CN109877343A - A kind of preparation method of the high-quality sized spherical titanium powder suitable for 3D printing - Google Patents
A kind of preparation method of the high-quality sized spherical titanium powder suitable for 3D printing Download PDFInfo
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Abstract
A kind of preparation method of the high-quality sized spherical titanium powder suitable for 3D printing, belongs to metal powder preparation technical field.Using average grain diameter for 1.5~2 μm of high pure metal titantium hydride micron powder is initial powder, then carries out agglomeration granulation and heat treatment to titantium hydride micron powder, obtains the fine grained micron order titanium powder with higher sphericity and certain bond strength；Radio frequency plasma nodularization finally is carried out to obtained micron order titanium powder, obtains the spherical pure titanium powder of fine grained that high-purity, full densification and high fluidity meet 3D printing requirement.Titanium powder particle of the present invention has high-purity, full compactness and high fluidity, and size tunable is strong；It is remarkably improved the consistency of prilling powder particle using micron order titanium hydride powders, and substantially reduces production cost；By radio frequency plasma spheronization techniques, purity, particle compactness and the mobility of final preparation titanium powder can be significantly improved.
Description
Technical field
The present invention relates to a kind of high-quality fine grained suitable for the high-purity of 3D printing, Quan Zhimi, high fluidity is spherical
The preparation method of titanium valve belongs to metal powder preparation technical field.
Background technique
Titanium in aerospace, is changed with its low-density, high specific strength, highly corrosion resistant and good biocompatibility
The fields such as work, petroleum industry and biomedicine are widely used.In recent years, with the rapid development of 3D printing technique,
It can effectively shorten the production cycle, produce the complicated shape part that conventional method is difficult to produce, research and development is suitable for
The high quality Spherical Ti Powder end technology of preparing of 3D printing obtains high-performance metal printout, causes domestic and international researcher couple
The interest in the field.However, pure titanium has high chemical activity, in 3D printing forming process, the presence of oxygen can reduce melt
Wetability, and the material (such as Fe, Cr element) containing oxytropism element usually cannot achieve formation of parts and densify entirely,
Therefore the control of its ingredient purity is the technological difficulties in titanium valve preparation process.On the other hand, since laser penetration depth is shallower,
When powder density or lower mobility, the density of powder bed is lower, and heating conduction is poor, and laser energy is difficult to the inside of bisque
Transmitting, on surface, accumulation can then cause powder to splash to a certain extent, increase the interference to laser, and make following table on bisque
Face temperature gradient significantly increases, and lower layer's powder particles fuse is incomplete, and Coating combination is poor, to reduce the densification of drip molding
Degree.Therefore the preparation of high-purity, high-compactness and high fluidity fine grained sized spherical titanium powder is to restrict 3D printing titanium or titanium alloy to produce
One of product popularization and the bottleneck element of application.
Gas atomization is to prepare the mainstream technology of titanium valve, by high pressure draught by metal bath it is broken dry obtain size compared with
Small powder particle.But the method easily forms satellite ball, hollow sphere etc. and seriously affects powder under high-strength airflow function
Consistency；And it is lower in the recovery rate of normal distribution and small sized particles (< 50 μm) to prepare powder particle size.Radio frequency plasma
Nodularization method is another preparation method for commonly using high sphericity powder, but powder particles fuse and cooling speed in this method
Fastly, there is certain limitation to the regulation of powder diameter.The patent of invention of Patent No. 201510159503.8 discloses one kind
The pure titanium with excellent sphericity and low oxygen content can be prepared in the preparation method of 3D printing fine grained sized spherical titanium powder
Belong to powder.The disadvantage of this method is that the large specific surface area of initial nanometer titanium hydride powders, adsorption gas content compared with
It is more, and nanometer powder volume contraction is larger after heat treatment, and it is lower that titanium valve apparent density is finally prepared；From the angle of preparation efficiency
Degree, nanometer powder preparation efficiency is lower, causes production cost higher.Therefore, pressing needs high-purity, high compactness and height at present
The novel preparation method of mobility, that is, high-quality 3D printing fine-grained metals titanium powder.
