CN108620598A - A kind of preparation method of tantalum powder - Google Patents
A kind of preparation method of tantalum powder Download PDFInfo
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- CN108620598A CN108620598A CN201810665315.6A CN201810665315A CN108620598A CN 108620598 A CN108620598 A CN 108620598A CN 201810665315 A CN201810665315 A CN 201810665315A CN 108620598 A CN108620598 A CN 108620598A
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- tantalum
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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
- B22F9/10—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 using centrifugal force
Abstract
The invention discloses a kind of preparation methods of tantalum powder, are related to high-quality metal powder preparing technical field.This method includes:Tantalum item is prepared into the first tantalum stick for meeting first condition with electron-beam smelting, the first condition includes:O≤150ppm, C≤100ppm, N≤50ppm, H≤15ppm;The first tantalum stick is processed as diameter between 50mm~60mm, second tantalum stick of the length between 300mm~400mm;The first end of the second tantalum stick is stretched into spray chamber, the second end of the second tantalum stick is connect with the electro spindle of plasma rotating electrode powder manufacturing apparatus;The second tantalum stick forms tantalum powder by plasma rotating electrode powder manufacturing apparatus.
Description
Technical field
The present invention relates to high-quality metal powder preparing technical fields, more particularly relate to a kind of preparation method of tantalum powder.
Background technology
Tantalum metal belongs to refractory metal, the corrosion resistance with exceptional, while still generally acknowledged biocompatibility is best
Metal material, monopolized for a long time by overseas enterprise by high-end biologic implant part prepared by pure tantalum material.It is most widely used at present
Tantalum implant be Jie Mai companies of the U.S. product, the tantalum implant product of the said firm be first by polyurethane foamed material precursor into
Row pyrolysis obtains the nature of glass with spongy porous structure and is pyrolyzed carbon skeleton, then using the pure tantalum of business as raw material, uses chemistry
(English is for vapor deposition:Chemical vapor deoposition, CVD) method, with chlorine reaction generate tantalic chloride, then
It is passed through hydrogen reducing, one layer of tantalum powder is generated on porous foamed material by controlling reduction temperature and time, finally through burning
The medical porous tantalum implant with some strength is made in knot.The mode that another kind prepares medical porous tantalum implant is first by tantalum
Powder is mixed with foaming agent, and forms the tantalum porous body with certain porosity by foaming under certain condition, then will drying
Porous body afterwards is sintered in vacuum drying oven, eventually forms the tantalum porous body of some strength.Recently as increases material manufacturing technology
Development, carry out the developing direction for being quickly manufactured as current research and assert of personalized porous tantalum implant, but increase material
The process characteristic of manufacturing technology requires the powder applied to the manufacturing technology that must have suitable size distribution, preferable spherical shape
Rate, preferable mobility and its lower impurity content.
It is mainly chemical method and Physical to prepare tantalum powder method at present, and chemical method is with the compound of tantalum metal and reduction
Agent carries out electronation and prepares tantalum metal powder;Physical is to pass through hydrogen by vapor deposition, plasma sputtering or compact metal
Change and is made;Also by the tantalum metal powder prepared by tantalum metal hydride, broken, classification, impurity removal process.Prepared by above-mentioned technology
Tantalum powder be mostly sheet, amorphous or subsphaeroidal powder, granularity is tiny, is less than 50 μm, tantalum powder prepared by Part Methods more
Oxygen content in 1000ppm or so.Above-mentioned power applications carry out the quick manufacture of personalized tantalum implant to material increasing field
There is its deficiency, powder flowbility is poor, is unfavorable for the conveying of powder and sprawls, and the interstitial element content of powder is higher, influences to increase
Material manufactures the mechanical property of tantalum implant.
Invention content
The embodiment of the present invention provides a kind of preparation method of tantalum powder, to solve to exist in the prior art tantalum powder mobility
The interstitial element content of difference, powder is higher, the problem of causing to influence to increase the mechanical property for just manufacturing tantalum implant.
The embodiment of the present invention provides a kind of preparation method of tantalum powder, including:
Tantalum item is prepared into the first tantalum stick for meeting first condition with electron-beam smelting, the first condition includes:O≤
150ppm, C≤100ppm, N≤50ppm, H≤15ppm;
The first tantalum stick is processed as diameter between 50mm~60mm, second tantalum of the length between 300mm~400mm
Stick;The first end of the second tantalum stick is stretched into spray chamber, second end and the plasma rotating electrode system of the second tantalum stick
The electro spindle of powder equipment connects;
The second tantalum stick forms tantalum powder by plasma rotating electrode powder manufacturing apparatus.
