CN106623952A - Preparation method of titanium or titanium alloy powder with micro-hydrogenated surface - Google Patents
Preparation method of titanium or titanium alloy powder with micro-hydrogenated surface Download PDFInfo
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- CN106623952A CN106623952A CN201611177668.9A CN201611177668A CN106623952A CN 106623952 A CN106623952 A CN 106623952A CN 201611177668 A CN201611177668 A CN 201611177668A CN 106623952 A CN106623952 A CN 106623952A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
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- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a preparation method of titanium or titanium alloy powder with micro-hydrogenated surface. The method comprises the following steps: (1) a titanium or titanium alloy bar with low pollution and specific size is prepared in advance; (2) an atomizing unit is pre-vacuumized and then filled with high-purity inert gas as shielding gas; (3) the lower end of the titanium or titanium alloy bar is heated to be melted by an induction coil, and atomized power preparation is performed; (4) titanium or titanium alloy powder obtained after atomization enters a cyclone separator, hydrogen is introduced into the cyclone separator, and low-temperature surface micro-hydrogenation treatment is finished in the cyclone separator; (5) after the powder is cooled completely, the titanium or titanium alloy powder with micro-hydrogenated surface is taken from a powder collecting tank. Aiming at the problem of high probability of oxidation of titanium or titanium alloy powder surface, crucible-free atomization and low-temperature surface micro-hydrogenation are combined, and the titanium or titanium alloy powder with the micro-hydrogenated surface, little pollution and excellent oxidation resistance for 3D printing is prepared.
Description
Technical field
The present invention relates to the preparation method of a kind of titanium of the micro- hydrogenation in surface or titanium alloy powder, belongs to field of material preparation.
Background technology
Gas atomization is that one kind is directly smashed by high velocity air and quickly cooling molten metal prepares metal dust
Method, it applies extremely wide, is used in particular in the production of 3D printing metal dust.3D printing is referred to mathematical model
It is foundation, the technology of 3D solid object manufacture is carried out by way of material successively adds up, represents world's development of manufacturing
New direction.The metal objects prepared using 3D printing technique in order to ensure the consistency and uniformity of its internal organizational structure,
To be respectively provided with high requirement using the size distribution of metal dust, sphericity and mobility, oxygen content etc..
Titanium alloy has a series of excellent properties such as light weight, high-strength and anti-corrosion because of it, be widely used in Aero-Space and
The fields such as military project, are also that metal 3D printing field uses a most class materials.Aerosolization rule is to prepare 3D printing to be closed with titanium
The common method at bronze end, a kind of fine grain hypoxemia spherical titanium and titanium alloy that such as Chinese invention patent CN104308168B is announced
The preparation method of powder.However, due to the high chemism of titanium elements, easily reacting in titanium alloy powder table with oxygen
Face generates fine and close oxide layer, and the presence of titanium oxide substantially increases the laser sintered difficulty of titanium alloy powder, and then affects
The Forming Quality of 3D printing part.To prevent the oxidation of titanium alloy powder, Chinese invention patent CN103846447B from disclosing one kind
The aerosolization preparation method of superfine spherical titanium or titanium alloy powder, the method is carried out using double-deck atomizer to titanium or titanium alloy
Atomization and hydrogenation, have the titanium of hydrogenation titanium film or the preparation of titanium alloy powder so as to complete Surface Creation.But the method is in system
There are some weak points in powder practice:First, using double-deck atomizing nozzle structure so that atomizing nozzle structure is complicated, manufacture
It is relatively costly;Secondly, the introducing position that air-flow is hydrogenated in the method is too near apart with atomization air flow, melts and is formed after body fluid flow atomization
Melt drop still there is higher temperature, and titanium or titanium alloy hydrogenation rate at high temperature is very high, causes powder easily excessive
Hydrogen is inhaled, powder hydrogenation process is difficult to control to;Again, because hydrogenation air-flow is introduced from atomizer, whole atomization cavity is caused
Inside there is hydrogen, on the one hand, the still titanium with the higher temperature or titanium alloy powder long-time in atomization cavity connects with hydrogen
Touch, cause powder excessively to inhale hydrogen, and the titantium hydride of a large amount of brittlement phases is internally generated in powder, affect powder quality, on the other hand,
Hydrogen is not only filled with whole atomization cavity, meanwhile, hydrogen can also diffuse into working chamber by the mozzle of atomizer, give
Powder production brings larger potential safety hazard;Finally, the hydrogen of titanium or titanium alloy powder excessive consumption is laser sintered in 3D printing
During concentration release, not only affect the Forming Quality of 3D printing part, and be discharged into and print hydrogen excessive in bin and also will
Form certain potential safety hazard.
