CN103406543A - Ultrafine titanium powder or titanium alloy powder and production method and device thereof - Google Patents

Ultrafine titanium powder or titanium alloy powder and production method and device thereof Download PDF

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CN103406543A
CN103406543A CN2013103285323A CN201310328532A CN103406543A CN 103406543 A CN103406543 A CN 103406543A CN 2013103285323 A CN2013103285323 A CN 2013103285323A CN 201310328532 A CN201310328532 A CN 201310328532A CN 103406543 A CN103406543 A CN 103406543A
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titanium
titanium powder
centrifugal atomizing
powder
purification ultrafine
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CN103406543B (en
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何安西
苗庆东
张继东
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Abstract

The invention discloses a production method of ultrafine titanium powder or titanium alloy powder. The method includes the steps: melting titanium or titanium alloy material into titanium melt or titanium alloy melt; subjecting the titanium melt or titanium alloy melt to primary centrifugal atomization; after primary centrifugal atomization, subjecting the titanium melt or titanium alloy melt to secondary centrifugal atomization; collecting titanium powder or titanium alloy powder obtained by the primary and secondary centrifugal atomization and cooling so as to obtain ultrafine titanium powder or titanium alloy powder. The steps are performed in the atmosphere of an insert gas. The ultrafine titanium powder or titanium alloy powder is produced by the production method. An ultrafine metal powder production device is used for implementing the production method. The production method is high in production efficiency and low in energy consumption; the titanium powder or titanium alloy powder produced by the production method is spheres or similar spheres and is low in oxygen content, high in density, fine in mobility and low in fineness.

Description

Purification ultrafine titanium powder or Titanium Powder and preparation method thereof, device for making
Technical field
The invention belongs to powder metallurgical technology, more particularly, relate to a kind of purification ultrafine titanium powder or Titanium Powder and preparation method thereof, device for making.
Background technology
Titanium or titanium alloy is the excellent properties such as density is little, specific strength is high, acid-alkali-corrosive-resisting owing to having, be widely used in Aero-Space, derived energy chemical, medicine equipment, metallurgy and each field such as civilian, but because the processing of titanium or titanium alloy product is complicated, lumber recovery is low, in the process of manufacturing parts, produce a large amount of titanium waste materials, during consumption energy consumption, manufacturing cost is high, makes it be difficult to be applied widely.
Obtain in recent years the powder metallurgy of greatly developing, injection moulding and 3D printing technique etc., make the large much progress of forming technique of part, produce less or without waste cut materials, improved the utilization rate of material, reduced production cost, especially the parts manufacture of complicated shape had more to advantage, market application foreground is widely arranged.Because titanium is at high temperature active to the height parent of oxygen, nitrogen, carbon, make the difficulty of the titanium valve of producing high-purity low-oxygen content or Titanium Powder very large, particularly be applicable to the superfine spherical powder of injection moulding and 3D printing-forming especially without the volume production product, thereby limited the extensive use of titanium or titanium alloy product.
The production method of metallic titanium powder mainly contains: electrolysis, hydrodeoxygenation method, ultrasonic aerosolization method, plasma rotating electrode method etc., but all come with some shortcomings, greatly limited production and the extensive use of titanium or titanium alloy powder.Wherein, the production efficiency of electrolysis is low, the poor fluidity of powder particle, and generally can not be for the production of alloyed powder; The product oxygen content of hydrogenation and dehydrogenization method is high, powder particle is cerioid, poor fluidity, dehydrogenation time is long and efficiency is low; Ultrasonic aerosolization method need to consume the aniseed argon gas, once becomes the powder qualification rate low, and compressor horsepower is large and powder is generally thicker; The plasma rotating electrode method is had relatively high expectations to electrode specification, and friction feeding is poor, and powder particle is more slightly used.
At present, the centrifugal atomizing method is the common method of producing metal dust, because of its economical rationality, output is large, equipment manufacturing cost is low, energy consumption is low, production efficiency is high is widely used.But existing centrifugal atomization apparatus is pulverized molten metal bath in the mode that high-speed electric expreess locomotive drives the centrifugal pan High Rotation Speed of minor diameter usually, more than the rotating speed of centrifugal pan main shaft will reach 30000r/min usually, therefore existing centrifugal atomizing method and device can not be for the production of dystectic metal dust such as titanium valves, can only be metal dust below 500 ℃ such as aluminium powder, copper powder for the preparation of fusing point.