Summary of the invention
For above-mentioned domain background, in order to solve the limitation of the prior art, the present invention provides a kind of suitable for 3D printing skill
High-purity, the preparation method of Quan Zhimi fine grained sized spherical titanium powder of art.
The process flow of preparation method provided by the invention and principle are: using average grain diameter for 1.5~2 μm of High Purity Gold
Category titantium hydride micron powder is initial powder, then carries out agglomeration granulation and heat treatment to titantium hydride micron powder, is had
The fine grained micron order titanium powder of higher sphericity and certain bond strength；Radio frequency finally is carried out to obtained micron order titanium powder
Plasma spheroidization obtains the spherical pure titanium powder of fine grained that high-purity, full densification and high fluidity meet 3D printing requirement.We
For method compared with other processes, Titanium powder particle has high-purity, full compactness and high fluidity, and size tunable
By force；It is remarkably improved the consistency of prilling powder particle using micron order titanium hydride powders, and substantially reduces production cost；Pass through
Radio frequency plasma spheronization techniques can significantly improve the final purity and particle compactness for preparing titanium powder, smooth to acquisition surface,
The high quality printout of institutional framework densification has very important significance.
A kind of high-purity suitable for 3D printing provided by the invention, the preparation method of fully dense sized spherical titanium powder, it is special
Sign is, comprising the following steps:
(1) titanium hydride powders and polyethylene glycol and 2~3h of deionized water mixing and ball milling are obtained stablizing slurry, it is carried out
Centrifugal spray drying is atomized disk rotating speed by adjusting, and obtains partial size in 50 μm of spherical titanium hydride particles below, wherein feed hydrogen
Change the average grain diameter of titanium powder in 1.5~2 μ ms, the mass percentage of titanium hydride powders is 60~65% in slurry,
Polyethylene glycol is the 2.5~3.5% of titanium hydride powders quality, and atomization disk rotating speed is 15000~16000rpm；
(2) it is heat-treated, is used using the spherical titanium hydride particles that vacuum dewaxing-sintering furnace obtains step (1)
Stage heat treatment carries out degumming, dehydrogenation and densification consolidation；First stage completes degumming in vacuum environment, protects at 300 DEG C
50~60min of temperature；Second stage, in 900~950 DEG C of 90~120min of heat preservation, carries out a step titantium hydride point in vacuum environment
Solution and densification consolidation, finally obtain the fine grained micron-size spherical titanium powder with higher sphericity and certain bond strength；
(3) the fine grained micron-size spherical titanium powder that step (2) obtains is carried out using radio frequency plasma spheronization techniques etc.
Ion nodularization, using gas centered on argon gas of the purity not less than 99.9%, ionization forms stable high temperature inert gas etc.
Gas ions, throughput are preferably 1.0~2.0m3/h；Nitrogen using purity not less than 99.9%, will be former as delivery gas
Feed powder is sent into plasmatorch, and throughput is preferably 0.7~1.0m3/h；Nitrogen using purity not less than 99.9% is as cold
But gas, by melt cooled and solidified at spherical powder, throughput is preferably 0.7~5m3/h；Fine grained micron-size spherical titanium powder
Feed rate is 2~10g/min.
The preferred vacuum degree of vacuum environment is not less than 10-4The environment of Pa.
