrogen of stove and argon gas must be high-purity gas, be warming up to 400 ~ 600 ℃, and be incubated 2 ~ 3h at this temperature, after insulation finishes, close gas, open vacuum system, start vacuum sintering, be warming up to 1200 ~ 1350 ℃, soaking time 4 ~ 6h, finally cool to 20 ℃ of room temperatures with the furnace, in vacuum sintering and process of cooling, vacuumize, in the sintered heat insulating stage, the vacuum tightness of sintering oven is answered < 10 always
-3pa.
Mixed gas described in step (4), purity reaches more than 99.999%, and in mixed gas, the content of hydrogen is volume ratio 13 ~ 20%.
In step (4), in atmosphere sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa.
The described titanium valve mean particle size of step (1) is≤48 μ m.
In step (1), described alloying element powder is one or more in Al60V40 powder, niobium powder, zirconium powder.
The mean particle size that other described in step (1) add alloying element powder is≤48 μ m.
Compacting pressure in step (2) is 300MPa ~ 400Mpa.
Temperature rise rate≤5 ℃ in atmosphere-vacuum sintering process/min in step (4).
Embodiment 1
The ti powder of 48 μ m is packed in mould, adopt isostatic cool pressing under 300MPa pressure, to be pressed into the article shape of design; Pressed compact is packed into and in sintering oven, carries out shove charge; Closed furnace door, is less than 10 by being evacuated to vacuum tightness in stove
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is carried out furnace atmosphere purification 3 times; Passing into purity is 99.999% above high-purity hydrogen and high-purity argon gas mixed gas, and in mixed gas, the content of hydrogen is volume ratio 20%, and the temperature rise rate with 5 ℃/min is warming up to 400 ℃ simultaneously, and is incubated 3 hours.In sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa; After insulation finishes, close gas, open vacuum system, the temperature rise rate with 5 ℃/min is warming up to 1200 ℃ simultaneously, soaking time 4 hours, and then furnace cooling, to 20 ℃ of room temperatures, had both obtained target compound metal titanium goods, by detecting its density, was 99.3%.
Embodiment 2
The ti powder of 48 μ m is packed in mould, adopt isostatic cool pressing under 300MPa pressure, to be pressed into the article shape of design; Pressed compact is packed into and in sintering oven, carries out shove charge; Closed furnace door, is less than 10 by being evacuated to vacuum tightness in stove
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is carried out furnace atmosphere purification 3 times; Passing into purity is 99.999% above high-purity hydrogen and high-purity argon gas mixed gas, and in mixed gas, the content of hydrogen is volume ratio 20%, and the temperature rise rate with 5 ℃/min is warming up to 600 ℃ simultaneously, and is incubated 1 hour.In sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa; After insulation finishes, close gas, open vacuum system, the temperature rise rate with 5 ℃/min is warming up to 1200 ℃ simultaneously, soaking time 4 hours, and then furnace cooling, to 20 ℃ of room temperatures, had both obtained target compound metal titanium goods, by detecting its density, was 99.6%.
Embodiment 3
The ti powder of 48 μ m is packed in mould, adopt isostatic cool pressing under 300MPa pressure, to be pressed into the article shape of design; Pressed compact is packed into and in sintering oven, carries out shove charge; Closed furnace door, is less than 10 by being evacuated to vacuum tightness in stove
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is carried out furnace atmosphere purification 3 times; Passing into purity is 99.999% above high-purity hydrogen and high-purity argon gas mixed gas, and in mixed gas, the content of hydrogen is volume ratio 15%, and the temperature rise rate with 5 ℃/min is warming up to 600 ℃ simultaneously, and is incubated 2 hours.In sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa; After insulation finishes, close gas, open vacuum system, the temperature rise rate with 5 ℃/min is warming up to 1200 ℃ simultaneously, soaking time 4 hours, and then furnace cooling, to 20 ℃ of room temperatures, had both obtained target compound metal titanium goods, by detecting its density, was 99.2%.
Embodiment 4
The titanium valve and the Al60V40 powder that are respectively 30 μ m are prepared burden by Ti-6Al-4V component proportions, under argon gas atmosphere protection, mix.Mixed powder is packed in mould, adopt and be embossed in the article shape that is pressed into design under 350MPa pressure; Pressed compact is packed into and in sintering oven, carries out shove charge; Closed furnace door, is less than 10 by being evacuated to vacuum tightness in stove
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is carried out furnace atmosphere purification 5 times; Passing into purity is 99.999% above high-purity hydrogen and high-purity argon gas mixed gas, and in mixed gas, the content of hydrogen is volume ratio 13%, and the temperature rise rate with 3 ℃/min is warming up to 450 ℃ simultaneously, and is incubated 2 hours.In sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa; After insulation finishes, close gas, open vacuum system, the temperature rise rate with 3 ℃/min is warming up to 1200 ℃ simultaneously, soaking time 6 hours, and then furnace cooling, to 20 ℃ of room temperatures, had both obtained target compound Ti-6Al-4V goods, by detecting its density, was 98.6%.
Embodiment 5
The titanium valve and the Al60V40 powder that are respectively 30 μ m are prepared burden by Ti-6Al-4V component proportions, under argon gas atmosphere protection, mix.Mixed powder is packed in mould, adopt and be embossed in the article shape that is pressed into design under 350MPa pressure; Pressed compact is packed into and in sintering oven, carries out shove charge; Closed furnace door, is less than 10 by being evacuated to vacuum tightness in stove
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is carried out furnace atmosphere purification 5 times; Passing into purity is 99.999% above high-purity hydrogen and high-purity argon gas mixed gas, and in mixed gas, the content of hydrogen is volume ratio 13%, and the temperature rise rate with 3 ℃/min is warming up to 450 ℃ simultaneously, and is incubated 2 hours.In sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa; After insulation finishes, close gas, open vacuum system, the temperature rise rate with 3 ℃/min is warming up to 1250 ℃ simultaneously, soaking time 4 hours, and then furnace cooling, to 20 ℃ of room temperatures, had both obtained target compound Ti-6Al-4V goods, by detecting its density, was 99.0%.