Therefore, need preparation method and the device for making that provides that a kind of technique is simple, technology is reliable, energy consumption is low and can produce purification ultrafine titanium powder or Titanium Powder badly.
Summary of the invention
For the deficiencies in the prior art, one of purpose of the present invention is to solve in above-mentioned prior art the one or more problems that exist.
The object of the invention is to overcome prior art particularly plasma rotating electrode method, ultrasonic aerosolization method and centrifugal atomizing law technology produce in existing deficiency, and then provide that a kind of technique is simple, technology reliable, product granularity is easy to control, energy consumption is low, production efficiency is high purification ultrafine titanium powder or the preparation method of Titanium Powder and centrifugal atomizing titanium valve or the centrifugal atomizing Titanium Powder of being produced by the method.
To achieve these goals, an aspect of of the present present invention provides the preparation method of a kind of purification ultrafine titanium powder or Titanium Powder, said method comprising the steps of: titanium or titanium alloy raw material are molten into to titanium liquid or titanium alloy liquid; Described titanium liquid or titanium alloy liquid are carried out to centrifugal atomizing one time by the first centrifugal atomizing dish rotated; Again the titanium drop after a centrifugal atomizing or titanium alloy drop are carried out to the secondary centrifuging atomization by the second centrifugal atomizing dish rotated; Collection obtains purification ultrafine titanium powder or Titanium Powder through twice centrifugal atomizing cooled titanium valve or Titanium Powder, and wherein, above each step is all carried out under inert gas atmosphere.
The preparation method of purification ultrafine titanium powder or Titanium Powder embodiment according to the present invention, the diameter of described the first centrifugal atomizing dish is Φ 30~70mm, rotating speed is 5000~15000r/min; The diameter of described the second centrifugal atomizing dish is Φ 80~120mm, and rotating speed is 15000~25000r/min.
The preparation method of purification ultrafine titanium powder or Titanium Powder embodiment according to the present invention, described method also comprises removes described titanium or the oxide on surface of titanium alloy raw material and the pre-treatment step of impurity.
The preparation method of purification ultrafine titanium powder or Titanium Powder embodiment according to the present invention, described method also comprises the step to sieving and/or pack through twice atomization cooled titanium valve or Titanium Powder.
The preparation method of purification ultrafine titanium powder or Titanium Powder embodiment according to the present invention, will carry out atomization after the titanium liquid after fusing or overheated 30~150 ℃ of titanium alloy liquid again.
The preparation method of purification ultrafine titanium powder or Titanium Powder embodiment according to the present invention, described inert gas is argon gas, helium, the pressure of inert gas atmosphere is greater than 30Pa and oxygen content is less than 0.1%.
Another aspect of the present invention also provides a kind of purification ultrafine titanium powder or Titanium Powder, and described purification ultrafine titanium powder or Titanium Powder are that the preparation method by above-mentioned purification ultrafine titanium powder or Titanium Powder makes.
Purification ultrafine titanium powder or Titanium Powder embodiment according to the present invention, described purification ultrafine titanium powder or Titanium Powder are spherical in shape or class is spherical, and by weight percentage, the described titanium valve more than 90% or the granularity of Titanium Powder are less than 45 μ m; The oxygen content of described purification ultrafine titanium powder is less than 0.1%, and the oxygen content of ultra-fine Titanium Powder is less than 0.15%.
The device for making that a kind of purification ultrafine titanium powder or Titanium Powder are provided on the one hand again of the present invention, described device for making is for implementing the preparation method of above-mentioned purification ultrafine titanium powder or Titanium Powder.
