CN104772473A - Preparation method of fine-particle spherical titanium powder for three-dimensional (3D) printing - Google Patents
Preparation method of fine-particle spherical titanium powder for three-dimensional (3D) printing Download PDFInfo
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Abstract
The invention discloses a preparation method of fine-particle spherical titanium powder for three-dimensional (3D) printing and belongs to the technical field of preparation of metal powder. The method comprises the following steps: firstly, by using a high-purity titanium block material as a raw material, performing arc evaporation under an inert gas environment, and meanwhile, charging hydrogen to synthesize titanium hydride nano powder through a gas-phase reaction; secondly, agglomerating and granulating the titanium hydride nano powder to obtain micron-sized titanium hydride powder with higher density; finally, performing heat treatment on the granulated micron-sized titanium hydride powder, and performing degumming, dehydrogenation and compacted consolidation to obtain pure-titanium powder particles of which the particle size, the sphericity and the fluidity meet a 3D printing requirement. According to the method, the sphericity and the particle size distribution of the titanium powder particles are highly controlled; the process is simple, and the cost is low; metal titanium with great activity is stabilized in a new way of generating oxidation-resistant titanium hydride nano powder particles firstly, and the content of oxygen in the titanium powder particles which are finally prepared can be controlled.
Description
Technical field
The present invention relates to a kind of preparation method of 3D printing fine grained sized spherical titanium powder, belong to metal powder preparation technical field.
Background technology
3D printing technique is particularly suitable for developing high added value complex structure product, personalized customization and the link such as checking of design and R&D before being applied to large-scale production.Compared with current international most advanced level, in the research and development of moulding material needed for China prints at 3D, still there is a big difference, and design of material and preparation technology mainly follow the tracks of foreign progress at present.In 3D printing with in moulding material product, the almost complete dependence on import such as domestic required fine grain spherical titanium and titanium alloy powder.The shortage of high-quality 3D printing moulding material is one of bottleneck key element of restriction China 3D printing technique propagation and employment.
For 3D printing fine-grained metals titanium powder, technical process has very high requirement to dusty material, as particle size range 20-50 micron, high sphericity, low oxygen content etc.Existing titanium valve technology of preparing mainly contains: electrochemical process, mechanical attrition method, atomization, reducing process etc.The titanium that these methods current are prepared or titanium alloy powder pattern are difficult to control, and particle diameter is thicker and distribution is wider.Wherein, gas atomization is lower due to air velocity, and the yield rate that the metal or alloy powder size prepared reaches less than 50 μm only has about 30% usually; Electrochemistry, reducing process cost are higher, and the solvent used and reducing agent have severe toxicity more, and easily introduce the impurity such as halogen, sulphur; Ball-milling method can only be used for fragile material, the higher and uncontrollable powder particle pattern of usual oxygen content.Therefore, the preparation method of the 3D printing metal or alloy powder of current pressing needs low cost, high-purity, size tunable.
For above-mentioned domain background, in order to solve the limitation of prior art, the invention provides a kind of preparation method being applicable to the fine grained sized spherical titanium powder of 3D printing technique.
Summary of the invention
Technological process and the principle of preparation method provided by the invention are: adopt high pure metal titanium bulk to be raw material, in an inert atmosphere arc evaporation, be filled with hydrogen simultaneously, by the synthesizing hydrogenated nano-ti powder end of gas-phase reaction; Then agglomeration granulation is carried out to titantium hydride nanometer powder, obtain the micron order titanium hydride powders of higher density; Finally micron order titanium hydride powders after granulation is heat-treated, by coming unstuck, dehydrogenation and densified consolidation, obtaining granularity, sphericity and mobility and meeting 3D and print the pure titanium powder particle required.This method compared with other processes, to the sphericity of metallic particles and the controllability of domain size distribution strong; Technique is simple, cost is low; By first generating the new way of sludge proof titantium hydride nanometer powder, stable have greatly active Titanium, effectively can control the oxygen content in the metal powder granulates of final preparation.
