CN102554242A - Method for manufacturing micro-fine spherical titanium powder - Google Patents
Method for manufacturing micro-fine spherical titanium powder Download PDFInfo
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Abstract
The invention discloses a method for manufacturing micro-fine spherical titanium powder, which includes the steps: using sponge titanium as raw materials, mixing the sponge titanium with hydrogen, holding the positive pressure of the hydrogen at 0.05-0.1MPa, preserving heat at the temperature of 650-730 DEG C, and cooling after ensuring the sponge titanium and the hydrogen to sufficiently react; crushing the hydrogenated sponge titanium with an air-stream mill, controlling the revolving speed of the air-stream mill within 1000r/min-1300r/min, and obtaining titanium hydride powder with a grain size smaller than 45 micrometers by means of crushing; and dehydrogenizing and balling the titanium hydride powder by using radio frequency plasma. The method for manufacturing the micro-fine spherical titanium powder has the advantages that the grain size of the powder and grain size distribution can be effectively controlled, and the powder is low in oxygen content, few in production procedure, low in cost, high in balling rate, fine in sphericility and suitable for industrialized popularization.
Description
Technical field
The invention belongs to the powder process technical field, relate to a kind of manufacturing approach of superfine spherical titanium powder.
Background technology
Titanium or titanium alloy is the structural material of high-quality, and the good characteristic such as heat-resisting, anti-corrosion that has that density is little, specific strength is high and good has widely in fields such as automobile, chemical industry, metallurgy, environmental protection, Aeronautics and Astronautics and weapons and to use.Powder metallurgic method is one of important means of producing by titanium or titanium alloy block elements and part, has to organize tiny, composition and organize characteristics such as controlled.Yet in ti powder metallurgical industry, the preparation component evenly, consistent in density, defective is few, intensity is high, sphericity is high ti powder be very crucial.Simultaneously,, be prone to problems such as pollution, development, the especially development of ti powder injection molding technology of the long-term restriction of the difficulty ti powder metallurgical industry of superfine spherical titanium powder technology of preparing because Titanium is active high.Require starting powder that good sphericity not only will be arranged for the ti powder injection molding technique, and granularity should be less than 45um, the oxygen content of powder can not surpass 2000ppm.
At present, the preparation sized spherical titanium powder is main with aerosolization method, plasma rotating electrode method.The aerosolization method is with raw material titanium (titanium ingot or titanium sponge piece) heating and melting; Adopt the inert gas atomizer cooling then, the sized spherical titanium powder size distribution of this method preparation is very wide, and the powder sphericity is poor; Be difficult to the powder below the preparation 100um, and equipment investment and production run cost are all very high.And the ti powder of plasma rotating electrode method preparation has good sphericity, but the finished product rate is low, can only prepare the above thick spherical powder of 150um.Adopt these two kinds of methods to prepare the raw material that satisfies ti powder injection molding technology demand and objectively have technical difficulty.
In recent years, along with the development of heat plasma technology, its application in material preparation and process field has obtained the excellent popularization application, like aspects such as plasma spraying, plasma electroplating, plasma welding.The processing of plasma sphereization is the successful model of heat plasma at the powder preparation technical elements, adopts this technology can prepare pottery, refractory metal, active metal powder.At present, this technology has been used for preparing the research of superfine spherical titanium powder, be thermal source with the radio frequency plasma how, has also that to adopt direct current plasma be the research of the thermal source chamber of experimentizing.Basically all being starting powder enters hot-zone and the fusion of plasma through injector, melt granules balling-up under capillary effect, and cooling makes it keep spherical preferably fast in dropping process.This method can prepare the very high titanium spherical powder of sphericity, and the granularity of preparation sized spherical titanium powder receives the restriction of starting powder granularity, and the granularity of starting powder and size distribution have directly determined the granularity and the distribution situation thereof of final products.