An embodiment according to the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder, described device for making comprises melting unit, the first centrifugal atomizing unit, the second centrifugal atomizing unit, aggregate tube and protective cover, wherein, described melting unit, the first centrifugal atomizing unit, the second centrifugal atomizing unit, aggregate tube all are arranged in protective cover, on protective cover, are provided with gas access and gas vent; Described melting unit comprises melting furnace and carrier pipe, and described carrier pipe is for being delivered to the first centrifugal atomizing unit by the titanium liquid of melting furnace or titanium alloy liquid; Described the first centrifugal atomizing unit comprises the first rotating shaft and is arranged at the first centrifugal atomizing dish in the first rotating shaft, and described the first centrifugal atomizing dish rotates described titanium liquid or titanium alloy liquid are carried out to centrifugal atomizing will be through titanium drop or titanium alloy drop Directional Throw to the second centrifugal atomizing unit of a centrifugal atomizing; Described the second centrifugal atomizing unit comprises the second rotating shaft and is arranged at the second centrifugal atomizing dish in the second rotating shaft, and described the second centrifugal atomizing dish rotates to described titanium drop or titanium alloy drop are carried out the secondary centrifuging atomization and will pulverize the drop throwing to described aggregate tube through the broken drop of the titanium valve of secondary centrifuging atomization or titanium alloy; Described aggregate tube pulverizes for collecting through the broken drop of the titanium valve of twice centrifugal atomizing or titanium alloy purification ultrafine titanium powder or the Titanium Powder that drop obtains after cooling.
According to an embodiment of the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder, described carrier pipe is arranged at the bottom of melting furnace, and the internal diameter of described carrier pipe is Φ 6~12mm.
According to an embodiment of the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder, described the first centrifugal atomizing unit or the second centrifugal atomizing unit adopt by the motor-driven gear transmission mechanism and drive the indirect drive mode that the first rotating shaft or the second rotating shaft are rotated again.
According to an embodiment of the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder, the axis of the axis of described the first centrifugal atomizing dish and the second centrifugal atomizing dish is orthogonal or parallel to each other.The axis angle of the two can be selected arbitrarily between 0~180 degree in principle.
According to an embodiment of the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder, the rotating speed of described the first centrifugal atomizing dish and diameter are less than rotating speed and the diameter of the second centrifugal atomizing dish.
According to an embodiment of the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder, the diameter of described the first centrifugal atomizing dish is Φ 30~70mm, and rotating speed is 5000~15000r/min; The diameter of described the second centrifugal atomizing dish is Φ 80~120mm, and rotating speed is 15000~25000r/min.
An embodiment according to the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder, be connected with inert gas in described protective cover.
The present invention compared with prior art has following advantage:
1, the required degree of superheat of the metal liquid of melt titanium or titanium alloy is low, lower than ultrasonic atomizatio and other atomization methods.This is particularly important for the atomization of the high titanium or titanium alloy of fusing point, and this can reduce the consumption of melting furnace (or crucible) refractory material and the damage of atomization plant effectively.
2, the centrifugal atomizing method is with mechanical force crushing metal liquid, and power demand is low, efficiency is high and free from environmental pollution, does not also need to consume a large amount of inert gases.
3, twice centrifugal atomizing of titanium liquid or titanium alloy liquid carried out simultaneously, atomizing effect is good, can obtain titanium valve or Titanium Powder that 90% above granularity is less than 45 μ m, and greatly reduce the atomizing disk rotating speed of centrifugal atomizer, greatly improve the steady operation life-span of atomizer, reduced the spare parts consumption of atomizer.
The accompanying drawing explanation
Fig. 1 is the structural representation of the device for making of the purification ultrafine titanium powder of an illustrative embodiment of the invention or Titanium Powder.
Fig. 2 is the first centrifugal atomizing dish in the device for making of the purification ultrafine titanium powder of another exemplary embodiment of the present invention or Titanium Powder and the combination schematic diagram of the second centrifugal atomizing dish.
Description of reference numerals:
1-protective cover, 2-melting unit, 3-melting furnace, 4-carrier pipe, 5-the first centrifugal atomizing unit, 5-1-the first rotating shaft, 5-2-the first centrifugal atomizing dish, 6-the second centrifugal atomizing unit, 6-1-the second rotating shaft, 6-2-the second centrifugal atomizing dish, 7-aggregate tube, 8-gas access, 9-gas vent.
The specific embodiment
Hereinafter, in connection with exemplary embodiment and accompanying drawing, specifically describe the present invention.
