CN101391306B - Device and method for preparing globular titanium micro-powder or ultra-micro powder - Google Patents
Device and method for preparing globular titanium micro-powder or ultra-micro powder Download PDFInfo
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- CN101391306B CN101391306B CN 200810180992 CN200810180992A CN101391306B CN 101391306 B CN101391306 B CN 101391306B CN 200810180992 CN200810180992 CN 200810180992 CN 200810180992 A CN200810180992 A CN 200810180992A CN 101391306 B CN101391306 B CN 101391306B
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Abstract
The invention belongs to a process for preparing and processing powder material by taking plasma as a heat source, in particular to a process and an apparatus of metal titanium powder material for powder metallurgy, plasma spray, injection forming, gel injection molding and the like. The invention has the advantages that: the adoption of the high temperature spheroidization and rapid condensation special spheroidization technique can improve the sphericity and purity of titanium powder, and both a reactor and the titanium powder spheroidization process are cooled with circulating water, thereby ensuring the sealing performance of equipment, also reducing the use of inert gases, effectively reducing costs, improving the production efficiency and guaranteeing the purity of spherical titanium powder.
Description
Technical field
The invention belongs to a kind of dusty material preparation facilities and method for processing, being specifically related to a kind of is the apparatus and method that thermal source carries out the dusty material preparation with the plasma.
Background technology
Plasma has the big characteristic of high temperature, Gao Han, high activity and thermograde, does thermal source aspect the spheroidising of micron sub-micron and some nano-powder material with plasma, has bigger technical advantage.The radio frequency plasma technology and equipment makes it to be applied even more extensively in the dusty material technical field than microwave and dc arc plasma heat source owing to it does not bring any impurity into, operation is continual and steady, material processed speed is fast, production capacity is high and equipment manufacturing cost is moderate.Has higher using value in preparation of high performance structures material or functional material and manufacture field.
Titanium and alloy thereof are a kind of important meals that grows up mid-term in 20th century; Because it has premium properties such as density is low, specific strength is high, corrosion resistance is good, hear resistance is high, no magnetic, good welding performance; Have unique application in military project and civil area, but expensive the becoming of titanium restricts the bottleneck that it enlarges the commercial market for a long time.In recent years; Low towards development cost and the direction that performance is high of titanium industry develops; Make great efforts that titanium is entered into and have the civilian industry of huge market potential; Like every field such as biomedicine, automobile, weaving, daily necessitiess, and manufacturing, the processing cost of reduction titanium alloy product become the key point that titanium alloy is produced.
At present, prepare the ripe method of titanium alloy and mainly contain vacuum melting, hot investment casting and powder metallurgic method.There is defective in these technologies of smelting process and hot investment casting, and composition is easy to segregation and tissue odds is even, introduction is mingled with, production efficiency is low and production cost is high.The prior powder metallurgy method adopts simple explained hereafter superior performance titanium alloy, but this method can only be produced the simple shape part.Though injection moulding can be realized the near net-shape preparation of complex parts, accessory size is restricted.And gel casting method can be produced the complicated shape large-scale part of composition and even tissue, near net-shape in batches; Raw material availability almost reaches 100%; And the good stability of parts; Uniformity and mechanical performance can be guaranteed fully, are applied to the titanium or titanium alloy field, can realize the low-cost serialization production of titanium alloy parts.But, in the injection moulding of titanium article and gel casting, need material powder to have sphericity preferably, the main at present aerosolization titanium alloy powder that adopts, cost is higher.Adopting plasma technology that erose Low cost technique of titanium powders is carried out spheroidising is the effective way that further reduces injection and gel casting titanium article cost; Meet the titanium article industrial development direction, have important practical significance in the large-scale application of civilian industry for realizing the low-cost and high-performance titanium article.