Adopting radio frequency plasma to handle that prior art that material powder prepares sized spherical titanium powder all needs titanium sponge is pulverized or adopted the titanium valve after the dehydrogenation is raw material, selects different raw materials directly to determine the performance and the production cost of prepared powder.Because titanium sponge has good ductility and plasticity; Make titanium sponge be difficult to adopt conventional method to be pulverized; The crisp broken technology of low temperature that adopt come broken a small amount of titanium sponge to make an experiment more in the laboratory research; The grinding mode of this titanium sponge makes that the preparation technology of whole sized spherical titanium powder is with high costs, is difficult to carry out Industry Promotion.And with the titanium valve after the dehydrogenation as material powder, adopting the radio frequency plasma torch is thermal source when carrying out the preparation of sized spherical titanium powder, if the granularity of material powder can meet the demands (enough carefully), just can obtain the very thin sized spherical titanium powder of granularity.This is the preparation technology of raw material with the fine titanium powder, and the greatest problem of existence is that the product oxygen content is high, and preparation technology's oxygenation can't be avoided, and can not satisfy the instructions for use of injection molding technique.This is due to fine titanium powder surface area in dehydrogenation and shattering process increases, also be this be that the technology of feedstock production spherical powder is inevitable with the titanium valve.Simultaneously; The raw material of this preparation spherical powder adopts the hydrogenation dehydrogenating technology to obtain; Be the technology that initiation material prepares sized spherical titanium powder is compared with the titanium sponge, increased hydrogenation, fragmentation, dehydrogenation, broken operation once more, increase operation except meeting influences product purity; Production cost is increased, and this makes this difficult technique with industrial applications.
Summary of the invention
The manufacturing approach that the purpose of this invention is to provide a kind of superfine spherical titanium powder solves the prior art for preparing granularity less than the problem that 45um micro-sized spherical titanium powder cost is high, oxygen content is high, and production efficiency is high, is fit to suitability for industrialized production.
The technical scheme that the present invention adopted is, the manufacturing approach of superfine spherical titanium powder is specifically carried out according to following steps:
The hydrogenation treatment of step 1 titanium sponge
With the titanium sponge is raw material, and titanium sponge is mixed with hydrogen, keeps hydrogen malleation 0.05MPa-0.1MPa, 650 ℃ of-730 ℃ of insulations, guarantees that titanium sponge and hydrogen fully react back cooling cooling;
Step 2 break process
Adopt airflow milling to carry out fragmentation the titanium sponge after step 1 hydrogenation, the rotating speed of airflow milling is controlled at 1000r/min-1300r/min, and fragmentation obtains the titanium hydride powders of granularity less than 45um;
Step 3 dehydrogenation and spheroidising
The granularity that step 2 is made as raw material, adopts radio frequency plasma to carry out dehydrogenation and spheroidising less than the titanium hydride powders of 45um, promptly obtains the superfine spherical titanium powder.
Characteristic of the present invention also is,
Following steps are specifically adopted in the dehydrogenation of step 3 and spheroidising: adopt argon gas as plasma gas, i.e. and working gas, the radio frequency plasma power output is 60kw-85kw; Protective gas and working gas use argon gas, and the protection throughput is chosen in 0.7m
3/ h-1.5m
3/ h, the working gas flow is chosen in 0.4m
3/ h-1.0m
3/ h makes to form stable plasmatorch; Adopt argon gas hydride powder to be delivered to plasmatorch central authorities then as carrier gas; The rate selection of sending titanium hydride powders is at 30g/min-300g/min; Hydride powder is process plasmatorch melted by heating globulate in dropping process; And in the protection deposit of argon gas in collecting tank, promptly get the superfine spherical titanium powder.
The preparation method of superfine spherical titanium powder of the present invention is initiation material with the titanium sponge, after titanium sponge and hydrogen at high temperature react, and the titantium hydride of production fragility; Titantium hydride carries out the fine powder that fragmentation obtains the granularity that requires, and is that carrier gas is directly sent into radio frequency plasma torch central authorities and carried out spheroidising with the argon gas with the fine hydride powder that obtains, and fine hydride powder receives high temperature and fusion in the radio frequency plasma torch; Molecular scission between titanium and the hydrogen and make titantium hydride be decomposed into the free state of titanium and hydrogen; Reach the purpose of dehydrogenation, the titanium of free state and hydrogen are because the proportion deviation is very big, and titanium can be fallen by the deadweight effect; Thereby separate with hydrogen; Titanium receives the cold by force of refrigerating gas in dropping process, under capillary effect, be frozen into sphere and reduce free energy, forms stable sized spherical titanium powder end.This invented technology had both been avoided the fragmentation of titanium sponge, had reduced the dehydrogenation operation again, had realized the combination of dynamic De-hydrogen Technology and spheroidising technology, and production process is reduced, and will inevitably reduce production costs greatly.Simultaneously, exist because attritive powder before carrying out spheroidising is a irregular form with titantium hydride, titantium hydride can not receive pollution and the oxygenation of air.And the powder after spheroidising is perfect spherical powder; The not enough same grade (45um) 1/10th of the irregular material powder of pattern of specific area; Little specific area improves spherical powder stability greatly, is not vulnerable to the pollution of element such as oxygen, nitrogen in the air.Technology of the present invention compared with prior art also has the following advantages:
1, the granularity of prepared titanium minute spherical powder and size distribution can effectively be controlled.