The content of the invention
The purpose of the present invention is to overcome the shortcomings of that above prior art is present, there is provided a kind of titanium or titanium of the micro- hydrogenation in surface is closed
The preparation method at bronze end, had both solved double-deck atomizer and had inhaled the uncontrollable problem of hydrogen process, and the safety of manufacture is improve again
Property.
To realize object above, the technical scheme is that:A kind of titanium of the micro- hydrogenation in surface or the system of titanium alloy powder
Preparation Method, with titanium or titanium alloy rod bar as raw material, is protected by forvacuum with high purity inert gas are passed through, and prevents titanium or titanium from closing
Oxidation of the gold in fusing with atomization process, and titanium or the fusing of titanium alloy bar one end and shape are made by the way of induction coil heating
Into stable liquid stream, the liquid stream carries out powder by atomization by the atomizer using high purity inert gas as medium again, atomization
Stress control is in 3~8MPa;The titanium or titanium alloy powder that atomization is completed is carried along into cyclone separator by air-flow, in whirlwind point
The high-purity hydrogen of 0.3~0.5MPa, 10~25at.% of hydrogen content and the mixed gas of high purity inert gas are passed through from device lower end, and
The suction hydrogen on its surface is completed using powder itself residual temperature, on powder surface very thin suction hydrogen layer is formed, realize that titanium or titanium are closed
Micro- hydrogenation on bronze end surface.
Further, forvacuum is to vacuum 1 × 10-4~1 × 10-2Pa。
Further, high purity inert gas are using high-purity argon gas or high-purity helium.
Further, the thickness for inhaling hydrogen layer is 30~100nm.
Compared with prior art, the invention has the beneficial effects as follows:
(1) due to substantially reducing into the titanium of cyclone separator or the temperature of titanium alloy powder, now, the suction hydrogen of powder
Speed is greatly reduced, and so as to only form very thin suction hydrogen layer on powder surface, has not both served the effect of micro- hydrogenation oxygen barrier, and not
Powder over-hydrogenation can be made;
(2) low pressure hydrogen for introducing from cyclone separator cavity lower end and the height from atomization cavity into cyclone separator
Pressure atomization gas go in the same direction, because its pressure is significantly less than atomization gas, thus can only be in cyclone separator one
Fraction region forms hydrogenating environment, without in atomization cavity, its security is greatly improved.
(3) titanium or titanium alloy powder of the micro- hydrogenation in surface prepared by the present invention, pollution less, mobility and non-oxidizability
It is good, it is especially suitable for 3D printing and uses.
Description of the drawings
Fig. 1 is the structural representation of gas atomization device involved in the present invention.
Fig. 2 is the X ray diffracting spectrum at TC4 titanium alloys bronze end prepared by the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph of TC4 titanium alloy powders prepared by the present invention.
1 is melting chamber in figure, and 2 are atomization air valve, and 3 is atomization chamber, and 4 is feeding rod, and 5 is alloy bar, and 6 is induction coil, 7
For atomizer, 8 is blast pipe, and 9 is cyclone separator, and 10 are hydrogenation air valve, and 11 is powder collecting tank.
Specific embodiment
A kind of titanium of the micro- hydrogenation in surface or the preparation method of titanium alloy powder, are carried out according to the following steps:
(1) need and equipment requirement, such as Fig. 1 according to powder processed, prepare the titanium or titanium alloy of low stain and specific dimensions in advance
Rod 5;
(2) to melting chamber 1, atomization chamber 3 and the inside forvacuum of cyclone separator 9 in atomising device, treat that vacuum reaches 1
×10-4~1 × 10-2Pa, by being atomized air valve 2 protection of 0.09MPa high purity inert gas is filled with, and prevents powder in atomization process
In oxidation;
(3) titanium or the lower end of titanium alloy bar 5 are carried out plus heat fusing by induction coil 6, and is formed by controlling feeding rod 4
Stable liquid stream, after powder by atomization is carried out by the atomizer 7 using high purity inert gas as medium, atomizing pressure control exists
3~8MPa;
(4) titanium alloy powder that atomization is completed is carried along into cyclone separator 9 by air-flow, leads to inside cyclone separator
Over hydrogenation air valve 10 is passed through the high-purity hydrogen of 0.3~0.5MPa, 10~25at.% of hydrogen content and the gaseous mixture of high purity inert gas
Body, the position of air inlet should be higher than that 10~20cm of exhaust outlet in cyclone separator, and complete it using powder itself residual temperature
The suction hydrogen on surface, on powder surface very thin suction hydrogen layer is formed, and realizes micro- hydrogenation on powder surface, effectively prevents the oxygen of powder
Change, the powder for completing to inhale hydrogen falls into the lower section powder collecting tank 11 of cyclone separator 9, and unnecessary hydrogen is then discharged by blast pipe 8
Cavity;
(5) after powder is cooled down completely, titanium or titanium alloy powder are obtained from powder collecting tank 11, and according to different grain size etc.