Molten metal stream of liquid droplets bump barrier plate is adopted in preparation sized spherical titanium powder Europe the earliest, receive drag effect to be split into droplet after cooling curing be shaped, resulting titanium ball, most for ellipsoid be the bar-shaped powder of round end with some two ends.After this Preston of the U.S. etc. succeeds with dc arc plasma fusion, cooling forming method, obtains not having the nodularization titanium valve of ellipsoid and rod-shpaed particle, but need detect not nodularization particle with the manufactured goods branch, reprocess.After getting into the nineties in last century, the demand of spherical powder is increasing, and the plasma spraying technology has obtained sufficient development.The plasma spraying technology is successfully applied to various fields such as producing spherical powder, superfines, spraying, CVD diamond deposition abroad.The end of the year 1998 plasma spraying will be used for the industrial-scale production sized spherical titanium powder like Canadian PyroGenesis Co., Ltd; What the said firm used is the non-commentaries on classics arc of direct current plasma nozzle; Plasma spraying equipment becomes the nozzle at 20-40 ° of angles to form by three with vertical direction, overcomes the deficiency that powder particle is difficult to send to plasma arcs core high-temperature region thus.But the major defect of these dc arc plasma methods is its electrode erosions, introduces impurity, and regularly replacing of electrode, influences the continous-stable operation of device systems.
Prepare the method for tiny spherical metal ti powder at present, productivity ratio is lower, and cost is higher.The radio frequency plasma method be prepare that component is even, defective is few, the titanium valve or the titanium alloy powder of good fluidity, good sphericity, have both lower production cost again, higher productivity ratio is that a kind of skill is preferably stated approach.
Summary of the invention
The spherical titanium micro mist of preparation of titanium valve good sphericity, purity height and the low production cost that the purpose of this invention is to provide a kind of production efficiency height, prepares or the apparatus and method of ultra micro powder.
The present invention is achieved in that a kind of device for preparing spherical titanium micro mist or ultra micro powder, and it comprises a fixture; The quartz ampoule external member that is connected with the fixture lower seal; The powder material injection gun that runs through fixture and be tightly connected with it is with radio-frequency induction coil outside the quartz ampoule external member, described quartz ampoule external member is to be formed by interior quartz ampoule, middle quartz ampoule and outer quartz ampoule coaxial arrangement; Outer quartz ampoule and interior quartz ampoule lower ends; Leave the circulation gap between the lower end of middle quartz ampoule and the bottom of outer quartz ampoule and interior quartz ampoule, between quartz ampoule and the middle quartz ampoule, form the cooling duct of quartz ampoule external member between middle quartz ampoule and the outer quartz ampoule in making; On fixture, be provided with the cooling water import and export, they communicate with the cooling duct of quartz ampoule external member; Said powder material injection gun is to be arranged by the interior pipe of steel, middle pipe and outer coaxial tube to form; Link to each other between the bottom of outer tube and interior pipe; Leave the circulation gap between the lower end of middle pipe and the bottom of outer tube and interior pipe, make between interior pipe and the middle pipe, the cooling duct of formation powder material injection gun between middle pipe and the outer tube; On fixture, also have injection gun cooling water import and export, they communicate with powder material injection gun cooling duct; On fixture, also be provided with reacting gas input port and protective gas input port simultaneously, they all communicate with interior quartz ampoule; Downside has the igniting tunnel outside the quartz ampoule external member, in the igniting tunnel, is provided with movably electric discharge device, and the bottom of quartz ampoule external member is provided with heat-exchanging chamber, and heat-exchanging chamber is connected with the gas solid separation chamber through tube connector.
Described radio-frequency induction coil is with the outer jacket teflon tube of copper tube, turns to straight through 4～5 identical circle coaxial coils.
Described heat-exchanging chamber outside is provided with cooling device, and coolant outlet is located at the top of coolant apparatus, and coolant entrance is located at the bottom of coolant apparatus.
