CN111283203B - Method for promoting blank densification by utilizing hydrogen absorption expansion of titanium-containing material - Google Patents
Method for promoting blank densification by utilizing hydrogen absorption expansion of titanium-containing material Download PDFInfo
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- CN111283203B CN111283203B CN201811490750.6A CN201811490750A CN111283203B CN 111283203 B CN111283203 B CN 111283203B CN 201811490750 A CN201811490750 A CN 201811490750A CN 111283203 B CN111283203 B CN 111283203B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention relates to a method for promoting blank densification by utilizing hydrogen absorption expansion of a titanium-containing material. Tightly matching a titanium-containing substance block, or a filled titanium-containing substance block with a material to be densified, or titanium-containing substance powder with the material to be densified, and then loading the material into a rigid mold to obtain a pretreatment assembly; introducing hydrogen into the pretreatment assembly to enable the titanium-containing material to absorb hydrogen; the titanium-containing substance and/or the material to be densified are/is densified by utilizing the volume expansion effect of the titanium-containing substance. The invention provides a method for preparing a high-density or fully-compact blank at medium and low temperature under hydrogen atmosphere. The method can improve the density and repair the defects, and simultaneously can refine the structure, thereby effectively improving the mechanical property of the material.
Description
Technical Field
The invention relates to a densification method of metal, alloy and metal matrix composite; in particular to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material.
Background
Titanium alloy is an important metal developed in the middle of the 20 th century, and is widely concerned by people due to the excellent properties of low density, high specific strength, good corrosion resistance, high heat resistance, no magnetism, good welding performance and the like. There are various methods for preparing titanium alloys, including cast forming, laser forming and powder metallurgy forming, but their high cost has influenced their widespread use.
During the preparation and use of titanium alloy, certain pores are often generated in the material. The liquid metal shrinks in volume during cooling and solidification, and can form loose or shrinkage cavities. The presence of residual porosity in sintered compacts of powder metallurgy titanium alloys is inevitable. During hot isostatic pressing, if the powder contains hollow powder, or gases that leak during canning, are compressed during densification, these gases are insoluble in the alloy and will expand into thermally induced pores during the subsequent heat treatment process. The titanium alloy material manufactured by the additive has tiny pores due to the influence of raw materials and processes. In the process of welding titanium alloy, excessive gas or gas generated by metallurgical reaction is absorbed by a welding pool at high temperature, and the gas is not allowed to escape in time before cooling and solidification and remains in weld metal to form micropores or bubbles. In addition, interfacial reactions may also lead to void generation during the preparation of metal composites. These pores are often the main defects of the alloy material and become the fracture sources of the alloy
The porosity is one of the main defects influencing the performance of the titanium alloy product, directly influences the mechanical property of the titanium alloy product and leads to material failure. By adopting a hot isostatic pressing technology, hot pressing sintering, discharge plasma sintering or hot processing treatment, the internal pores of the titanium alloy part can be effectively eliminated. But these processes are expensive.
Disclosure of Invention
Aiming at the defects of the prior art, the invention firstly provides a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; tightly matching a titanium-containing substance block, or a filled titanium-containing substance block with a material to be densified, or titanium-containing substance powder with the material to be densified, and loading the material into a rigid mold to obtain a pretreatment assembly, and introducing hydrogen into the pretreatment assembly to enable the titanium-containing substance to absorb hydrogen; the titanium-containing material and/or the material to be densified are/is densified by utilizing the volume expansion effect of the titanium-containing material;
the hydrogen absorption process is controlled as follows: firstly, heating a pretreatment component C to a temperature of H1 in an inert atmosphere or vacuum, then introducing hydrogen, preserving heat, then cooling to a temperature of H2, and preserving heat, wherein the value range of H1 is 600-;
or
The hydrogen absorption process is controlled as follows: firstly, heating a pretreatment component C to a temperature H3 in an inert atmosphere or vacuum, then introducing hydrogen, preserving heat, continuously heating to H1, and continuously introducing hydrogen; preserving heat; then, cooling to a temperature H2, continuously introducing hydrogen, and preserving heat, wherein the value range of H1 is 600-1000 ℃; the H3 is less than H1;