A kind of preparation method being applicable to the fine grained sized spherical titanium powder of 3D printing demand provided by the invention, is characterized in that, comprise the following steps:
(1) using high purity titanium bulk as anode, under inert gas argon gas or helium environment, high intensity electric arc is formed by discharge process, striking current is 100 ~ 250A, arc voltage is 10 ~ 30V, then pass into hydrogen, the volume ratio of hydrogen and inert gas is 1:(1 ~ 3), generate titantium hydride (TiH by gas-phase reaction
2), form solid-state titantium hydride nano particle after condensation;
(2) titantium hydride nano particle prepared by polyvinyl alcohol, polyethylene glycol and deionized water and step (1) is mixed with suspension slip, after agglomeration granulation, obtains the spherical titanium hydride particles of 20 ~ 50 μm;
(3) after the granulation adopting the tube furnace of argon shield to prepare step (2), spherical titanium hydride particles is heat-treated, and first stage heat treatment temperature is 230 ~ 280 DEG C, and temperature retention time is 60 ~ 120min; Second stage heat treatment temperature is 700 ~ 750 DEG C, and temperature retention time is 120 ~ 180min; Phase III heat treatment temperature is 900 ~ 950 DEG C, and temperature retention time is 60 ~ 90min, finally cools to room temperature with the furnace, obtains the fine grained micron-size spherical titanium powder with high compactness, high fluidity, low oxygen content.
Technical characteristic of the present invention and advantage mainly contain: in the process that (1) evaporates in the starting the arc of titanium bulk, be filled with hydrogen, at high temperature hydrogen and metal gas react rapidly, the titantium hydride that product is mutually pure, utilize the regulation and control of striking current, voltage and hydrogen and inert gas ratio, productive rate and the particle size of titantium hydride can be adjusted, make average grain diameter controlled within the scope of 30 ~ 80nm; (2) with the titanium hydride powders of good stability for original material, utilize the method granulations such as centrifugal spray, effectively can control the introducing of the impurity such as oxygen in granulation process, obtain good sphericity and higher micron particles density simultaneously; (3) Technology for Heating Processing after granulation, the metal dust final acquisition being met to 3D printing requirement is extremely important.In the present invention, adopt three stage heat treatment regimens, first stage heat treated effect is the organic binder bond volatilization making to add in granulation process; The heat treated effect of second stage titantium hydride is decomposed completely obtain Titanium; Phase III heat treated effect makes to form solid phase bonding between titanium powder particle, both ensured to have enough interparticle bond strength and density, particle (or internal microstructure) alligatoring or integral sintered fast does not occur again.The present invention by the parameters combination of each processing step of regulation and control, can prepare there is excellent sphericity, high fluidity and average grain diameter and domain size distribution meet 3D and print the high-quality fine grained spherical titanium metal dust required.Especially, by first generating the new way of sludge proof titantium hydride nano-powder particles, stable have greatly active Titanium, effectively can control the oxygen content in the titanium powder particle of final preparation, and whole piece syntheti c route technique simple, be easy to operation, the preparation method of other pure titanium micron powders comparatively existing greatly reduces cost.
Accompanying drawing explanation
The thing of nanometer titanium hydride powders prepared by Fig. 1 embodiment of the present invention 1 detects collection of illustrative plates mutually.
The microstructure of nanometer titanium hydride powders, crystal structure and domain size distribution prepared by Fig. 2 embodiment of the present invention 2; Wherein a is the high power transmission electron microscope shape appearance figure of nanometer titanium hydride powders, and b is the SEAD collection of illustrative plates of nanometer titanium hydride powders particle, and c is the domain size distribution statistics of nanometer titanium hydride powders particle.
The thing of the titanium powder that Fig. 3 embodiment of the present invention 1 prepares detects collection of illustrative plates mutually.
The microstructure of the titanium powder particle that Fig. 4 embodiment of the present invention 2 prepares and domain size distribution; Wherein a is the ESEM shape appearance figure of titanium powder, and b is the high power shape appearance figure of single titanium particle, and c is the domain size distribution statistics of titanium powder particle.
The sphericity of the Titanium powder particle that table 1 embodiment of the present invention 1 and embodiment 2 prepare, mobility and Density Detection result.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but the present invention is not limited to following examples.