According to the preparation method of purification ultrafine titanium powder of the present invention or Titanium Powder, comprise the following steps: titanium or titanium alloy raw material are molten into to titanium liquid or titanium alloy liquid; Described titanium liquid or titanium alloy liquid are carried out to centrifugal atomizing one time by the first centrifugal atomizing dish rotated; Again the second centrifugal atomizing dish of the titanium drop after a centrifugal atomizing or the rotation of titanium alloy drop is carried out to the secondary centrifuging atomization; Collection obtains purification ultrafine titanium powder or Titanium Powder through twice centrifugal atomizing cooled titanium valve or Titanium Powder, and wherein, above each step is all carried out under inert gas atmosphere.
Particularly, the preparation method of purification ultrafine titanium powder of the present invention or Titanium Powder makes the titanium sponge melted or titanium alloy simultaneously through twice centrifugal atomizing break process (even motlten metal is ground into the method for powder by the effect of centrifugal force) and in inert gas such as argon gas, be rapidly solidificated into the method for powder, specifically can comprise the preparation process such as pretreatment of raw material, fusing, centrifugal atomizing, cooling, screening and the packing of product, its key step is analyzed as follows:
Pretreatment of raw material: select applicable titanium sponge or titanium alloy piece as raw material according to the performance requirement of product, remove its oxide on surface and impurity to obtain purer titanium valve or Titanium Powder by chemistry or mechanical means.But this step is not essential step, those skilled in the art can increase or delete this step according to actual needs.
Fusing: raw material or raw material after pretreatment are put into to the crucible of being made by calcium oxide, zirconia refractory; and it is melted under the protection of inert gas atmosphere such as argon gas in heating furnace; after the raw material in crucible is fused into titanium liquid or titanium alloy liquid; in order further to reduce the viscosity of titanium liquid or titanium alloy liquid, preferably its overheated 30~150 ℃ also are incubated to treat centrifugal atomizing.Wherein, can to raw material, carry out heat fused by Efco-Northrup furnace, but also can adopt other melting methods.
Centrifugal atomizing: the titanium liquid after melting or titanium alloy liquid carry out centrifugal atomizing one time by the first centrifugal atomizing dish rotated, and titanium liquid or titanium alloy liquid are by primary fragmentation; Then, before the titanium drop after a centrifugal atomizing or titanium alloy drop solidify, promptly it is not carried out to the secondary centrifuging atomization by the second centrifugal atomizing dish rotated, by titanium drop or the further second-time breakage of titanium alloy drop to reach the purpose of further refinement.Wherein, the diameter of the first centrifugal atomizing dish is Φ 30~70mm, and rotating speed is 5000~15000r/min; The diameter of the second centrifugal atomizing dish is Φ 80~120mm, and rotating speed is 15000~25000r/min.
Cooling: as to take out and namely obtain purification ultrafine titanium powder or Titanium Powder product after the titanium drop after twice centrifugal atomizing or titanium alloy drop are cooled to room temperature and are frozen into powder.
In addition, can also comprise the step of screening, namely with as titanium valve or the Titanium Powder of the screening plants such as ultrasonic vibration sieve to gained, sieving, with the product that is divided into different size or non-compliant product is screened out and return fusing use again.The titanium valve that is less than 45 μ m or the Titanium Powder that for example, can be set to sieve out be qualified products.
Wherein, at high temperature oxygen, nitrogen, carbon to be had to a high parent active due to titanium and titanium alloy, so above-mentioned steps all should carry out under the protective atmosphere of inert gas such as argon gas, helium etc., to guarantee the high-purity and low oxygen content of product.Wherein, the oxygen content in inert gas is less than 0.1%, and atmosphere pressures is greater than 30Pa.
What those skilled in the art should know is, although the preparation method in the present invention is for the production of purification ultrafine titanium powder and Titanium Powder, the present invention can also be applied to preparation and the production of the submicron metal that other fusing point is lower, as aluminium powder, copper powder etc.
