CN108568528A - A kind of micron-size spherical Ti powder and preparation method thereof - Google Patents
A kind of micron-size spherical Ti powder and preparation method thereof Download PDFInfo
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- CN108568528A CN108568528A CN201810841648.XA CN201810841648A CN108568528A CN 108568528 A CN108568528 A CN 108568528A CN 201810841648 A CN201810841648 A CN 201810841648A CN 108568528 A CN108568528 A CN 108568528A
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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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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Abstract
The invention discloses a kind of preparation methods of micron-size spherical Ti powder, which is characterized in that using Ti powders in irregular shape as raw material, is prepared using following steps：(1) radio frequency plasma nodularization；(2) deionized water rinsing, dehydration；(3) it is dried in vacuo.In the method for the present invention, atmosphere is controllable in plasma powder nodularization equipment plasma reactor used, sized spherical titanium powder sphericity height, good fluidity, the grain size prepared are small, and be evenly distributed, impurity is few, compactness is high, technique more rapidly, simple and direct, one-pass molding, it is at low cost, have good industrial prospect, preparation method can be obtained high Oxygen potential (>95%), high sphericity, high-bulk-density, hypoxic sized spherical titanium powder.
Description
Technical field
The present invention relates to metal powder preparing technical field, more particularly to a kind of micron-size spherical Ti powder and its preparation side
Method.
Background technology
Titanium has many advantages, such as that specific strength is high, corrosion resisting property is good, therefore it is extensive to be increasingly focused on sized spherical titanium powders
Ground is applied in the fields such as powder metallurgy, thermal spraying, laser formation, the preparation process of sized spherical titanium powder have become research both at home and abroad and
The hot spot of exploitation.
The advanced technology that powder metallurgy is processed as a kind of material played an important role in Ti industry field, adopt
With titanium powder metallurgy near-net-shape technology, directly preparing finished articles or the parts close to finished size, the technology there can be reduction
The characteristics of process-cycle is shortened in raw materials consumption, and cost saves 20%~50% than common process；Meanwhile powder metallurgy is to powder
Body requires very high, some are directly related with powder diameter for the finished product of compression moulding, and plasma spheroidization powder diameter is more unified, point
Cloth is uniform, is easy to control, and can be perfectly suitable for powder metallurgy；In addition powder metallurgy requires chemical property also very high, compared with
High oxygen content can reduce the mechanical property of suppression performance, compact strength and sintered article.Powder prepared by plasma spheroidization
Oxygen content is extremely low, has unrivaled advantage, therefore have certain regulation to this in powder metallurgy major part technical conditions.Example
Such as, the permission oxygen content of powder is 0.2%~1.5%, and it is 1%~10% that this, which is equivalent to oxide content,；
Laser forming technology can directly use the complex-shaped final part of sized spherical titanium powder one-pass molding using computer model,
The performance of the titanium parts produced is between cast member and forge piece, and cost reduces 15%~30%, time of delivery contracting
It is short by 50%~75%.When preparing porous material, sized spherical titanium powder is best.In addition, preparing densification using laser forming technology
Bio-medical material can save time and materials, realize personalized designs and processing, meet the personalized need of medical material
It asks.
Thermal spraying titanium coating technology be with modern Aviation, space technology appearance and grow up.The technique is one
Kind can reduce the novel process of production cost, and workpiece surface can be made to obtain the titanium coating of required size and property,
Both titanium processing difficulties had been solved the problems, such as, production cost, the titanium valve requirement grain that thermal spraying uses are reduced further through material is saved
Diameter distribution is relatively more unified, and good fluidity is very high to the physical property requirements of powder；The titanium coating of incorporation nanometer spherical titanium valve has
Excellent antistatic property, anti-corrosion anti-scale is also studied and using the continuous development that is applied with sized spherical titanium powder, for spherical shape
The demand of titanium valve quickly increases.High-purity, low cost and stabilized sized spherical titanium powder production technology have become domestic and international powder system
The hot spot of standby technological development.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of micron-size spherical Ti powder and its preparation sides
Method.
The present invention uses following technical scheme：
A kind of preparation method of micron-size spherical Ti powder, which is characterized in that using Ti powders in irregular shape as raw material, adopt
It is prepared with following steps：(1) radio frequency plasma nodularization；(2) plasma water cleans；(3) it is dehydrated；(4) it is dried in vacuo.
Preferably, in step (1), the radio frequency plasma nodularization, the equipment used is TekSphero-40KW
SY165 radio frequency plasma nodularization systems.
It is further preferred that the radio frequency plasma nodularization system powder feeder rotating speed is set as 11~20r/min, powder feeding
Gap is set as 1.5~2mm.