the titanium-containing material contains metallic titanium. The titaniferous material is preferably a titaniferous metal. The pretreatment component C is a sample with a mold.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the blank is a metal blank or a composite material blank. Preferably a metal blank. Still more preferably a titanium-containing metal body.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the method comprises the following steps:
step one
Placing the pre-compact blank A into a mold; packaging, fastening and reserving an air vent; obtaining a pretreatment component C, wherein the pre-compact blank A contains a titanium-containing substance with hydrogen absorption capacity; the titaniferous material has a hydrogen-absorbing expansion effect;
or
Putting the pre-compact blank B and the titanium-containing material block into a die together; packaging, fastening and reserving an air vent; obtaining a pretreatment component C; the titaniferous material has a hydrogen-absorbing expansion effect;
or
Putting the pre-compact blank B and the powder of the titanium-containing substance into a die together; packaging, fastening and reserving an air vent; obtaining a pretreatment component C; the titaniferous material has a hydrogen-absorbing expansion effect;
or
Filling titanium-containing material powder into the inner cavity of the mold, and packaging, fastening and reserving an air vent; obtaining a pretreatment component C; the titaniferous material has a hydrogen-absorbing expansion effect;
or
Placing powder to be densified at a set position in the inner cavity of the mold; placing titanium-containing material powder at other positions of the inner cavity of the die; packaging, fastening and reserving an air vent; obtaining a pretreatment assembly; the titaniferous material has a hydrogen-absorbing expansion effect;
the mould is a rigid mould; in the pretreatment component C, the outer wall of the pre-compact blank A is in contact with the inner wall of the mold or a gap is reserved between the outer wall of the pre-compact blank A and the inner wall of the mold; the gap is smaller than the linear expansion of the pre-compact blank A after hydrogen absorption;
step two
Placing the pretreatment assembly obtained in the step one in a sintering furnace, heating to a temperature of H1 in an inert atmosphere or vacuum, introducing hydrogen, preserving heat, cooling to a temperature of H2, and preserving heat, wherein the value range of H1 is 600-1000 ℃;
or
Placing the pretreatment assembly obtained in the step one in a sintering furnace, firstly heating to the temperature of H3 in an inert atmosphere or vacuum, then introducing hydrogen, preserving heat, then continuously heating to H1, and continuously introducing hydrogen; preserving heat; then, cooling to a temperature H2, continuously introducing hydrogen, and preserving heat, wherein the value range of H1 is 600-1000 ℃; the H3 is less than H1;
after hydrogen absorption is finished, hydrogen is released in a vacuum atmosphere; obtaining a sample after hydrogen desorption;
step three
And removing the mold on the sample after hydrogen discharge to obtain a densified metal blank.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; all parts of the packaged die are kept fastened and cannot loosen in the heating and hydrogen absorption processes.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the material of the mould does not react with hydrogen.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the titanium-containing metal powder has a particle size of 5 to 1000 microns.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the relative compactness of pre-densified blank A and/or pre-densified blank B is less than or equal to 98%. In industrial applications, it may be a metal block or a composite block (including a titanium alloy block) having pores therein; or a metal product or composite material block (including a composite of a titanium alloy product and another metal material) in which defects such as cracks exist in the block and cracks and pores exist inside the block.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of titanium-containing metal; the holding time of H1 is less than or equal to 20 hours, preferably 0.5 to 20 hours;
after the temperature is kept at H1, the temperature is reduced to H2 at the cooling speed of 0.1-5 ℃/min; the holding time in H2 is 20 hours or less, preferably 0.5 to 20 hours.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the inert atmosphere is argon atmosphere or vacuum; the rate of cooling from H1 to H2 is 0.1-2 ℃/min, and the range of H1 is 800-; the range of H2 is 600-800 ℃; the H2 is less than H1.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; after the hydrogen absorption is finished, the heat preservation vacuum annealing is carried out at the dehydrogenation temperature D, the dehydrogenation temperature D ranges from 600 ℃ to 900 ℃, and the vacuum degree of the vacuum annealing is lower than 10-3Pa。
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; and repeating the second step until a product with set density is obtained.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; and sequentially repeating the first step, the second step and the third step until a product with set density is obtained.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the material of the mold is preferably: at least one of heat-resistant steel, high-temperature-resistant stainless steel, high-temperature alloy and high-temperature ceramic.
In industrial application, the hydrogen absorption temperature is less than or equal to 0.7 times of the melting point of the pre-compact metal blank. The best selection is as follows: the maximum amount of hydrogen absorption is achieved as much as possible.