A kind of method for preparing spherical titanium micro mist or ultra micro powder, it comprises following step,
1) sets up the argon plasma torch of stable operation;
2) the core high-temperature region heating that gas injects metallic titanium powder on the argon plasma torch is carried in utilization;
3) the titanium valve particle drop cooling curing behind the heating and melting is formed the sized spherical titanium powder end;
4) gas is detached, collect sized spherical titanium powder.
Advantage of the present invention is; Use apparatus and method provided by the present invention to adopt high temperature nodularization and the special spheronization techniques of rapid condensation; Can improve the sphericity and the purity of titanium valve; All make in reactor and the titanium valve nodularization process to be cooled with circulating water, not only guaranteed the Seal of Equipment performance, but also reduced the use amount of inert gas, effectively reduce cost, enhance productivity and can ensure the purity of sized spherical titanium powder.
Description of drawings
Fig. 1 is a kind of apparatus structure generalized section for preparing spherical titanium micro mist or ultra micro powder provided by the present invention;
Fig. 2 is a powder material injection gun structural profile sketch map in this a kind of device for preparing spherical titanium micro mist or ultra micro powder provided by the present invention;
Fig. 3 is the scanning electron microscopy sheet of the former powder of titanium valve;
Fig. 4 is the scanning electron microscopy sheet of sized spherical titanium powder.
Among the figure, 1 powder material injection gun, 2 reacting gas input ports, quartz ampoule in the 3 protective gas input ports 4,5 quartz ampoule coolant outlets, 6 fixtures; 7 quartz ampoule cooling water inlets, 8 radio-frequency induction coils, quartz ampoule in 9,10 quartz ampoule external members, 11 electric discharge devices; 12 igniting tunnels, 13 plasma torch, 14 outer quartz ampoules, 15 injection gun cooling water inlets, 16 injection gun coolant outlets; Pipe in 17, pipe in 18,19 outer tubes, 21 coolant outlets, 22 heat-exchanging chambers; 23 tube connectors, 24 coolant entrances, 25 dust outlets, gas solid separation chambers 26,27 cooling devices.
The specific embodiment
Process titanium valve according to the present invention with plasma device; Utilize the high energy characteristic of radio frequency (RF) plasma; With carrying gas (argon gas) through feeding gun injected plasma torch, the former powder particles of irregular titanium is heated rapidly and is melted with the former powder particles of titanium in irregular shape, and the particle of fusion forms the very high drop of sphericity under capillary effect; And under high thermograde, solidify rapidly, can form the titanium valve of good sphericity.
Apparatus of the present invention mainly comprise the high-frequency plasma power supply, plasma generator and reactor, a feeder, a heat-exchanging chamber, gas solid separation, dusty material collecting chamber and a feeding gun.But that these equipment are formed is stable, continuous operation, industrialization production system that production capacity is high.
The present invention adopts high temperature nodularization and the special spheronization techniques of rapid condensation; All make in reactor and the titanium valve nodularization process and be cooled with circulating water; Not only guarantee the Seal of Equipment performance, but also reduced the use amount of inert gas, effectively reduced cost, ensured the purity of sized spherical titanium powder.
The present invention requires the system that sets up that designs to make the adjusting range of each item technical parameter be able to widen according to the titanium valve nodularization; Help optimising and adjustment plasma power, density; Parameter combinations such as reactor pressure, air-flow, join with an amount of powder that meets raw material titanium valve treatment characteristic with carry gas and obtain best nodularization effect.Fig. 3,4 comparison are visible, and the nodularization rate almost reaches 100%, and the spheroidal particle pattern is all good.
The invention provides a kind of to the metallic titanium powder method for processing.This method may further comprise the steps: with feeder the former powder of Titanium is passed through in the feeding gun injected plasma torch, form the droplet of fusion with the plasma torch fusing titanium valve of this device; The titanium valve droplet of fusion leaves plasma torch with the speed that is exceedingly fast, and in the cooling flight course, under capillary effect, forms the very high ti powder of sphericity; This spherical titanium valve has than the former powder of titanium better mobile higher density, purity and particle surface fineness, has reduced the material porosity, has improved the integrated application performance of titanium valve material.