According to purification ultrafine titanium powder of the present invention or Titanium Powder, by said method, prepared.In one exemplary embodiment of the present invention, prepared purification ultrafine titanium powder or Titanium Powder are spherical in shape or class is spherical, and by weight percentage, the described titanium valve more than 90% or the granularity of Titanium Powder are less than 45 μ m; The oxygen content of purification ultrafine titanium powder is less than 0.1%, the oxygen content of ultra-fine Titanium Powder is less than 0.15%, but the superfines product of gained of the present invention is not limited to this, can also be the as required concrete adjusting process parameter of those skilled in the art is to obtain the superfines product of different grain size and specification.
According to the device for making of purification ultrafine titanium powder of the present invention or Titanium Powder be used to implementing said method.Particularly, Fig. 1 is the structural representation of the device for making of the purification ultrafine titanium powder of an exemplary embodiment or Titanium Powder, and Fig. 2 is the first centrifugal atomizing dish in the device for making of the purification ultrafine titanium powder of another exemplary embodiment or Titanium Powder and the combination schematic diagram of the second centrifugal atomizing dish.With reference to Fig. 1; the device for making of described purification ultrafine titanium powder or Titanium Powder comprises melting unit 2, the first centrifugal atomizing unit 5, the second centrifugal atomizing unit 6, aggregate tube 7 and protective cover 1; wherein; melting unit 2, the first centrifugal atomizing unit 5, the second centrifugal atomizing unit 6, aggregate tube 7 all are arranged in protective cover 1, on protective cover 1, are provided with gas access 8 and gas vent 9.Because titanium etc. is at high temperature active to the height parent of oxygen, nitrogen, carbon; if produce purification ultrafine titanium powder or the Titanium Powder of high-purity low-oxygen content; whole processing process is carried out under the protective atmosphere of inert gas, gas access 8 is be used to inputting gas, and gas vent 9 is for Exhaust Gas.Particularly, inert gas can be argon gas, helium etc., and gas pressure is greater than 30Pa.
Melting unit 2 comprises melting furnace 3 and carrier pipe 4, and melting furnace 3, for raw material is heated, makes titanium material be molten into titanium liquid or titanium alloy liquid, and melting furnace 3 can be the stoves such as Efco-Northrup furnace, but is not limited to this; Carrier pipe 4 is delivered to the first centrifugal atomizing unit 5 for the titanium liquid by melting furnace 3 or titanium alloy liquid, and carrier pipe 4 is arranged at the bottom of melting furnace 3, and the bottom of melting furnace 3 is provided with the hole of Φ 6~12mm, and the internal diameter of carrier pipe 4 is Φ 6~12mm.When needs carried titanium liquid or titanium alloy liquid to produce, titanium liquid or titanium alloy liquid can flow to the first centrifugal atomizing unit 5 from melting furnace 3 by carrier pipe 4 under Gravitative Loads.Preferably, carrier pipe 4 is made by refractory material, and such as by calcium oxide or zirconia etc., being made, above-mentioned material is high temperature resistant and the heat of heat conduction loss is few, has reduced titanium liquid or the thermal loss of titanium alloy liquid before entering the centrifugal atomizing unit.But the flow driving mode of the setting position of carrier pipe 4, material, size and titanium liquid or titanium alloy liquid is not limited to this.
The first centrifugal atomizing unit 5 comprises the first rotating shaft 5-1 and is arranged at the first centrifugal atomizing dish 5-2 on the first rotating shaft 5-1, and the first centrifugal atomizing dish 5-2 rotates titanium liquid or titanium alloy liquid are carried out to centrifugal atomizing will be through molten drop Directional Throw to the second centrifugal atomizing unit 6 of a centrifugal atomizing.The second centrifugal atomizing unit 6 comprises the second rotating shaft 6-1 and is arranged at the second centrifugal atomizing dish 6-2 on the second rotating shaft 6-1, and the second centrifugal atomizing dish 6-2 rotates to titanium liquid or titanium alloy liquid are carried out the secondary centrifuging atomization and will pulverize the drop throwing to aggregate tube 7 through the metal of secondary centrifuging atomization.