2, prepared micro-sized spherical titanium powder (granularity is less than 45um) oxygen content is low, is no more than 0.20wt%.
3, the production process of technology of the present invention is few, cost is low, the nodularization rate high, is fit to industrialization promotion.
4, prepared powder has good sphericity, the powder property high conformity.
Description of drawings
The ball-type ti powder photo of Fig. 1 for adopting existing aerosolization to make.
The ball-type ti powder photo of Fig. 2 for adopting the inventive method to make.
The specific embodiment
Through the specific embodiment the present invention is elaborated below.
The manufacturing approach of superfine spherical titanium powder of the present invention, specifically implement according to following steps:
The hydrogenation treatment of step 1 titanium sponge
With the titanium sponge is raw material, and titanium sponge is mixed with hydrogen, keeps hydrogen malleation 0.05MPa-0.1MPa, 650 ℃ of-730 ℃ of insulations, guarantees that titanium sponge and hydrogen fully react back cooling cooling;
Step 2 break process
Adopt airflow milling to carry out fragmentation the titanium sponge after step 1 hydrogenation, the rotating speed of airflow milling is controlled at 1000r/min-1300r/min, and fragmentation obtains the titanium hydride powders of granularity less than 45um;
Step 3 dehydrogenation and spheroidising
The granularity that step 2 is made as raw material, adopts radio frequency plasma to carry out dehydrogenation and spheroidising less than the titanium hydride powders of 45um;
Be specifically with argon gas as plasma gas (being working gas), the radio frequency plasma power output can be adjusted at 60kw-85kw; Protective gas and working gas use argon gas, and the protection throughput is chosen in 0.7m
3/ h-1.5m
3/ h, the working gas flow is chosen in 0.4m
3/ h-1.0m
3/ h makes to form stable plasmatorch; Adopt argon gas hydride powder to be delivered to plasmatorch central authorities then as carrier gas; Powder feeding rate is chosen in 30g/min-300g/min; Hydride powder is process plasmatorch melted by heating globulate in dropping process; And in the protection deposit of argon gas in collecting tank, obtain fine sized spherical titanium powder end.
Performance evaluation and evaluation
Spherical powder with after handling carries out the analysis of granularity and chemical composition.Owing to do not introduce any impurity element in the whole process flow of this technology, has only the variation of protium in the product, so general of the micro-sized spherical titanium powder of production needs measure oxygen, nitrogen and hydrogen content just passable; Analytical element oxygen, nitrogen mainly are the serviceabilities that very easily influences it owing to titanium with airborne oxygen and the stable compound of nitrogen reacted.
Crucial in the technology of preparing of the present invention is spheroidising and the synchronous completion of hydride powder dehydrogenation, the preparation of fine titantium hydride, the selection of plasma parameter.Varigrained hydride powder needs article on plasma body parameter suitably to adjust, and to guarantee obtaining perfect spheric granules, titantium hydride is decomposed, and reaches the purpose of dehydrogenation.
Draw through experiment; Powder feeding (hydride powder) speed increases, and the powder concn in the gas-solid mixture increases, also increase greatly of the chance of collision each other between the titanium drop of fusion; The also corresponding increase of the particle diameter of the powder particle of the gained that makes is so powder feed rate need be controlled at 30g/min-300g/min.
Embodiment 1
With the titanium sponge is raw material, and titanium sponge is mixed with hydrogen, keeps hydrogen malleation 0.05MPa; 650 ℃ of insulations; Adopt airflow milling to carry out fragmentation the titanium sponge after the hydrogenation, the rotating speed of airflow milling is controlled at 1000r/min, and fragmentation obtains the titanium hydride powders of granularity less than 45um; Selecting average grain diameter is the titanium hydride powders of 17um, adopts radio frequency plasma to carry out dehydrogenation and spheroidising; Radio frequency plasma power output 60kw; Protective gas and working gas etc. all use argon gas, and the protection throughput is chosen in 0.7m
3/ h, the working gas flow is chosen in 0.4m
3/ h; Adopt argon gas as carrier gas hydride powder to be delivered to plasmatorch central authorities then, powder feeding rate is chosen in 30g/min, and hydride powder is process plasmatorch melted by heating globulate in dropping process; And in the protection deposit of inert gas in collecting tank, obtain fine sized spherical titanium powder end.
The spherical powder analysis result for preparing is: spherical rate 99%, oxygen content 0.13wt%, hydrogen content 0.018wt%, nitrogen content 0.015wt%, particle mean size 14um.