Level is sieved and is vacuum-packed.
Below in conjunction with the accompanying drawings the principle and feature of the present invention are described with embodiment, example is served only for explaining this
Invention, is not intended to limit the scope of the present invention.
Embodiment 1
Ti-6Al-4V (TC4) alloy powder of the micro- hydrogenation in surface is prepared without crucible gas atomization.
With diameter 40mm, TC4 titanium alloy bar of the impurity content less than 0.1% is raw material, to atomization plant forvacuum, is treated
Vacuum reaches 1 × 10-4Pa, is filled with the high-purity argon gas protection of 0.09MPa, anti-oxidation.By induction coil to titanium alloy bar
Lower end is carried out plus heat fusing, forms stable liquid stream, is then atomized by the atomizer using high-purity argon gas as medium
Powder processed, atomizing pressure control is atomized the titanium alloy powder for completing and is carried along into cyclone separator by air-flow in 5~7MPa, revolves
Wind separator bottom is passed through the hydrogen and argon gas mixed gas of 0.3MPa hydrogen content 10at.%, and the position of air inlet should be higher than that rotation
Exhaust outlet 10cm in wind separator, and complete the suction hydrogen on its surface using powder itself residual temperature.After powder is cooled down completely,
Titanium alloy powder is obtained from powder collecting tank, and is sieved and is vacuum-packed according to different grain size grade.Jing test analysis,
The surface hydriding thickness degree of TC4 powder is about 30nm, and overall oxygen content is less than 800ppm, and it is 10~50 μm that size distribution is interval.
Fig. 2 illustrates the X ray diffracting spectrum at the TC4 titanium alloys bronze end of preparation, as illustrated, powder is α titaniums consolidating with the mixing of β titaniums
Solution phase, does not have substantial amounts of titantium hydride to generate without obvious titantium hydride diffraction maximum, namely powder surface.Fig. 3 provides the TC4 for preparing
The scanning electron microscope (SEM) photograph of titanium alloy powder, as illustrated, powder shows good sphericity, even particle size distribution, particle diameter is 10
Between~50 μm.
Embodiment 2
The Ti-45Al-2Cr-8Nb alloy powders of the micro- hydrogenation in surface are prepared without crucible gas atomization.
With diameter 40mm, Ti-45Al-2Cr-8Nb titanium alloy bar of the impurity content less than 0.1% is raw material, and atomization is set
Standby forvacuum, treats that vacuum reaches 1 × 10-4Pa, is filled with the high-purity helium protection of 0.09MPa, anti-oxidation.By the line of induction
Circle is carried out plus heat fusing to titanium alloy bar lower end, stable liquid stream is formed, then by the atomization using high-purity helium as medium
Nozzle carries out powder by atomization, and atomizing pressure control is atomized the titanium alloy powder for completing and is carried along into rotation by air-flow in 6~8MPa
Wind separator, cyclone separator bottom is passed through the hydrogen and helium mix gas of 0.5MPa hydrogen content 25at.%, the position of air inlet
Put and should be higher than that exhaust outlet 20cm in cyclone separator, and the suction hydrogen on its surface is completed using powder itself residual temperature.Treat powder
After cooling down completely, titanium alloy powder is obtained from powder collecting tank, and sieved and be vacuum-packed according to different grain size grade.Jing
Test analysis, the surface hydriding thickness degree of Ti-45Al-2Cr-8Nb powder is about 100nm, and overall oxygen content is less than 500ppm,
It is 10~30 μm that size distribution is interval.
Embodiment 3
The pure titanium powder of the micro- hydrogenation in surface is prepared without crucible gas atomization.