Wherein, the angle of the axis of the axis of the first centrifugal atomizing dish 5-2 and the second centrifugal atomizing dish 6-2 can be selected in 0~180 degree, but when the axis of two centrifugal atomizing dishes is orthogonal or parallel to each other, more easily implement, these two kinds of concrete set-up modes can be respectively referring to Fig. 1 and Fig. 2.And, the rotating speed of the first centrifugal atomizing dish 5-2 and diameter are less than rotating speed and the diameter of the second centrifugal atomizing dish 5-2, because the running temperature of the first centrifugal atomizing dish is higher, for the reliability service of equipment, to consider, rotating speed and the diameter of the first centrifugal atomizing dish 5-2 are all less.In one embodiment of the invention, the diameter of the first centrifugal atomizing dish 5-2 is Φ 30~70mm, and rotating speed is 5000~15000r/min; The diameter of the second centrifugal atomizing dish 6-2 is Φ 80~120mm, and rotating speed is 15000~25000r/min.Preferably, the first centrifugal atomizing dish 5-2 is made by refractory material, and the heat loss of the titanium liquid after a centrifugal atomizing is pulverized or titanium alloy liquid is few, is conducive to the process of secondary-atomizing; The second centrifugal atomizing dish 6-2 is made by tungsten-molybdenum alloy, and the tungsten-molybdenum alloy heat resisting is suitable as the material of centrifugal atomizing dish very much.Due to the mode that has adopted twice centrifugal atomizing to carry out simultaneously, reduced the rotating speed of centrifugal atomizing unit shaft, thus in the first centrifugal atomizing unit 5 or the second centrifugal atomizing unit 6 adopt by the motor-driven gear transmission mechanism and drive again the indirect drive mode that the first rotating shaft 5-1 or the second rotating shaft 6-1 rotate, this makes the structure heat resistance of device increase substantially.
Aggregate tube 7 pulverizes for collecting through the broken drop of the titanium valve of twice centrifugal atomizing or titanium alloy purification ultrafine titanium powder or the Titanium Powder that drop obtains after cooling, in inert gas atmosphere, carries out cooled and solidified and becomes metal dust through the pulverizing drop of twice centrifugal atomizing.
In the process of centrifugal atomizing, the parameters such as the diameter of the degree of superheat that can be by controlling titanium liquid or titanium alloy liquid, diameter, rotating speed and the second centrifugal atomizing dish of the first centrifugal atomizing dish, rotating speed, obtain titanium valve or the Titanium Powder of different-shape and particle diameter.In exemplary embodiment of the present invention, the diameter of the first atomizing disk is Φ 30~70mm, and rotating speed is 5000~15000r/min; The diameter of the second centrifugal atomizing dish is Φ 80~120mm, and rotating speed is 15000~25000r/min.And what those skilled in the art should know is, although the device for making in the present invention is for the production of purification ultrafine titanium powder and Titanium Powder, this device can also be applied to preparation and the production of other submicron metal.
Below in conjunction with concrete example, the present invention is described.
Example 1
Get the titanium sponge (PTi-100) of 5kg, after carrying out the removal of surface impurity and oxide, put it in the Efco-Northrup furnace that is filled with argon gas and make it 1670 ℃ of fusings, 80 ℃ to 1750 ℃ of its temperature overheatings of fusing relief, then make point molten metal flow to the first centrifugal atomizing dish by carrier pipe, carry out centrifugal atomizing one time, wherein, the diameter of the first centrifugal atomizing dish is that Φ 70mm, rotating speed are 5000r/min.Molten drop after a centrifugal atomizing enters in the second centrifugal atomizing dish and carries out the secondary centrifuging atomization by Directional Throw, and the diameter of the second centrifugal atomizing dish is that Φ 120mm, rotating speed are 15000r/min.Cooled and solidified in the environment of titanium drop at argon gas after twice centrifugal atomizing pulverized, to be cooledly to room temperature, take out, by ultrasonic vibration, sieve again, according to grading, obsolete coarse granule is returned to fusing again to be used, acquisition is less than the titanium valve of 45 μ m, becomes product with the plastic foil vacuum packaging.The granule-morphology of the purification ultrafine titanium powder product of producing is spherical in shape or class is spherical, wherein 90wt% above powder size be less than 45 μ m, the main chemical elements content of titanium valve product is as shown in table 1.