Model SG792 or SI792 it is further preferred that the radio frequency plasma nodularization system powder feeder is popped one's head in, send
Powder device probe height is set as -12~0mm.
It is further preferred that 15~20splm of the radio frequency plasma nodularization system argon gas sheath air flow rate, helium sheath
50~70splm of air flow rate.
It is further preferred that radio frequency plasma nodularization system argon gas center 17~23splm of gas air flow rate.
It is further preferred that the radio frequency plasma nodularization system powder feeding gas flow is 2.5~8splm.
Preferably, in step (2), the rinsing, the time is 2~5min；The dehydration, time are 2~7min, are turned
500~600r/min of speed, dehydration number 2~3 times.
Preferably, in step (3), the vacuum drying, temperature is set as 60~100 DEG C, and soaking time is set as 1h.
A kind of micron-size spherical Ti powder is prepared by any of the above-described preparation method.
Plasma spheroidization equipment operation flow is as follows：Equipment opens system switching, selects manual mode, opens main electricity
Source determines powder feeder probe height and powder feeding gap, sets powder feeder rotating speed, and cooling system booting selects water cooling and probe cold
But, powder feeder and reative cell connecting valve are opened, purification system (beating) is opened, and after purification, is closed powder feeder and is opened with reative cell
It closes, adjusting reaction room pressure to 2.0psi, opens vacuum system and argon gas switch, purification reaction room and receipts powder device, adjustment
Argon gas sheath air flow rate, adjustment argon gas center gas air flow rate after aforesaid operations, open radio frequency plasma power supply, etc.
Wait for that radio frequency plasma system steady operation, dispersion gas are adjusted to 1.5psi, adjust helium sheath air flow rate, regulation power is extremely
40kw adjusts chamber pressure to 15psi, powder feeding gas flow is arranged, opens powder feeder valve, opens ultrasound, equipment starts
Into production procedure.
The principle of the present invention：Raw material powder pattern used in the present invention is irregular, and particle size distribution range is 200~500
Mesh, irregular titanium valve are sent into pdp body torch, under the transmission mechanism effect of radiation, convection current, heat transfer, in the extremely short time
Interior, metallic particles is melt into droplet, and sphericity very high particle is shrunk under the action of surface tension, and high temperature drop is fast
Quickly cooling but, forms micro-sized metal titanium valve.Radio frequency plasma has energy density height, heating intensity big, plasma arcs
Bulky feature, due to there is no electrode, will not because electrode evaporate and polluted product.Under the action of high frequency electric source, inertia
Gas is ionized, and forms stable high temperature inert plasma, original powder in irregular shape is under the action of current-carrying gas, through powder feeding
Device enters pdp body torch, and powder particle absorbs a large amount of heat in high-temperature plasma, and surface is melted rapidly, and with high
Speed enter reactor, be quickly cooled down in an inert atmosphere, under the action of surface tension, cooled and solidified at spherical powder,
It enters back into rewinding room and collects.Heart district temperature is up to 10 in the plasma4DEG C, after leaving plasma, temperature is with 106℃/s
Speed drastically decline, this special temperature field is that the rapid of refractory metal particle surface melts and be quickly cooled down sizing wound
Good temperature environment is made.Because its energy density is concentrated, and nodularization process does not need to all melt powder, so hot
Damage small, heat utilization efficiency is up to 75%, this is also the particular advantages of plasma heat source.
Beneficial effects of the present invention：
1, preparation method of the present invention can be obtained high Oxygen potential (>95%), high sphericity, high-bulk-density, hypoxic
Sized spherical titanium powder is suitable for 3D printing.
2, in the method for the present invention, atmosphere is controllable in plasma powder nodularization equipment plasma reactor used,
The sized spherical titanium powder sphericity height prepared, good fluidity, grain size is small and is evenly distributed, impurity is few, compactness is high, and technique is faster
Fast, simple and direct, one-pass molding, it is at low cost, there is good industrial prospect.
Description of the drawings
Fig. 1 TekSphero-40KW SY165 nodularization equipment drawings.
Fig. 2 titanium valve raw material patterns.
Micron-size spherical Ti powder patterns prepared by Fig. 3 embodiments 1.
Fig. 4 titanium valve raw material powder particle diameter distributions.
Micron-size spherical Ti powder powder diameters distribution prepared by Fig. 5 embodiments 1.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Unless otherwise indicated, the raw material addition percentage employed in the following example of the present invention is mass percent.