The technical characteristic and advantage of the method for the present invention mainly have: (1) preparing using pure titanium hydride powders as original material outstanding
Floating solution slurry, initial powder average grain diameter is in 1.5~2 μ ms, compared with the technique for using nano powder to be granulated, greatly
It reduces production cost greatly, improve production efficiency, and reducing the foreign gas content in prilling powder；(2) structure is used
The more stable easily prepared slurry for obtaining stable and uniform of polyethylene glycol and deionized water combination ball-milling technology, in vacuum environment
In, a step completes titantium hydride and decomposes and densify consolidation, and titanium hydride powders particle, which is easy to decompose completely, obtains pure titanium powder, and greatly
Manufacturing cycle is shortened greatly；(3) plasma spheroidization technology is used, metallic titanium powder particle occurs fusing rapidly and is quickly cooled down, easily
Surface is smooth and the spheric granules of uniform texture in obtaining, and low melting point element and small sized particles, which are easy to vaporize, to disappear
It loses, to substantially increase the mobility, purity and consistency for finally preparing titanium valve.
Detailed description of the invention
The pattern and individual particle surface topography of granulation titanium powder prepared by Fig. 1 embodiment of the present invention 1: wherein a is to be granulated
The scanning electron microscope shape appearance figure of micron-size spherical titanium hydride powders is obtained, b is to obtain single titanium valve after being granulated hydride powder heat treatment
The scanning electron microscope shape appearance figure of last particle.
The pattern for the single spherical titanium powder that Fig. 2 embodiment of the present invention 1 is finally prepared.
The pattern and particle diameter distribution for the spherical titanium powder that Fig. 3 embodiment of the present invention 2 is finally prepared: wherein a is preparation
The scanning electron microscope shape appearance figure of titanium powder, b are the particle diameter distribution statistical result for preparing titanium powder particle.
The two-dimensional section organization chart for the Titanium powder that Fig. 4 embodiment of the present invention 2 is finally prepared.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but the present invention is not limited to following embodiments.
Ingredient, consistency and the flowing for the Titanium powder particle that 1 Example 1 and Example 2 of the present invention of table is prepared
Property testing result.
Wherein the mobility and apparent density of metal powder use Hall flowmeter, according to ASTM B213-03 and ASTM
B212-99 standard test.
Vacuum as described below is 10-4The vacuum environment of Pa.
Embodiment 1, by average grain diameter be 1.5 μm pure hydride powder powder stock and 3.5% hydride powder quality poly- second
Glycol, deionized water are configured to the suspension slurry that titanium hydride powders content is 60%, and ball milling 2h obtains uniform and stable suspended
Liquid material slurry is carried out agglomeration granulation using centrifugal atomizing drying equipment, is granulated using the atomization disk rotating speed of 15000rpm, obtained
With high sphericity, titanium hydride particles of the partial size less than 50 μm；Using vacuum dewaxing-sintering furnace to the titantium hydride after granulation
Powder is heat-treated, and the first stage uses vacuum environment, and heat treatment temperature is 300 DEG C, soaking time 50min；Second stage
Using vacuum environment, 900 DEG C of heat treatment temperature, soaking time 120min, obtain that there is higher sphericity and certain bond strength
Fine grained micron order titanium powder；Using radio frequency plasma spheronization techniques, use purity for 99.9% argon gas centered on gas
Body, throughput 1.0m3/ h, the nitrogen that purity is 99.9% is as delivery gas, throughput 0.7m3/ h, purity 99.9%
Nitrogen as cooling gas, throughput 1m3/ h when powder feed rate is 2g/min, is prepared with high-purity, entirely
Fine and close and high fluidity fine grained titanium valve.The microstructure figure and particle diameter distribution statistical chart such as Fig. 1 for being granulated titanium valve is prepared,
The two-dimensional section organization chart such as Fig. 3 for the Titanium powder being finally prepared, ingredient and consistency testing result compare
It is shown in Table 1.