The main chemical elements content of titanium valve in table 1 example 1
Composition Ti O H Cl C N Fe
Content/wt% 99.6 0.06 0.004 0.04 0.01 0.01 0.05
Example 2
Get 5 kilograms of Ti6Al4V titanium alloy pieces, after removing oxide on surface and impurity, put into the Efco-Northrup furnace that is filled with argon gas and make it 1650 ℃ of fusings, 70 ℃ to 1710 ℃ of its temperature overheatings of fusing relief, then make the molten metal fused solution flow to the first centrifugal atomizing dish by carrier pipe, carry out centrifugal atomizing one time, wherein the diameter of the first centrifugal atomizing dish is that Φ 30mm, rotating speed are 15000r/min.Molten drop after a centrifugal atomizing enters in the second centrifugal atomizing dish and carries out the secondary centrifuging atomization by Directional Throw, and the diameter of the second centrifugal atomizing dish is that Φ 80mm, rotating speed are 25000r/min.Cooled and solidified in the environment of titanium alloy drop at argon gas after twice atomization pulverized, to be cooledly to room temperature, take out, by ultrasonic vibration, sieve again, according to grading, obsolete coarse granule is returned to fusing again to be used, acquisition is less than the Titanium Powder of 45 μ m, becomes product with the plastic foil vacuum packaging.The granule-morphology of the ultra-fine Titanium Powder product of producing is spherical in shape or class is spherical, wherein 90wt% above powder size be less than 45 μ m, the main chemical elements content of Titanium Powder product is as shown in table 2.
The main chemical elements content of Titanium Powder in table 2 example 2
Composition Al V Fe Si O H N C Ti
Content/wt% 6.12 3.96 0.04 0.06 0.15 0.01 0.03 0.02 Surplus
Preparation method's production efficiency of purification ultrafine titanium powder of the present invention or Titanium Powder is high, energy consumption is low; The titanium valve of being produced by this method or the particle of Titanium Powder is spherical in shape or class is spherical, oxygen content is low, density is high, good fluidity, fine size, is the very good material that injection moulding, 3D print and prepared by powdered metal parts; The producing equipment of purification ultrafine titanium powder or Titanium Powder is more reliable and more stable, and its production efficiency is higher than other superfines device for making.
The invention is not restricted to above-described embodiment, without departing from the present invention, can carry out various changes and modifications.

Claims (16)

1. the preparation method of a purification ultrafine titanium powder or Titanium Powder, is characterized in that, said method comprising the steps of:
Titanium or titanium alloy raw material are molten into to titanium liquid or titanium alloy liquid;
Described titanium liquid or titanium alloy liquid are carried out to centrifugal atomizing one time by the first centrifugal atomizing dish rotated;
Again the titanium drop after a centrifugal atomizing or titanium alloy drop are carried out to the secondary centrifuging atomization by the second centrifugal atomizing dish rotated;
Collection obtains purification ultrafine titanium powder or Titanium Powder through twice centrifugal atomizing cooled titanium valve or Titanium Powder,
Wherein, above each step is all carried out under inert gas atmosphere.
2. the preparation method of purification ultrafine titanium powder according to claim 1 or Titanium Powder, is characterized in that, the diameter of described the first centrifugal atomizing dish is Φ 30~70mm, and rotating speed is 5000~15000r/min; The diameter of described the second centrifugal atomizing dish is Φ 80~120mm, and rotating speed is 15000~25000r/min.
3. the preparation method of purification ultrafine titanium powder according to claim 1 or Titanium Powder, is characterized in that, described method also comprises removes described titanium or the oxide on surface of titanium alloy raw material and the pre-treatment step of impurity.
4. the preparation method of purification ultrafine titanium powder according to claim 1 or Titanium Powder, is characterized in that, described method also comprises the step to sieving and/or pack through twice centrifugal atomizing cooled titanium valve or Titanium Powder.
5. the preparation method of purification ultrafine titanium powder according to claim 1 or Titanium Powder, is characterized in that, will after the titanium liquid after fusing or overheated 30~150 ℃ of titanium alloy liquid, carry out centrifugal atomizing again.