Embodiment 1：
The preparation method of micron-size spherical Ti powder
Raw material prepares original titanium valve in irregular shape using HDH method, and powder specifics are 15~53 μm, are used
Radio frequency plasma nodularization unit type be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SG792, powder feeding gap be 2mm, probe height -10mm, powder feeder rotating speed 15r/min, argon gas sheath air flow rate 20splm,
Helium sheath air flow rate 50splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 5splm, primary dewatering parameter
For：Water is added to rinse 2min, dehydrating speed 500r/min, second dehydration parameter is：Water is added to rinse 3min, dehydrating speed is
500r/min, slurry are put into 100 DEG C of heat preservation 1h of vacuum drying chamber.
Embodiment 2：
The preparation method of micron-size spherical Ti powder
Raw material prepares original titanium valve in irregular shape using HDH method, and powder specifics are 15~53 μm, are used
Radio frequency plasma nodularization unit type be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SG792, powder feeding gap be 1.5mm, probe height -10mm, powder feeder rotating speed 20r/min, argon gas sheath air flow rate
20splm, helium sheath air flow rate 70splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 8splm, primary de-
Water parameter is：Water is added to rinse 2min, dehydrating speed 550r/min, second dehydration parameter is：Water is added to rinse 3min, dehydrating speed
For 550r/min, slurry is put into 100 DEG C of heat preservation 1h of vacuum drying chamber.
Embodiment 3：
The preparation method of micron-size spherical Ti powder
Raw material prepares original titanium valve in irregular shape using HDH method, and powder specifics are 15~53 μm, are used
Radio frequency plasma nodularization unit type be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 2mm, probe height -10mm, powder feeder rotating speed 11r/min, argon gas sheath air flow rate 15splm,
Helium sheath air flow rate 50splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 8splm, primary dewatering parameter
For：Water is added to rinse 2min, dehydrating speed 600r/min, second dehydration parameter is：Water is added to rinse 3min, dehydrating speed is
600r/min, slurry are put into 100 DEG C of heat preservation 1h of vacuum drying chamber..
Embodiment 4：
The preparation method of micron-size spherical Ti powder
Raw material prepares original titanium valve in irregular shape using HDH method, and powder specifics are 15~53 μm, are used
Radio frequency plasma nodularization unit type be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 1.8mm, probe height -10mm, powder feeder rotating speed 20r/min, argon gas sheath air flow rate
18splm, helium sheath air flow rate 60splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 8splm, primary de-
Water parameter is：Water is added to rinse 4min, dehydrating speed 500r/min, second dehydration parameter is：Water is added to rinse 5min, dehydrating speed
For 500r/min, slurry is put into 100 DEG C of heat preservation 0.5h of vacuum drying chamber.
Embodiment 5：
The preparation method of micron-size spherical Ti powder
Raw material prepares original titanium valve in irregular shape using HDH method, and powder specifics are 15~53 μm, are used
Radio frequency plasma nodularization unit type be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 1.5mm, probe height -10mm, powder feeder rotating speed 20r/min, argon gas sheath air flow rate
20splm, helium sheath air flow rate 70splm, argon gas central fluidizing gas flow 23splm, powder feeding gas flow are 2.5splm, once
Being dehydrated parameter is：Water is added to rinse 4min, dehydrating speed 550r/min, second dehydration parameter is：Water is added to rinse 5min, dehydration turns
Speed is 550r/min, and slurry is put into 80 DEG C of heat preservation 1h of vacuum drying chamber.
Embodiment 6：
The preparation method of micron-size spherical Ti powder
Raw material prepares original titanium valve in irregular shape using HDH method, and powder specifics are 15~53 μm, are used
Radio frequency plasma nodularization unit type be TekSphero-40Plasma System SY165.Nodularization parameter setting is：It send
Powder device pop one's head in model SG792, powder feeding gap be 1.5mm, probe height -12mm, powder feeder rotating speed 20r/min, argon gas sheath gas
It is 8splm to flow flow 20splm, helium sheath air flow rate 70splm, argon gas central fluidizing gas flow 17splm, powder feeding gas flow,
Primary dewatering parameter is：Water is added to rinse 4min, dehydrating speed 550r/min, second dehydration parameter is：Add water to rinse 5min, takes off
Water rotating speed is 550r/min, and triple dewatering parameter is：Water is added to rinse 5min, dehydrating speed 550r/min, slurry is put into vacuum
60 DEG C of heat preservation 1h of drying box.
Embodiment 7：
The preparation method of micron-size spherical Ti powder
Raw material prepares original titanium valve in irregular shape using HDH method, and powder specifics are 15~53 μm, are used
Radio frequency plasma nodularization unit type be TekSphero-40Plasma System SY165.Nodularization parameter setting is：It send
Powder device is popped one's head in model SI792, and powder feeding gap is 1.5mm, probe height 0mm, powder feeder rotating speed 20r/min, argon gas sheath air-flow
Flow 20splm, helium sheath air flow rate 70splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow be 8splm, one
Secondary dehydration parameter is：Water is added to rinse 5min, dehydrating speed 550r/min, second dehydration parameter is：Water is added to rinse 7min, dehydration
Rotating speed is 550r/min, and slurry is put into 100 DEG C of heat preservation 2h of vacuum drying chamber.