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated:
A kind of device for preparing spherical titanium micro mist or ultra micro powder; It comprises a fixture 6; Quartz ampoule external member 10 that is connected with fixture 6 lower seal and the powder material injection gun 1 that runs through fixture 6 and be tightly connected with it; Outside quartz ampoule external member 10, be with radio-frequency induction coil 8, wherein, said quartz ampoule external member 10 is to be formed by interior quartz ampoule 4, middle quartz ampoule 9 and outer quartz ampoule 14 coaxial arrangement; Outer quartz ampoule 14 and interior quartz ampoule 4 lower ends; Leave the circulation gap between the lower end of middle quartz ampoule 9 and the bottom of outer quartz ampoule 14 and interior quartz ampoule 4, quartz ampoule 4 and middle quartz ampoule 9 in making, and the cooling duct that forms quartz ampoule external member 10 between middle quartz ampoule 9 and the outer quartz ampoule 14.On fixture 6, be provided with cooling water import and export 7,5, they communicate with the cooling duct of quartz ampoule external member 10; Powder material injection gun 1 be by manage 17 in the steel, middle pipe 18 and outer tube 19 coaxial arrangement form; Link to each other between the bottom of outer tube 19 and interior pipe 17, leave the circulation gap between the bottom of the lower end of middle pipe 18 and outer tube 19 and interior pipe 17, make between interior pipe 17 and the middle pipe 18; And the cooling duct that forms powder material injection gun 1 between middle pipe 18 and the outer tube 19; On fixture 6, also have injection gun cooling water entry and exit 16,15, they communicate with powder material injection gun 1 cooling duct; On fixture 6, also be provided with reacting gas input port 2 and protective gas input port 3 simultaneously, all communicate with interior quartz ampoule 4; Downside has igniting tunnel 12 outside quartz ampoule external member 10, in igniting tunnel 12, is provided with movably electric discharge device 11.The bottom of quartz ampoule external member 10 is provided with heat-exchanging chamber 22, and heat-exchanging chamber 22 is connected with gas solid separation chamber 26 through tube connector 23.Described heat-exchanging chamber 22 outsides are provided with cooling device 27, and coolant outlet 21 is located at the top of coolant apparatus 27, and coolant entrance 24 is located at the bottom of coolant apparatus 27.Cooling water is " low in and high out " like this, helps keeping the stable of plasma torch, the useful life that prolongs quartz ampoule simultaneously.
The radio-frequency induction coil 8 that is with on said quartz ampoule external member 10 outer walls can adopt the outer jacket teflon tube of copper tube, turn to straight through 5 identical circle coaxial coils, quartz ampoule water-cooled external member 10 and radio-frequency induction coil 8 coaxial installations.
The water-cooled quartz ampoule structure of three coaxial arrangement in China and foreign countries in quartz ampoule external member 10 adopts: each root in three quartz ampoules and the junction of reactor fixture 6 all seal with the O-RunddichtringO.Connecting to accomplish needs water test, guarantees that all seals at are all water-tight.
Sealing is equipped with material powder injection gun 1 in quartz ampoule external member 10, on the reactor fixture 6; Promptly be inserted through the circular port at reactor fixture 6 tops; Locate after reserving required length the lower end; And with O-RunddichtringO sealing, be fastenedly connected, its structure adopts the steel-tube construction of the interior China and foreign countries three piece coaxial arrangement identical with water-cooled quartz ampoule external member 10, itself has but loop of independent water-cooled; Promptly seal weld is connected to respectively the little quartz ampoule that is connected with middle pipe 18, outer tube 19 on reactor fixture 6, as injection gun coolant outlet 16 and injection gun cooling water inlet 15.
Electric discharge device can use the electric spark vacuum detector of outsourcing, and its front end end dateline is one section hairspring, therefore can when mobile, not clash into and damage quartz ampoule.