6. the preparation method of purification ultrafine titanium powder according to claim 1 or Titanium Powder, is characterized in that, described inert gas is argon gas, helium, and the oxygen content in inert gas is less than 0.1%, and atmosphere pressures is greater than 30Pa.
7. a purification ultrafine titanium powder or Titanium Powder, is characterized in that, described purification ultrafine titanium powder or Titanium Powder are that the preparation method by the described purification ultrafine titanium powder of any one in claim 1 to 6 or Titanium Powder makes.
8. purification ultrafine titanium powder according to claim 7 or Titanium Powder, is characterized in that, described purification ultrafine titanium powder or Titanium Powder are spherical in shape or class is spherical, and by weight percentage, the described titanium valve more than 90% or the granularity of Titanium Powder are less than 45 μ m; The oxygen content of described purification ultrafine titanium powder is less than 0.1%, and the oxygen content of ultra-fine Titanium Powder is less than 0.15%.
9. the device for making of a purification ultrafine titanium powder or Titanium Powder, is characterized in that, described device for making is for implementing the claims the preparation method of the described purification ultrafine titanium powder of 1 to 6 any one or Titanium Powder.
10. the device for making of purification ultrafine titanium powder according to claim 9 or Titanium Powder, is characterized in that, described device for making comprises melting unit, the first centrifugal atomizing unit, the second centrifugal atomizing unit, aggregate tube and protective cover, wherein,
Described melting unit, the first centrifugal atomizing unit, the second centrifugal atomizing unit, aggregate tube all are arranged in protective cover, on protective cover, are provided with gas access and gas vent;
Described melting unit comprises melting furnace and carrier pipe, and described carrier pipe is for being delivered to the first centrifugal atomizing unit by the titanium liquid of melting furnace or titanium alloy liquid;
Described the first centrifugal atomizing unit comprises the first rotating shaft and is arranged at the first centrifugal atomizing dish in the first rotating shaft, and described the first centrifugal atomizing dish rotates described titanium liquid or titanium alloy liquid are carried out to centrifugal atomizing will be through titanium drop or titanium alloy drop Directional Throw to the second centrifugal atomizing unit of a centrifugal atomizing;
Described the second centrifugal atomizing unit comprises the second rotating shaft and is arranged at the second centrifugal atomizing dish in the second rotating shaft, and described the second centrifugal atomizing dish rotates to described titanium drop or titanium alloy drop are carried out the secondary centrifuging atomization and will pulverize the drop throwing to described aggregate tube through the broken drop of the titanium valve of secondary centrifuging atomization or titanium alloy;
Described aggregate tube pulverizes for collecting through the broken drop of the titanium valve of twice centrifugal atomizing or titanium alloy purification ultrafine titanium powder or the Titanium Powder that drop obtains after cooling.
11. the device for making of purification ultrafine titanium powder according to claim 10 or Titanium Powder, is characterized in that, described carrier pipe is arranged at the bottom of melting furnace, and the internal diameter of described carrier pipe is Φ 6~12mm.
12. the device for making of purification ultrafine titanium powder according to claim 10 or Titanium Powder, it is characterized in that, described the first centrifugal atomizing unit or the second centrifugal atomizing unit adopt the indirect drive mode that drives again the first rotating shaft or the second rotating shaft rotation by the motor-driven gear transmission mechanism.
13. the device for making of purification ultrafine titanium powder according to claim 10 or Titanium Powder, is characterized in that, the axis of the axis of described the first centrifugal atomizing dish and the second centrifugal atomizing dish is orthogonal or parallel to each other.
14. the device for making of purification ultrafine titanium powder according to claim 10 or Titanium Powder, is characterized in that, the rotating speed of described the first centrifugal atomizing dish and diameter are less than rotating speed and the diameter of the second centrifugal atomizing dish.
15. the device for making of purification ultrafine titanium powder according to claim 10 or Titanium Powder, is characterized in that, the diameter of described the first centrifugal atomizing dish is Φ 30~70mm, and rotating speed is 5000~15000r/min; The diameter of described the second centrifugal atomizing dish is Φ 80~120mm, and rotating speed is 15000~25000r/min.
16. the device for making of purification ultrafine titanium powder according to claim 10 or Titanium Powder, is characterized in that, is connected with inert gas in described protective cover.
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