In industrial applications, the dehydrogenation temperature is less than the melting point of the pre-densified metal blank. Preferably 0.7 times or less the melting point of the pre-densified metal blank.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; after the titanium-containing substance absorbs hydrogen, the absorbed hydrogen can be completely removed by heating and raising the temperature or reducing the hydrogen partial pressure.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; and (4) replacing the hydrogen-absorbable metal powder with larger volume expansion after hydrogen absorption, taking the product obtained in the step four as a processing object, and sequentially repeating the step one, the step two and the step three until a product with set density is obtained. The product with set density comprises a finished product with the density of more than or equal to 99.5 percent.
The invention relates to a method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; in industrial applications, the article may be, but is not limited to: non-fully dense sintered compact produced by powder metallurgy; a metal or alloy blank with residual pores produced by cast metal manufacturing method; a metal or alloy product produced by an additive manufacturing process having internal residual porosity defects; a porous metal material to be subjected to surface densification treatment; there is a need for metal matrix composites with improved densification or improved bond strength.
Principles and advantages
The invention firstly proposes that: the method for promoting the densification of the blank body by utilizing the synergistic effect of hydrogen absorption expansion of the titanium-containing metal and a rigid mold.
The titaniferous material (particularly, the titaniferous metal) of the present invention exerts an expansion stress on a green body (including a metal article) having pores during hydrogen absorption, or the hydrogen-absorbing and/or hydrogen-storing metal itself. In the case where the volume of the enclosed space (mold cavity) is constant or the volume change is smaller than the hydrogen absorption expansion volume, the stress causes the material to deform and creep, and the internal pores are reduced and closed.
Compared with the traditional powder metallurgy densification technology or the metal plastic processing technology, the method has the following advantages:
(1) the near net shaping can well keep the original complex shape of the product, and can be used for densification treatment of processed complex metal products, additive manufacturing products, powder metallurgy sintering products and powder injection molding products. The advantages of the invention are especially apparent when the structure of the product is more complex and the accuracy requirement is higher.
(2) The production equipment and the die are simple, the production cost is low, and the efficiency is high.
(3) The process treatment temperature is far lower than the temperature of the traditional powder densification treatment, the grain growth in the densification process can be effectively inhibited, a fine-grained and uniform tissue structure is obtained, and the product performance is improved.
Drawings
Fig. 1 shows two experimental rigid molds with different sizes and shapes.
FIG. 2 shows a microstructure of commercially pure titanium without the treatment according to the invention,
FIG. 3 is a microstructure view of industrial pure titanium treated in example 1,
FIG. 4 is a graph comparing the room temperature tensile properties of commercially pure titanium before and after treatment according to the present invention.
The basic structure of the rigid mold can be seen in fig. 1.
As can be seen from fig. 2: the porosity is high.
As can be seen in fig. 3: the porosity of the treated material is obviously reduced.
As can be seen in fig. 4: by comparison, the processing technology of the invention fully improves the strength and plasticity of the material and maintains the mechanical stability of the material.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the present invention, the mold after encapsulation; in the heating process, the condition that the parts are loosened and fall off cannot occur.
The first embodiment is as follows:
1. putting a titanium product (industrial pure titanium, titanium content is more than 98%) with the density of 83% into a stainless steel mould, and packaging and fastening the mould, wherein the fit clearance between the product and the mould is less than 0.1 mm.
2. Placing the assembled mould into an atmosphere sintering furnace, heating to 800 ℃ under the argon atmosphere, and preserving heat for one hour; introducing hydrogen (hydrogen flow is 1L/min), cooling to 600 ℃ at the speed of 1 ℃/min, keeping introducing the hydrogen, keeping the temperature for 4 hours, and cooling the furnace.
3. Turning to a vacuum sintering furnace, and vacuumizing (vacuum degree is less than 10)-3Pa), raising the temperature to 650 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
4. And opening the vacuum sintering furnace, taking out and opening the mold to obtain the titanium alloy product with the density of more than 91%.
Comparative example 1
The other conditions were the same as in the example except that hydrogen was not introduced in the step (2) and argon was introduced; the density of the obtained product has no obvious change.
Example two:
1. and (3) putting the titanium alloy product with the density of 93% into a stainless steel die, wherein the fit clearance between the product and the die is less than 0.1 mm, and packaging and fastening the die.
2. Placing the assembled mould into an atmosphere sintering furnace, heating to 800 ℃ under the argon atmosphere, and preserving heat for 1 hour; introducing hydrogen (hydrogen flow is 1L/min), cooling to 650 ℃ at the speed of 0.5 ℃/min, keeping introducing the hydrogen, keeping the temperature for 4 hours, and cooling the furnace.
3. Putting the mould into a vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 800 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
4. And opening the vacuum sintering furnace, taking out and opening the mold to obtain the titanium alloy product with the density of more than 99.5 percent.