Preferably, the second tantalum stick forms tantalum powder by plasma rotating electrode powder manufacturing apparatus, specifically includes:
Second tantalum stick high speed rotation under electro spindle drive, the second end face of the second tantalum stick is in plasma
The lower fusing of arc effect, and Centrifugal dispersion, form the tantalum powder after condensation.
Preferably, the electro spindle drive the high-speed rotating rotating speed of the second tantalum stick between 15000r/min~
Between 20000r/min.
Preferably, the fusion current of the plasma arc is between 4000A~5000A.
Preferably, the second tantalum stick stretches into 1/3 of the indoor length of atomization less than the spray chamber length.
Preferably, between diameter Jie 60mm~70mm of the first tantalum stick.
An embodiment of the present invention provides a kind of preparation methods of tantalum powder, including:Tantalum melting is prepared into satisfaction first
First tantalum stick of part, the first condition include:O≤150ppm, C≤100ppm, N≤50ppm, H≤12ppm;By described
One tantalum stick is processed as diameter between 50mm~60mm, second tantalum stick of the length between 300mm~400mm;By the second tantalum stick
First end stretch into spray chamber, the second end of the second tantalum stick and the electro spindle of plasma rotating electrode powder manufacturing apparatus connect
It connects;The second tantalum stick forms tantalum powder by plasma rotating electrode powder manufacturing apparatus.Preparation method production efficiency simple for process
Height, contaminated risk is small, the tantalum powder of the high ball form quotient of high-quality suitable for scale production.Pass through the ball of tantalum powder prepared by this method
Shape degree is relatively high, wherein spherical rate can reach 90% or more, furthermore, the powder degree range of the tantalum powder ball between 10~130 μm it
Between;It is low that other interstitial element contents such as oxygen content of the tantalum powder of powder are prepared by this method, are suitable for medical porous tantalum and are implanted into material
The preparation of material further applies also for increasing the personalization quickly manufacture that material technology carries out tantalum porous implant.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Obtain other attached drawings according to these attached drawings.
Fig. 1 is a kind of preparation method flow diagram for tantalum powder that the embodiment of the present invention carries;
Fig. 2 is the preparation spherical shape tantalum powder SEM schematic diagrames that the embodiment of the present invention 1 provides;
Fig. 3 is the preparation spherical shape tantalum powder SEM schematic diagrames that the embodiment of the present invention 2 provides.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Fig. 1 is a kind of preparation method flow diagram for tantalum powder that the embodiment of the present invention carries, as shown in Figure 1, this method master
Include the following steps:
Step 101, tantalum item is prepared into the first tantalum stick for meeting first condition, the first condition packet with electron-beam smelting
It includes:O≤150ppm, C≤100ppm, N≤50ppm, H≤15ppm;
Step 102, the first tantalum stick is processed as diameter between 50mm~60mm, length is between 300mm~400mm's
Second tantalum stick;The first end of the second tantalum stick is stretched into spray chamber, second end and the plasma of the second tantalum stick rotate
The electro spindle of electrode powder manufacturing apparatus connects;
Step 103, the second tantalum stick forms tantalum powder by plasma rotating electrode powder manufacturing apparatus.
In a step 101, tantalum item is prepared by the first tantalum stick by electron-beam smelting method, wherein the first tantalum stick it is straight
Diameter is between 60mm~70mm, in embodiments of the present invention, specific restriction is not done to the diameter of the first tantalum stick.
It should be noted that the first tantalum stick being prepared into needs to meet first condition, and in embodiments of the present invention, first
Part includes O≤150ppm, C≤100ppm, N≤50ppm, H≤15ppm.
In a step 102, the first tantalum stick is processed into diameter between 50mm~60mm again, length between 300mm~
The second tantalum stick between 400mm, in embodiments of the present invention, the specific method to the first tantalum stick to be processed into the second tantalum stick are not done
It limits.
The first end for the second tantalum stick being prepared into is extend into spray chamber, and first end stretches into the length of spray chamber and is less than
The second end of second tantalum stick is connect by the 1/3 of spray chamber length with the electro spindle of plasma rotating electron powder manufacturing apparatus, main in electricity
When axis rotates, the second tantalum stick can be driven to be rotated.