Embodiment 2
With the titanium sponge is raw material, and titanium sponge is mixed with hydrogen, keeps hydrogen malleation 0.1MPa; 730 ℃ of insulations; Adopt airflow milling to carry out fragmentation the titanium sponge after the hydrogenation, the rotating speed of airflow milling is controlled at 1300r/min, and fragmentation obtains the titanium hydride powders of granularity less than 45um; Selecting average grain diameter is the titanium hydride powders of 45um, adopts radio frequency plasma to carry out dehydrogenation and spheroidising; Radio frequency plasma power output 85kw; Protective gas and working gas etc. all use argon gas, and the protection throughput is chosen in 1.5m
3/ h, the working gas flow is chosen in 1.0m
3/ h; Adopt argon gas as carrier gas hydride powder to be delivered to plasmatorch central authorities then, powder feeding rate is chosen in 300g/min, and hydride powder is process plasmatorch melted by heating globulate in dropping process; And in the protection deposit of inert gas in collecting tank, obtain fine sized spherical titanium powder end.
The spherical powder analysis result for preparing is: spherical rate 99%, oxygen content 0.12wt%, hydrogen content 0.02wt%, nitrogen content 0.012wt%, particle mean size 42um.
Embodiment 3
With the titanium sponge is raw material, and titanium sponge is mixed with hydrogen, keeps hydrogen malleation 0.08MPa; 7300 ℃ of insulations; Adopt airflow milling to carry out fragmentation the titanium sponge after the hydrogenation, the rotating speed of airflow milling is controlled at 1150r/min, and fragmentation obtains the titanium hydride powders of granularity less than 45um; Selecting average grain diameter is the titanium hydride powders of 36um, adopts radio frequency plasma to carry out dehydrogenation and spheroidising; Radio frequency plasma power output 70kw; Protective gas and working gas etc. all use argon gas, and the protection throughput is chosen in 1.0m
3/ h, the working gas flow is chosen in 10.7m
3/ h; Adopt argon gas as carrier gas hydride powder to be delivered to plasmatorch central authorities then, powder feeding rate is chosen in 100g/min, and hydride powder is process plasmatorch melted by heating globulate in dropping process; And in the protection deposit of inert gas in collecting tank, obtain fine sized spherical titanium powder end.
The spherical powder analysis result for preparing is: spherical rate 99%, oxygen content 0.11wt%, hydrogen content 0.016wt%, nitrogen content 0.010wt%, particle mean size 32um.
The spherical powder pattern that adopts embodiment 3 to prepare is as shown in Figure 2; As shown in Figure 1 with the existing photo of the spherical powder that aerosolization makes that adopts, compare and can find out, the powder that adopts the inventive method to make has good sphericity; The powder property high conformity, and granularity is little.
Claims (2)
1. the manufacturing approach of a superfine spherical titanium powder is characterized in that, specifically implements according to following steps:
The hydrogenation treatment of step 1 titanium sponge
With the titanium sponge is raw material, and titanium sponge is mixed with hydrogen, keeps hydrogen malleation 0.05MPa-0.1MPa, 650 ℃ of-730 ℃ of insulations, guarantees that titanium sponge and hydrogen fully react back cooling cooling;
Step 2 break process
Adopt airflow milling to carry out fragmentation the titanium sponge after step 1 hydrogenation, the rotating speed of airflow milling is controlled at 1000r/min-1300r/min, and fragmentation obtains the titanium hydride powders of granularity less than 45um;
Step 3 dehydrogenation and spheroidising
The granularity that step 2 is made as raw material, adopts radio frequency plasma to carry out dehydrogenation and spheroidising less than the titanium hydride powders of 45um, promptly obtains the superfine spherical titanium powder.
2. according to the manufacturing approach of the described superfine spherical titanium powder of claim 1; It is characterized in that; Following steps are specifically adopted in the dehydrogenation of said step 3 and spheroidising: adopt argon gas as plasma gas, i.e. and working gas, the radio frequency plasma power output is 60kw-85kw; Protective gas and working gas use argon gas, and the protection throughput is chosen in 0.7m
3/ h-1.5m
3/ h, the working gas flow is chosen in 0.4m
3/ h-1.0m
3/ h makes to form stable plasmatorch; Adopt argon gas hydride powder to be delivered to plasmatorch central authorities then as carrier gas; The rate selection of sending titanium hydride powders is at 30g/min-300g/min; Hydride powder is process plasmatorch melted by heating globulate in dropping process; And in the protection deposit of argon gas in collecting tank, promptly get the superfine spherical titanium powder.
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