Embodiment 6
The titanium valve and niobium powder, the zirconium powder that are respectively 10 μ m are prepared burden by Ti-13Nb-13Zr component proportions, under argon gas atmosphere protection, mix.Mixed powder is packed in mould, adopt isostatic cool pressing under 400MPa pressure, to be pressed into the article shape of design; Pressed compact is packed into and in sintering oven, carries out shove charge; Closed furnace door, is less than 10 by being evacuated to vacuum tightness in stove
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is carried out furnace atmosphere purification 5 times; Passing into purity is 99.999% above high-purity hydrogen and high-purity argon gas mixed gas, and in mixed gas, the content of hydrogen is volume ratio 17%, and the temperature rise rate with 3 ℃/min is warming up to 500 ℃ simultaneously, and is incubated 1,5 hour.In sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa; After insulation finishes, close gas, open vacuum system, the temperature rise rate with 3 ℃/min is warming up to 1350 ℃ simultaneously, soaking time 5 hours, and then furnace cooling, to 20 ℃ of room temperatures, had both obtained target compound Ti-13Nb-13Zr goods, by detecting its density, was 99.2%.
Embodiment 7
The titanium valve and niobium powder, the zirconium powder that are respectively 20 μ m are prepared burden by Ti-13Nb-13Zr component proportions, under argon gas atmosphere protection, mix.Mixed powder is packed in mould, adopt isostatic cool pressing under 400MPa pressure, to be pressed into the article shape of design; Pressed compact is packed into and in sintering oven, carries out shove charge; Closed furnace door, is less than 10 by being evacuated to vacuum tightness in stove
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is carried out furnace atmosphere purification 5 times; Passing into purity is 99.999% above high-purity hydrogen and high-purity argon gas mixed gas, and in mixed gas, the content of hydrogen is volume ratio 17%, and the temperature rise rate with 3 ℃/min is warming up to 500 ℃ simultaneously, and is incubated 2 hours.In sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa; After insulation finishes, close gas, open vacuum system, the temperature rise rate with 3 ℃/min is warming up to 1350 ℃ simultaneously, soaking time 5 hours, and then furnace cooling, to 20 ℃ of room temperatures, had both obtained target compound Ti-13Nb-13Zr goods, by detecting its density, was 99.3%.
Claims (8)
1. a powder metallurgy process of preparing high-compactness titanium or titanium alloy goods, is characterized in that comprising the following steps: the mixed powder of batching, compression moulding, atmosphere purification, atmosphere-vacuum sintering, be specially:
(1) the mixed powder of batching: according to the titanium or titanium alloy component proportions of drawing up standby, titanium valve and other are added to alloying element powder, under argon gas atmosphere protection, powder is mixed;
(2) compression moulding; Pack the good powder of mixed preparing into mould and be pressed into needed article shape, compacting can adopt isostatic cool pressing or mold pressing compacting;
(3) atmosphere purification; Pressed compact is packed into after atmosphere sintering furnace, in stove, be evacuated to vacuum tightness < 10
-3pa, passes into argon gas, then vacuumizes, and repeatable operation is more than 3 times;
(4) atmosphere-vacuum sintering: complete after furnace atmosphere purification, start atmosphere sintering, pass into hydrogen and argon gas mixed gas, passing into the interior hydrogen of stove and argon gas must be high-purity gas, be warming up to 400 ~ 600 ℃, and be incubated 2 ~ 3h at this temperature, after insulation finishes, close gas, open vacuum system, start vacuum sintering, be warming up to 1200 ~ 1350 ℃, soaking time 4 ~ 6h, finally cool to 20 ℃ of room temperatures with the furnace, in vacuum sintering and process of cooling, vacuumize always, in the sintered heat insulating stage, the vacuum tightness < 10 of sintering oven
-3pa.
2. the powder metallurgy process of preparing high-compactness titanium or titanium alloy goods according to claim 1, is characterized in that the mixed gas described in step (4), and purity reaches more than 99.999%, and in mixed gas, the content of hydrogen is volume ratio 13 ~ 20%.
3. the powder metallurgy process of preparing high-compactness titanium or titanium alloy goods according to claim 1, is characterized in that in step (4), and in atmosphere sintering process, keeping furnace pressure is 1.1 * 10
5~ 1.2 * 10
5pa.
4. the powder metallurgy process of preparing high-compactness titanium or titanium alloy goods according to claim 1, is characterized in that the titanium valve mean particle size described in step (1) is for≤48 μ m.
5. the powder metallurgy process of preparing high-compactness titanium or titanium alloy goods according to claim 1, is characterized in that, in step (1), described alloying element powder is one or more in Al60V40 powder, niobium powder, zirconium powder.
6. the powder metallurgy process of preparing high-compactness titanium or titanium alloy goods according to claim 1, is characterized in that other mean particle sizes of adding alloying element powder described in step (1) are≤48 μ m.
7. the powder metallurgy process of preparing high-compactness titanium or titanium alloy goods according to claim 1, is characterized in that the compacting pressure in step (2) is 300MPa ~ 400Mpa.
8. the powder metallurgy process of preparing high-compactness titanium or titanium alloy goods according to claim 1, is characterized in that in step (4) in atmosphere-vacuum sintering process temperature rise rate≤5 ℃/min.
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