In step 103, when electro spindle starts high speed rotation, the second tantalum stick can be driven in plasma rotating electron powder
High speed rotation is carried out in equipment, meanwhile, the second end face of the second tantalum stick in plasma rotating electron powder manufacturing apparatus by it is equal from
The effect of subarc starts to melt, and when rotating at high speed, and from second end face Centrifugal dispersion, tantalum powder is formd after condensation.
It should be noted that the electronics main shaft in plasma rotating electron powder manufacturing apparatus is when rotating at high speed, plasma arc
Fusion current between 4000A~5000A.
In order to the clearer preparation method for introducing tantalum powder provided in an embodiment of the present invention, individually below with embodiment
1~embodiment 3 introduces the preparation method of tantalum powder.
Embodiment 1
Step 1: using electron beam melting processes by tantalum melting as the first tantalum stick of high-purity;
O=130ppm, C=90ppm, N=30ppm, H=12ppm in first tantalum stick.
Step 2: the first tantalum stick is passed through the second tantalum stick of mechanical processing diameter 50mmmm, length 300mm;
Step 3: the second end of the second pure tantalum stick is connected to electro spindle, first end stretches into argon gas protection spray chamber, with electricity
Main shaft drives tantalum stick high speed rotation in the horizontal direction;
Step 4: the high-power equal arc of recess with 4000A fusion currents melt high-speed rotating second tantalum stick, the second tantalum stick
High ball form quotient tantalum powder is obtained after first end face fusing and Centrifugal dispersion, condensation.
A diameter of 60mm of first tantalum stick in step 1, the first end of the second tantalum stick stretches into argon gas protection atomization in step 3
Indoor length is less than the 1/3 of argon gas protection spray chamber length, and step 4 rotating speed of the second tantalum stick described in pulverizing process is
20000r/min。
Fig. 1 is the SEM figures of spherical tantalum powder prepared by the embodiment of the present invention, as can be seen that the shape of tantalum powder from Fig. 1
Rule, sphericity is higher, and spherical rate is 92%;The grain size of tantalum powder is 20 μm~130 μm, O=160ppm, C=in powder
90ppm, N=50ppm, H=13ppm.
Embodiment 2
Step 1: using electron beam melting processes by tantalum melting as the first tantalum stick of high-purity;
O=130ppm, C=90ppm, N=30ppm, H=12ppm in first tantalum stick.
Step 2: the first tantalum stick is passed through the second tantalum stick of mechanical processing diameter 60mmmm, length 400mm;
Step 3: the second end of the second pure tantalum stick is connected to electro spindle, first end stretches into argon gas protection spray chamber, with electricity
The second tantalum of main shaft drives stick high speed rotation in the horizontal direction;
Step 4: melt high speed rotation the second tantalum stick with the high-power equal arc of recess of 5000A fusion currents, the of the second tantalum stick
High ball form quotient tantalum powder is obtained after end face fusing and Centrifugal dispersion, condensation.
A diameter of 70mm of first tantalum stick in step 1, the first end of the second tantalum stick stretches into argon gas protection atomization in step 3
Indoor length is less than the 1/3 of argon gas protection spray chamber length, and step 4 rotating speed of the second tantalum stick in pulverizing process is
15000r/min。
Fig. 2 is the SEM figures of spherical tantalum powder prepared by the embodiment of the present invention, as can be seen that the shape of tantalum powder from Fig. 2
Rule, sphericity is higher, and spherical rate is 93%;The grain size of tantalum powder is 10 μm~130 μm, O=170ppm, C=in powder
95ppm, N=45ppm, H=15ppm.
Embodiment 3
Step 1: using electron beam melting processes by tantalum melting as the first tantalum stick of high-purity;
O=130ppm, C=80ppm, N=40ppm, H=10ppm in first tantalum stick.
Step 2: the first tantalum stick is passed through the second tantalum stick of mechanical processing diameter 55mm, length 350mm;
Step 3: the second end of the second pure tantalum stick is connected to electro spindle, first end stretches into argon gas protection spray chamber, with electricity
The second tantalum of main shaft drives stick high speed rotation in the horizontal direction;
Step 4: melt high speed rotation the second tantalum stick with the high-power equal arc of recess of 4500A fusion currents, the of the second tantalum stick
High ball form quotient tantalum powder is obtained after end face fusing and Centrifugal dispersion, condensation.