Comparative example No. two
The other conditions were the same as those in example two except that hydrogen was not introduced in step (2) and argon was introduced; the density of the obtained product is not changed.
Example three:
1. the stainless steel mould is filled with titanium alloy with Ti-6Al-4V and 88% density, and the mould is packaged and fastened.
2. Placing the assembled mould into an atmosphere sintering furnace, heating to 800 ℃ under the argon atmosphere, and preserving heat for one hour; changing hydrogen (hydrogen flow is 1L/min), cooling to 650 ℃ at the speed of 2 ℃/min, keeping introducing the hydrogen, keeping the temperature for 4 hours, and cooling the furnace.
3. Turning to a vacuum sintering furnace, and vacuumizing (vacuum degree is less than 10)-3Pa), raising the temperature to 750 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
4. And opening the vacuum sintering furnace, taking out and opening the mold to obtain the titanium alloy product with the density of more than 95%.
Comparative example No. three
The other conditions are the same as those in the third embodiment, except that hydrogen is not introduced in the step (2), and argon is introduced; the density of the obtained product has no obvious change.
Example four:
1. filling a stainless steel mold with a titanium alloy with the components of Ti-6Al-4V and the density of 95% and a titanium composite material with the density of 96% and the content of TiC of 20 vol% to form a composite block, and packaging and fastening the mold.
2. Placing the assembled mould into an atmosphere sintering furnace, heating to 800 ℃ under the argon atmosphere, and preserving heat for one hour; changing hydrogen (hydrogen flow is 1L/min), cooling to 650 ℃ at the speed of 0.5 ℃/min, keeping introducing the hydrogen, keeping the temperature for 4 hours, and cooling the furnace.
3. Turning to a vacuum sintering furnace, and vacuumizing (vacuum degree is less than 10)-3Pa), raising the temperature to 750 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
4. And opening the vacuum sintering furnace, taking out and opening the mold to obtain the titanium composite material product with the integral density of more than 99%.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (8)
1. A method for promoting the densification of a blank by utilizing the hydrogen absorption expansion of a titanium-containing material; the method is characterized in that: loading a titanium-containing substance block, or a filled titanium-containing substance block and a material to be densified, or titanium-containing substance powder and a material to be densified into a rigid mold in a tight fit manner to obtain a pretreatment assembly C, and introducing hydrogen into the pretreatment assembly C to enable the titanium-containing substance to absorb hydrogen; the titanium-containing material and/or the material to be densified are/is densified by utilizing the volume expansion effect of the titanium-containing material;
the hydrogen absorption process is controlled as follows: firstly, heating a pretreatment component C to a temperature of H1 in an inert atmosphere or vacuum, then introducing hydrogen, preserving heat, then cooling to a temperature of H2, and preserving heat, wherein the value range of H1 is 800-;
or
The hydrogen absorption process is controlled as follows: firstly, heating a pretreatment component C to a temperature H3 in an inert atmosphere or vacuum, then introducing hydrogen, preserving heat, continuously heating to H1, and continuously introducing hydrogen; preserving heat; then, cooling to a temperature H2, continuously introducing hydrogen, and preserving heat, wherein the value range of H1 is 800-1000 ℃; the H3 is less than H1;
the titanium-containing material contains metallic titanium;
the inert atmosphere is an argon atmosphere,
the rate of cooling from H1 to H2 is 0.1-2 ℃/min,
the range of H2 is 600-800 ℃; the H2 is less than H1.
2. The method of claim 1, wherein the method comprises promoting green body densification by hydrogen absorption and expansion of the titanium-containing material; it is characterized in that; the blank is a metal blank or a composite material blank.