Example 1, using raw material high purity titanium bulk (purity 99.99wt%) as anode, under inert gas ar gas environment, high intensity electric arc is formed by discharge process, striking current is 100A, arc voltage is 10V, then pass into hydrogen, the ratio of hydrogen and inert gas is 1:1, generates titantium hydride (TiH by gas-phase reaction
2), form solid-state titantium hydride nano particle after condensation, as Fig. 1; Polyvinyl alcohol, polyethylene glycol and deionized water and titantium hydride nano particle are mixed with suspension slip, utilize centrifugal atomizing drying means to carry out agglomeration granulation, obtain the spherical titanium hydride particles of 20 μm; Adopt the tube furnace of argon shield to heat-treat the titanium hydride powders after granulation, first stage heat treatment temperature is 230 DEG C, temperature retention time 120min; Second stage heat treatment temperature is 700 DEG C, and temperature retention time is 180min; Phase III heat treatment temperature is 900 DEG C, and temperature retention time is 90min, finally cools to room temperature with the furnace, obtains the fine grained micron-size spherical titanium powder with high compactness, high fluidity, low oxygen content.The titanium valve thing prepared detects collection of illustrative plates mutually as Fig. 3, and its sphericity, apparent density, mobility and measurement of oxygen content the results are shown in Table 1.
Example 2, using raw material high purity titanium bulk (purity 99.99wt%) as anode, under inert gas helium environment, high intensity electric arc is formed by discharge process, striking current is 250A, arc voltage is 30V, then pass into hydrogen, the ratio of hydrogen and inert gas is 1:3, generates titantium hydride (TiH by gas-phase reaction
2), form solid-state titantium hydride nano particle after condensation, its microstructure and domain size distribution are as Fig. 2; Polyvinyl alcohol, polyethylene glycol and deionized water and titantium hydride nano particle are mixed with suspension slip, utilize centrifugal atomizing drying means to carry out agglomeration granulation, obtain the spherical titanium hydride particles of 50 μm; Adopt the tube furnace of argon shield to heat-treat the titanium hydride powders after granulation, first stage heat treatment temperature is 280 DEG C, temperature retention time 90min; Second stage heat treatment temperature is 750 DEG C, and temperature retention time is 120min; Phase III heat treatment temperature is 950 DEG C, and temperature retention time is 60min, finally cools to room temperature with the furnace, obtains the fine grained micron-size spherical titanium powder with high compactness, high fluidity, low oxygen content.The titanium valve microstructure prepared and domain size distribution are as Fig. 4, and its sphericity, apparent density, mobility and measurement of oxygen content the results are shown in Table 1.
The physical parameter of the titanium powder that table 1 embodiment of the present invention 1 and embodiment 2 prepare
Claims (2)
1. be applicable to the preparation method that 3D prints the fine grained sized spherical titanium powder of demand, it is characterized in that, comprise the following steps:
(1) using high purity titanium bulk as anode, under inert gas argon gas or helium environment, high intensity electric arc is formed by discharge process, striking current is 100 ~ 250A, arc voltage is 10 ~ 30V, then pass into hydrogen, the volume ratio of hydrogen and inert gas is 1:(1 ~ 3), generate titantium hydride (TiH by gas-phase reaction
2), form solid-state titantium hydride nano particle after condensation;
(2) titantium hydride nano particle prepared by polyvinyl alcohol, polyethylene glycol and deionized water and step (1) is mixed with suspension slip, carries out agglomeration granulation, obtain the spherical titanium hydride particles of 20 ~ 50 μm;
(3) after the granulation adopting the tube furnace of argon shield to prepare step (2), spherical titanium hydride particles is heat-treated, and first stage heat treatment temperature is 230 ~ 280 DEG C, and temperature retention time is 60 ~ 120min; Second stage heat treatment temperature is 700 ~ 750 DEG C, and temperature retention time is 120 ~ 180min; Phase III heat treatment temperature is 900 ~ 950 DEG C, and temperature retention time is 60 ~ 90min, finally cools to room temperature with the furnace, obtains the fine grained micron-size spherical titanium powder with high compactness, high fluidity, low oxygen content.
2. be applicable to according to a kind of of claim 1 preparation method that 3D prints the fine grained sized spherical titanium powder of demand, it is characterized in that, utilize the regulation and control of step (1) striking current, voltage and hydrogen and inert gas ratio, the productive rate of adjustment nanometer titanium hydride powders particle and particle size, make average grain diameter within the scope of 30 ~ 80nm.
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| CN105499605A (en) * | 2015-12-08 | 2016-04-20 | 南通金源智能技术有限公司 | Preparation method of spherical titanium powder for 3D printing |
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| CN106334791A (en) * | 2016-10-24 | 2017-01-18 | 贵州省钛材料研发中心有限公司 | Production method of spherical titanium powder for 3D printing |
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