Performance test：
By titanium valve mobility, tap density, pine before and after the micron-size spherical Ti powder prepared in above-described embodiment 1 progress nodularization
Fill density measurement, test result such as table one：
Table one：Titanium valve mobility, tap density, apparent density before and after nodularization
Above-described embodiment is merely illustrative of the technical solution of the present invention and is not intended to limit it, all without departing from the present invention
Any modification of spirit and scope or equivalent replacement should all cover the range in technical solution of the present invention.
Claims (10)
1. a kind of preparation method of micron-size spherical Ti powder, which is characterized in that using Ti powders in irregular shape as raw material, use
It is prepared by following steps：(1) radio frequency plasma nodularization；(2) deionized water rinsing, dehydration；(3) it is dried in vacuo.
2. a kind of preparation method of micron-size spherical Ti powder according to claim 1, which is characterized in that in step (1), institute
The radio frequency plasma nodularization stated, the equipment used is TekSphero-40KW SY165 radio frequency plasma nodularization system.
3. a kind of preparation method of micron-size spherical Ti powder according to claim 2, which is characterized in that described radio frequency etc. from
Daughter nodularization system powder feeder rotating speed is set as 11~20r/min, powder feeding gap is set as 1.5~2mm.
4. a kind of preparation method of micron-size spherical Ti powder according to claim 2, which is characterized in that described radio frequency etc. from
Daughter nodularization system powder feeder probe model SG792 or SI792, powder feeder probe height are set as -12~0mm.
5. a kind of preparation method of micron-size spherical Ti powder according to claim 2, which is characterized in that described radio frequency etc. from
15~20splm of daughter nodularization system argon gas sheath air flow rate, 50~70splm of helium sheath air flow rate.
6. a kind of preparation method of micron-size spherical Ti powder according to claim 2, which is characterized in that described radio frequency etc. from
Daughter nodularization system argon gas center 17~23splm of gas air flow rate.
7. a kind of preparation method of micron-size spherical Ti powder according to claim 2, which is characterized in that described radio frequency etc. from
Daughter nodularization system powder feeding gas flow is 2.5~8splm.
8. a kind of preparation method of micron-size spherical Ti powder according to claim 1, which is characterized in that in step (2), institute
The rinsing stated, time are 2~5min；The dehydration, the time be 2~7min, 500~600r/min of rotating speed, dehydration number 2~
3 times.
9. a kind of preparation method of micron-size spherical Ti powder according to claim 1, which is characterized in that in step (3), institute
The vacuum drying stated, temperature are set as 60~100 DEG C, and soaking time is set as 0.5~2h.
10. a kind of micron-size spherical Ti powder, which is characterized in that micron-size spherical Ti powder is prepared by any one of claim 1 to 9
Method is prepared.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110756807A (en) * | 2019-11-29 | 2020-02-07 | 中国工程物理研究院材料研究所 | Laser melting deposition method of hydrogenated titanium dehydrogenated powder |
| CN113333768A (en) * | 2021-05-10 | 2021-09-03 | 苏州英纳特纳米科技有限公司 | Shaping treatment method of spherical high-temperature alloy powder GH4169 |
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| CN110756807A (en) * | 2019-11-29 | 2020-02-07 | 中国工程物理研究院材料研究所 | Laser melting deposition method of hydrogenated titanium dehydrogenated powder |
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| CN113333768A (en) * | 2021-05-10 | 2021-09-03 | 苏州英纳特纳米科技有限公司 | Shaping treatment method of spherical high-temperature alloy powder GH4169 |
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Address after: 528400 two of the 1 workshop of No. 36 West tech Road, Torch Development Zone, Zhongshan, Guangdong. Applicant after: GENT MATERIALS SURFACE TECHNOLOGY (GUANGDONG) Co.,Ltd. Address before: 528400, first, second building, Twentieth building, No. 18, Pioneer Road, Torch Development Zone, Guangdong, Zhongshan Applicant before: GENT MATERIALS SURFACE TECHNOLOGY (GUANGDONG) Co.,Ltd. |
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