Embodiment 2, by average grain diameter be 1.5 μm pure hydride powder powder stock and 2.5% hydride powder quality poly- second
It is 65% suspension slurry that glycol, deionized water, which are configured to titanium hydride powders content, and ball milling 3h obtains uniform and stable suspension
Slurry is carried out agglomeration granulation using centrifugal atomizing drying equipment, is granulated, is had using the atomization disk rotating speed of 16000rpm
There are high sphericity, titanium hydride particles of the partial size less than 50 μm；Using vacuum dewaxing-sintering furnace to the hydride powder after granulation
End is heat-treated, and the first stage uses vacuum environment, and heat treatment temperature is 300 DEG C, soaking time 60min；Second stage is adopted
With vacuum environment, 950 DEG C of heat treatment temperature, soaking time 90min, obtain thin with higher sphericity and certain bond strength
Particle micron order titanium powder；Using radio frequency peak ion spheronization techniques, use purity for 99.9% argon gas centered on gas, gas
Flow is 2.0m3/ h, the nitrogen that purity is 99.9% is as delivery gas, throughput 1.0m3/ h, the nitrogen that purity is 99.9%
Gas is as cooling gas, throughput 5m3/ h when powder feed rate is 10g/min, is prepared with high-purity, full cause
Close and high fluidity fine grained titanium valve.The microstructure figure and particle diameter distribution statistical chart such as Fig. 2 of titanium valve, ingredient is prepared
1 is relatively shown in Table with consistency testing result.
The ingredient and consistency for the titanium powder that 1 Example 1 and Example 2 of the present invention of table is prepared
Claims (4)
1. a kind of high-purity suitable for 3D printing, the preparation method of Quan Zhimi fine grained sized spherical titanium powder, which is characterized in that including
Following steps:
(1) titanium hydride powders and polyethylene glycol and 2~3h of deionized water mixing and ball milling are obtained stablizing slurry, it is centrifuged
Spray drying is atomized disk rotating speed by adjusting, and obtains partial size in 50 μm of spherical titanium hydride particles below, wherein raw material titantium hydride
The average grain diameter of powder is in 1.5~2 μ ms, and the mass percentage of titanium hydride powders is 60~65% in slurry, poly- second
Glycol is the 2.5~3.5% of titanium hydride powders quality；
(2) it is heat-treated using the spherical titanium hydride particles that vacuum dewaxing-sintering furnace obtains step (1), using the stage
Formula heat treatment carries out degumming, dehydrogenation and densification consolidation；First stage completes degumming in vacuum environment, keeps the temperature 50 at 300 DEG C
~60min；Second stage is in vacuum environment, in 900~950 DEG C of 90~120min of heat preservation, carry out a step titantium hydride decompose and
Densification consolidation, finally obtains the fine grained micron-size spherical titanium powder with higher sphericity and certain bond strength；
(3) plasmasphere is carried out to the fine grained micron-size spherical titanium valve that step (2) obtains using radio frequency plasma spheronization techniques
Change, using gas centered on argon gas of the purity not less than 99.9%, ionization forms stable high temperature inert gas plasma；
Raw material powder is sent into plasmatorch by the nitrogen using purity not less than 99.9% as delivery gas；It is not less than using purity
99.9% nitrogen is as cooling gas, by melt cooled and solidified at spherical powder.
2. a kind of preparation of high-purity, Quan Zhimi fine grained sized spherical titanium powder suitable for 3D printing described in accordance with the claim 1
Method, which is characterized in that it is 15000~16000rpm that step (1), which is atomized disk rotating speed,.
3. a kind of preparation of high-purity, Quan Zhimi fine grained sized spherical titanium powder suitable for 3D printing described in accordance with the claim 1
Method, which is characterized in that argon flow is 1.0~2.0m3/ h, carrier gas flow are preferably 0.7~1.0m3/ h, cooling gas
Flow is preferably 0.7~5m3/ h, fine grained micron-size spherical titanium valve feed rate are 2~10g/min.
4. a kind of preparation of high-purity, Quan Zhimi fine grained sized spherical titanium powder suitable for 3D printing described in accordance with the claim 1
Method, which is characterized in that the preferred vacuum degree of vacuum environment is not less than 10-4The environment of Pa.
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