A kind of method for preparing spherical titanium micro mist or ultra micro powder, this method is carried out according to the following steps:
1) set up the argon plasma torch of stable operation: 50-65slpm continues argon gas stream to the plasma reactor input; Induction coil loads high voltage 6-8kV; Igniter discharge simultaneously, the coil inductively coupled and igniter corona triggering of high-voltage line makes argon gas ionization produce plasma torch.At this moment, open centrifugal blower and make maintenance negative pressure state in the reactor, plasma torch gets final product stable operation.
2) the core high-temperature region heating that gas injects metallic titanium powder (former powder) on the argon plasma torch is carried in utilization.Carry gas can use argon gas, hydrogen etc. in hot environment not with the gas of metal-powder generation chemical reaction.Finish with gas powder stream " flying away from " plasma torch heat time heating time, and the duration is merely the 140-170 millisecond.
3) the titanium valve particle drop cooling curing behind the heating and melting is formed the sized spherical titanium powder end: under radiation, convection current, conduction and four kinds of heat transfer mechanism effects of chemistry, melted by rapid heating.When particle is melted at least 50% (calculating by weight) when above, the particle of fusion forms the very high drop of sphericity under capillary effect, and in high thermograde (10
-6K/m) cooling rapidly down, the quenching of entering heat-exchanging chamber are solidified, thereby are formed spherical particle.
4) gas is detached, collect sized spherical titanium powder.
The said input flow rate of setting up the needed reacting gas argon of argon plasma torch is 1slpm～10slpm, and the high voltage that loads on the induction coil is 6kV～8kV; Reacting gas input flow rate during described argon plasma stable operation is 20slpm～40slpm, protective gas 10slpm～100slpm, and system's negative pressure is 200mm mercury column～300mm mercury column; The average grain diameter of the former powder of Titanium that is added step 2) is 0.5～45 μ m, and carrying gas control flow is 3slpm～7slpm, and titanium valve feeding control flow is 60g/min～80g/min.
Example 1, average grain diameter are 115 μ m titanium valves, and the spheroidising major parameter is: carrying gas flow is 5.0slpm, titanium valve feeding capacity 68g/min., and the plasma torch operate power is 50kW; Reacting gas 23slpm, protective gas 75slpm; System's negative pressure is the 230mm mercury column.
Example 2, average grain diameter are 25 μ m titanium valves, and the spheroidising major parameter is: carrying gas flow is 3.9slpm, titanium valve feeding capacity 65g/min., and the plasma torch operate power is 55kW; Reacting gas 26slpm, protective gas 80slpm; System's negative pressure is the 240mm mercury column.
The former powder of titanium valve is passed through the feeding gun injected plasma torch from feeder, and this powder is the spongy titanium valve that mechanical disintegration or air-flow are pulverized.Irregular titanium valve particle is heated rapidly and is melted, and the particle of fusion forms the very high drop of sphericity under capillary effect, and these drops get into heat-exchanging chamber fast, under high thermograde, solidify rapidly.Can collect sized spherical titanium powder in the heat-exchanging chamber bottom.In the gas solid separation chamber, also can collect sized spherical titanium powder, but, the sized spherical titanium powder size more collected than heat-exchanging chamber bottom of the sized spherical titanium powder size here is relatively littler
Feeder adopts the spiral vibrating discharging, loads little airflow, gas powder mixing feeding style.This mode can guarantee unfinished uniformity.The collection of nodularization titanium valve then uses storage tank to import and export respectively has an automatic valve, and level-sensing device is installed in jar.Level-sensing device is provided with that two of height are spacing, and system just opens, and the charging valve open is piled up paramount spacingly when powder, and the charging valve is closed automatically, and the discharging valve open is collected and packed products nodularization titanium valve.In case in the storage tank powder discharge drop to low spacing, discharging valve closing then, the charging valve open, so Automatic Cycle work does not need manual intervention.But this mode automatic gauge of doing is filled the small amounts of inert gas topic in jar, prevent the titanium valve oxidation.