3. The method of claim 1, wherein the method comprises promoting green body densification by hydrogen absorption and expansion of the titanium-containing material; it is characterized in that; the method comprises the following steps:
step one
Placing the pre-compact blank A into a mold; packaging, fastening and reserving an air vent; obtaining a pretreatment component C, wherein the pre-compact blank A contains a titanium-containing substance with hydrogen absorption capacity; the titaniferous material has a hydrogen-absorbing expansion effect; in the pretreatment component C, the outer wall of the pre-compact blank A is contacted with the inner wall of the mold or a gap is reserved between the outer wall of the pre-compact blank A and the inner wall of the mold; the gap is smaller than the linear expansion of the pre-compact blank A after hydrogen absorption;
or
Putting the pre-compact blank B and the titanium-containing material block into a die together; packaging, fastening and reserving an air vent; obtaining a pretreatment component C; the titaniferous material has a hydrogen-absorbing expansion effect;
or
Putting the pre-compact blank B and the powder of the titanium-containing substance into a die together; packaging, fastening and reserving an air vent; obtaining a pretreatment component C; the titaniferous material has a hydrogen-absorbing expansion effect;
or
Filling titanium-containing material powder into the inner cavity of the mold, and packaging, fastening and reserving an air vent; obtaining a pretreatment component C; the titaniferous material has a hydrogen-absorbing expansion effect;
or
Placing powder to be densified at a set position in the inner cavity of the mold; placing titanium-containing material powder at other positions of the inner cavity of the die; packaging, fastening and reserving an air vent; obtaining a pretreatment component C; the titaniferous material has a hydrogen-absorbing expansion effect;
the moulds are all rigid moulds;
step two
Placing the pretreatment assembly C obtained in the step one in a sintering furnace, heating to a temperature of H1, introducing hydrogen, preserving heat, cooling to a temperature of H2, and preserving heat, wherein the value range of H1 is 800-;
or
Placing the pretreatment assembly C obtained in the step one into a sintering furnace, firstly heating to a temperature of H3 in an inert atmosphere, then introducing hydrogen, preserving heat, then continuously heating to H1, and continuously introducing hydrogen; preserving heat; then, cooling to a temperature H2, continuously introducing hydrogen, and preserving heat, wherein the value range of H1 is 800-1000 ℃; the H3 is less than H1;
after hydrogen absorption is finished, hydrogen is released in a vacuum atmosphere; obtaining a sample after hydrogen desorption;
step three
And removing the mold on the sample after hydrogen discharge to obtain a densified blank.
4. The method for promoting the densification of the green body by utilizing the hydrogen absorption expansion of the titanium-containing material according to claim 3; the method is characterized in that: all parts of the packaged die are kept fastened and cannot loosen in the heating and hydrogen absorption processes.
5. The method for promoting the densification of the green body by utilizing the hydrogen absorption expansion of the titanium-containing material according to claim 3; the method is characterized in that: the material of the mould does not react with hydrogen.
6. The method for promoting the densification of the green body by utilizing the hydrogen absorption expansion of the titanium-containing material according to claim 3; the method is characterized in that: the relative compactness of pre-densified blank A and/or pre-densified blank B is less than or equal to 98%.
7. The method for promoting the densification of the green body by utilizing the hydrogen absorption expansion of the titanium-containing metal according to claim 3; the method is characterized in that: the heat preservation time of H1 is less than or equal to 20 hours;
after the temperature is kept at H1, the temperature is reduced to H2 at the cooling speed of 0.1-2 ℃/min; the holding time at H2 is 20 hours or less.
8. The method for promoting the densification of the green body by utilizing the hydrogen absorption expansion of the titanium-containing material according to claim 3; the method is characterized in that: after the hydrogen absorption is finished, the heat preservation vacuum annealing is carried out at the dehydrogenation temperature D, the dehydrogenation temperature D ranges from 600 ℃ to 900 ℃, and the vacuum degree of the vacuum annealing is lower than 10-3 Pa。
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| JPH01290766A (en) * | 1988-05-18 | 1989-11-22 | Nippon Mining Co Ltd | Ti-containing high-purity ta target and its production |
| CN1404948A (en) * | 2002-10-25 | 2003-03-26 | 中国科学院上海微系统与信息技术研究所 | Preparation for intermediate of nano material |
| CN101530916A (en) * | 2009-04-15 | 2009-09-16 | 中南大学 | Method for controlling the defect of sintering expansion of powder metallurgy material and products thereof and mold |
| CN104087772A (en) * | 2014-07-03 | 2014-10-08 | 昆明冶金研究院 | Powder metallurgy method for preparing high-density titanium and titanium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01290766A (en) * | 1988-05-18 | 1989-11-22 | Nippon Mining Co Ltd | Ti-containing high-purity ta target and its production |
| CN1404948A (en) * | 2002-10-25 | 2003-03-26 | 中国科学院上海微系统与信息技术研究所 | Preparation for intermediate of nano material |
| CN101530916A (en) * | 2009-04-15 | 2009-09-16 | 中南大学 | Method for controlling the defect of sintering expansion of powder metallurgy material and products thereof and mold |
| CN104087772A (en) * | 2014-07-03 | 2014-10-08 | 昆明冶金研究院 | Powder metallurgy method for preparing high-density titanium and titanium alloy |
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