The first end of the second tantalum stick stretches into argon gas protection and is atomized indoor length less than argon gas protection spray chamber in step 3
The rotating speed of the 1/3 of length, step 4 second tantalum stick in pulverizing process is 18000r/min.
A diameter of 65mm of first tantalum stick in step 1, the first end of the second tantalum stick stretches into argon gas protection atomization in step 3
Indoor length is less than the 1/3 of argon gas protection spray chamber length, and step 4 rotating speed of the second tantalum stick described in pulverizing process is
15000r/min。
In conclusion an embodiment of the present invention provides a kind of preparation methods of tantalum powder, including:Tantalum melting is prepared into full
First tantalum stick of sufficient first condition, the first condition include:O≤150ppm, C≤100ppm, N≤50ppm, H≤12ppm;
The first tantalum stick is processed as diameter between 50mm~60mm, second tantalum stick of the length between 300mm~400mm;It will be described
The first end of second tantalum stick stretches into spray chamber, the electricity of the second end and plasma rotating electrode powder manufacturing apparatus of the second tantalum stick
Main shaft connects;The second tantalum stick forms tantalum powder by plasma rotating electrode powder manufacturing apparatus.The tantalum powder prepared by this method
Sphericity it is relatively high, wherein spherical rate can reach 90% or more, furthermore, the powder degree range of the tantalum powder ball is between 10~130
Between μm;It is low that other interstitial element contents such as oxygen content of the tantalum powder of powder are prepared by this method, are suitable for medical porous tantalum and are planted
Enter the preparation of material, further, applies also for increasing the personalization quickly manufacture that material technology carries out tantalum porous implant.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (6)
1. a kind of preparation method of tantalum powder, which is characterized in that including:
Tantalum item is prepared into the first tantalum stick for meeting first condition with electron-beam smelting, the first condition includes:O≤
150ppm, C≤100ppm, N≤50ppm, H≤15ppm;
The first tantalum stick is processed as diameter between 50mm~60mm, second tantalum stick of the length between 300mm~400mm;It will
The first end of the second tantalum stick stretches into spray chamber, second end and the plasma rotating electrode powder manufacturing apparatus of the second tantalum stick
Electro spindle connection;
The second tantalum stick forms tantalum powder by plasma rotating electrode powder manufacturing apparatus.
2. preparation method as described in claim 1, which is characterized in that the second tantalum stick passes through plasma rotating electrode powder
Equipment forms tantalum powder, specifically includes:
The second end face of second tantalum stick high speed rotation under electro spindle drive, the second tantalum stick is made in plasma arc
With lower fusing, and Centrifugal dispersion, the tantalum powder is formed after condensation.
3. preparation method as claimed in claim 2, which is characterized in that the electro spindle drives the second tantalum stick high speed rotation
Rotating speed between 15000r/min~20000r/min.
4. preparation method as claimed in claim 2, which is characterized in that the fusion current of the plasma arc between 4000A~
Between 5000A.
5. preparation method as described in claim 1, which is characterized in that the second tantalum stick stretches into the indoor length of atomization
Less than the 1/3 of the spray chamber length.
6. preparation method as described in claim 1, which is characterized in that diameter Jie 60mm~70mm of the first tantalum stick it
Between.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112620636A (en) * | 2020-12-15 | 2021-04-09 | 江门富祥电子材料有限公司 | Production method of high-pressure-resistant sheet-shaped tantalum powder |
CN116652198A (en) * | 2023-05-31 | 2023-08-29 | 西安建筑科技大学 | Method for preparing tantalum powder by gas atomization of plasma rotary electrode |
CN116652207A (en) * | 2023-05-31 | 2023-08-29 | 西安建筑科技大学 | Method for preparing metal tantalum by additive manufacturing |
-
2018
- 2018-06-26 CN CN201810665315.6A patent/CN108620598A/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112620636A (en) * | 2020-12-15 | 2021-04-09 | 江门富祥电子材料有限公司 | Production method of high-pressure-resistant sheet-shaped tantalum powder |
CN116652198A (en) * | 2023-05-31 | 2023-08-29 | 西安建筑科技大学 | Method for preparing tantalum powder by gas atomization of plasma rotary electrode |
CN116652207A (en) * | 2023-05-31 | 2023-08-29 | 西安建筑科技大学 | Method for preparing metal tantalum by additive manufacturing |
CN116652207B (en) * | 2023-05-31 | 2024-03-01 | 西安建筑科技大学 | Method for preparing metal tantalum by additive manufacturing |
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