Fig. 3 provides the scanning electron microscopy sheet of the former powder of titanium valve.As shown in the figure, the former powder of titanium valve has irregular shape, and each particle has tangible acute angle, and the surface is extremely coarse.Fig. 4 provides the scanning electron microscopy sheet of handling the sized spherical titanium powder of back acquisition with apparatus and method according to the invention.Each coating of particles becomes sphere, and the surface of each particle is extremely smooth.
During with the ASTMB212-99 canonical measure, the apparent density of the titanium valve after the process plasma nodularization processed is by 3.2g/cm
3Increase to 4.3g/cm
3The increase of apparent density and the change of grain shape help improving the titanium valve flowability; The flowability that said sized spherical titanium powder is good; Prepare in the process at metal injection moulding, gel casting, guarantee that the component of titanium or titanium alloy product is even, defective is few, excellent performance.
In a word, plasma nodularization titanium micro mist or ultra micro powder can change the titanium valve coating of particles and increase the apparent density of powder, and it is mobile to have increased titanium valve.
Claims (3)
1. device for preparing spherical titanium micro mist or ultra micro powder; It comprises a fixture (6); With the quartz ampoule external member (10) that fixture (6) lower seal is connected, the powder material injection gun (1) that runs through fixture (6) and be tightly connected with it is with radio-frequency induction coil (8) outside quartz ampoule external member (10); It is characterized in that: described quartz ampoule external member (10) is to be formed by interior quartz ampoule (4), middle quartz ampoule (9) and outer quartz ampoule (14) coaxial arrangement; Outer quartz ampoule (14) and interior quartz ampoule (4) lower ends leave the circulation gap between the bottom of the lower end of middle quartz ampoule (9) and outer quartz ampoule (14) and interior quartz ampoule (4), make between interior quartz ampoule (4) and the middle quartz ampoule (9); Form the cooling duct of quartz ampoule external member (10) between middle quartz ampoule (9) and the outer quartz ampoule (14); On fixture (6), be provided with cooling water import and export (7,5), they communicate with the cooling duct of quartz ampoule external member (10); Said powder material injection gun (1) is to be formed by the interior pipe (17) of steel, middle pipe (18) and outer tube (19) coaxial arrangement; Link to each other between the bottom of outer tube (19) and interior pipe (17); Leave the circulation gap between the lower end of middle pipe (18) and the bottom of outer tube (19) and interior pipe (17); Make between interior pipe (17) and the middle pipe (18), form the cooling duct of powder material injection gun (1) between middle pipe (18) and the outer tube (19), on fixture (6), also have injection gun cooling water import and export (15; 16), they communicate with powder material injection gun (1) cooling duct; On fixture (6), also be provided with reacting gas input port (2) and protective gas input port (3) simultaneously, they all communicate with interior quartz ampoule (4); Downside has igniting tunnel (12) outside quartz ampoule external member (10); In igniting tunnel (12), be provided with movably electric discharge device (11); The bottom of quartz ampoule external member (10) is provided with heat-exchanging chamber (22), and heat-exchanging chamber (22) is connected with gas solid separation chamber (26) through tube connector (23).
2. a kind of device for preparing spherical titanium micro mist or ultra micro powder as claimed in claim 1 is characterized in that: described radio-frequency induction coil (8) is with the outer jacket teflon tube of copper tube, turns to straight through 4～5 identical circle coaxial coils.
3. a kind of device for preparing spherical titanium micro mist or ultra micro powder as claimed in claim 1; It is characterized in that: described heat-exchanging chamber (22) outside is provided with cooling device (27); Coolant outlet (21) is located at the top of coolant apparatus (27), and coolant entrance (24) is located at the bottom of coolant apparatus (27).
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| CN114653960A (en) * | 2022-03-31 | 2022-06-24 | 四川真火等离子研究院有限公司 | Method for preparing superfine high-purity spherical titanium powder by magnetizing radio frequency plasma |
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2008
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