With diameter 40mm, pure titanium rod of the impurity content less than 0.1% is raw material, to atomization plant forvacuum, treats vacuum
Degree reaches 1 × 10-4Pa, is filled with the high-purity argon gas protection of 0.09MPa, anti-oxidation.Pure titanium rod lower end is entered by induction coil
Row plus heat fusing, form stable liquid stream, then carry out powder by atomization, mist by the atomizer using high-purity argon gas as medium
Change Stress control in 3~5MPa, be atomized the titanium alloy powder for completing and cyclone separator, cyclone separator are carried along into by air-flow
Bottom is passed through the hydrogen and argon gas mixed gas of 0.4MPa hydrogen content 20at.%, and the position of air inlet should be higher than that cyclone separator
Interior exhaust outlet 15cm, and complete the suction hydrogen on its surface using powder itself residual temperature.After powder is cooled down completely, receive from powder
Collection tank obtains pure titanium powder, and is sieved and be vacuum-packed according to different grain size grade.Jing test analysis, the table of pure titanium powder
Face hydride layer thickness is about 70nm, and overall oxygen content is less than 600ppm, and it is 20~50 μm that size distribution is interval.
Claims (5)
1. the preparation method of a kind of titanium of the micro- hydrogenation in surface or titanium alloy powder, it is characterised in that be with titanium or titanium alloy rod bar
Raw material, is protected by forvacuum with high purity inert gas are passed through, and prevents the oxygen of titanium or titanium alloy in fusing with atomization process
Change, and melt titanium or titanium alloy bar one end by the way of induction coil heating and form stable liquid stream, the liquid stream is again
Powder by atomization is carried out by the atomizer using high purity inert gas as medium, atomizing pressure is controlled in 3~8MPa;It has been atomized
Into titanium or titanium alloy powder cyclone separator is carried along into by air-flow, be passed through 0.3~0.5MPa in cyclone separator lower end
The high-purity hydrogen of 10~25at.% of hydrogen content and the mixed gas of high purity inert gas, and it is complete using powder itself residual temperature
Into the suction hydrogen on its surface, formed on powder surface and inhale hydrogen layer.
2. preparation method as claimed in claim 1, it is characterised in that forvacuum is to vacuum 1 × 10-4~1 × 10-2Pa。
3. preparation method as claimed in claim 1, it is characterised in that high purity inert gas are using high-purity argon gas or high-pure helium
Gas.
4. preparation method as claimed in claim 1, it is characterised in that the thickness for inhaling hydrogen layer is 30~100nm.
5. preparation method as claimed in claim 1, it is characterised in that the position of the air inlet of high-purity hydrogen is higher than cyclonic separation
10~20cm of exhaust outlet in device.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108580874A (en) * | 2018-05-15 | 2018-09-28 | 南京尚吉增材制造研究院有限公司 | Hydrogen processing method is set for improve increasing material manufacturing titanium alloy microstructure |
CN113319283A (en) * | 2021-06-04 | 2021-08-31 | 孙晓华 | Airflow milling pretreatment and trace hydrogen auxiliary sintering method for titanium coating |
CN115213400A (en) * | 2021-03-31 | 2022-10-21 | 泰州市新龙翔金属制品有限公司 | Production process for improving mechanical property of medical metal alloy |
CN115535961A (en) * | 2022-10-24 | 2022-12-30 | 云南电网有限责任公司电力科学研究院 | Hydrogen absorption and desorption device for hydrogen storage alloy and preparation method thereof |
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CN105195750A (en) * | 2015-10-16 | 2015-12-30 | 北京工业大学 | Preparation method of micro low-oxygen titanium hydride powder |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN108580874A (en) * | 2018-05-15 | 2018-09-28 | 南京尚吉增材制造研究院有限公司 | Hydrogen processing method is set for improve increasing material manufacturing titanium alloy microstructure |
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CN113319283A (en) * | 2021-06-04 | 2021-08-31 | 孙晓华 | Airflow milling pretreatment and trace hydrogen auxiliary sintering method for titanium coating |
CN113319283B (en) * | 2021-06-04 | 2023-08-22 | 孙晓华 | Air flow mill pretreatment and micro hydrogen assisted sintering method for titanium coating |
CN115535961A (en) * | 2022-10-24 | 2022-12-30 | 云南电网有限责任公司电力科学研究院 | Hydrogen absorption and desorption device for hydrogen storage alloy and preparation method thereof |
CN115535961B (en) * | 2022-10-24 | 2024-03-19 | 云南电网有限责任公司电力科学研究院 | Hydrogen absorbing and releasing device for hydrogen storage alloy and preparation method thereof |
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