CN108217612A - Prepare the method and apparatus of spherical titanium nitride powder - Google Patents
Prepare the method and apparatus of spherical titanium nitride powder Download PDFInfo
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- CN108217612A CN108217612A CN201810089385.1A CN201810089385A CN108217612A CN 108217612 A CN108217612 A CN 108217612A CN 201810089385 A CN201810089385 A CN 201810089385A CN 108217612 A CN108217612 A CN 108217612A
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- spherical titanium
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- 239000000843 powder Substances 0.000 title claims abstract description 118
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 39
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010936 titanium Substances 0.000 claims abstract description 25
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 113
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 238000000889 atomisation Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000009826 distribution Methods 0.000 claims description 13
- 230000006641 stabilisation Effects 0.000 claims description 8
- 238000011105 stabilization Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 7
- 230000005611 electricity Effects 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 19
- 239000002994 raw material Substances 0.000 abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 15
- 239000001301 oxygen Substances 0.000 abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 abstract description 15
- 238000005121 nitriding Methods 0.000 abstract description 14
- 239000002245 particle Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000004615 ingredient Substances 0.000 abstract description 3
- 239000012495 reaction gas Substances 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 19
- 230000035611 feeding Effects 0.000 description 11
- 108010066057 cabin-1 Proteins 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000112 cooling gas Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 241001465382 Physalis alkekengi Species 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- -1 at this point Chemical compound 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0761—Preparation by direct nitridation of titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention relates to the method and apparatus for preparing spherical titanium nitride powder, and in particular to radio frequency plasma powder production technology prepares the method and apparatus of spherical titanium nitride powder.The technical problem to be solved by the present invention is to provide a kind of preparation process is simple, the method for the spherical titanium nitride powder of the high preparation of Oxygen potential.This method is using titanium valve as raw material, using nitrogen as reaction gas, titanium nitride powder is prepared in one step, its technological process is short, the reaction time is extremely short, production efficiency is substantially increased, the product free from admixture of acquisition pollutes, and preparation process is simple, relatively low to ingredient requirement, the industrialized production to realize spherical titanium nitride powder is laid a good foundation.The spherical titanium nitride powder being prepared using the method for the present invention, Oxygen potential and nitriding rate are all very high.It prepares raw material and does not need to be largely broken, particle size is small.
Description
Technical field
The present invention relates to the method and apparatus for preparing spherical titanium nitride powder, and in particular to utilizes radio frequency plasma powder
The method that production equipment prepares spherical titanium nitride powder.
Background technology
Metallic compound TiN has many excellent physics and chemical property, its corrosion resistance, abrasion resistance and anti-oxidant
Property it is all very excellent, have higher fusing point (3205 DEG C) and the (× 9.8N/mm of hardness 19902).TiN is deposited on jewellery and lamps and lanterns
On can not only reach aesthetic effect, but also wear-resisting property can be enhanced, be the potential material instead of now widely used WC, Ke Yi great
The big cost for reducing material application.TiN compounds have higher bio-compatibility, in terms of clinical medicine and dentistry
With very high application value.In addition TiN also is used as manufacture crucible, cutting tool, additive etc..The application of TiN powder is wide
Degree and depth are extremely unbecoming with excellent properties that it is possessed, need people and research and develop, can indicate, titanium nitride powder will
As century new material.
As what TiN was studied deepens continuously, the method for preparing TiN powder is also more and more.It is prepared by traditional TiN powder
Method, such as：The TiN powder shape that metallic titanium powder nitriding, titanium dioxide CRN method, vapor phase method etc. obtain is not advised
Then, mobility is poor, and performance is had a greatly reduced quality, and nitriding rate is not high, and nitridation time is longer, and particle size range is wider, the energy
Consumption is big.Up to the present, there are no effective and the problem above containing lid solutions.
Compared with aspherical titanium nitride powder, the mechanical performance of spherical titanium nitride is the same in all directions,
The product haveing excellent performance easily is obtained in powder metallurgy and 3D printing.Therefore, it is simple to be badly in need of a kind of preparation process, Oxygen potential is high
The preparation method of spherical titanium nitride.
Patent 200410072553.4 discloses a kind of method of reaction plasma spraying nano crystal titanium nitride powder, uses
Plasma gun is sprayed, and what is specifically included have main steps that：Titanium valve is packed into powder feeder, be sent into hybrid ionic gas, to
Lead to nitrogen in reative cell, titanium valve powder is sent to enter flame stream, spray and collect into the container being filled with water, using this method, can obtain
To the titanium nitride powder particle of a diameter of 30~100nm, still, this method prepares titanium nitride powder using plasma gun,
Titanium valve powder is sent to enter flame stream, during spraying and collecting into the container being filled with water, energy loss is big.And obtained titanium nitride
Sphericity is bad, and Oxygen potential needs further improve.
Invention content
For disadvantages described above, the technical problem to be solved by the present invention is to provide a kind of preparation process is simple, the high system of Oxygen potential
The method of standby spherical shape titanium nitride powder.
The method that the present invention prepares spherical titanium nitride powder, is prepared using radio frequency plasma equipment, specifically included
Following steps：
A, the starting the arc：Using argon gas as the ionized gas starting the arc, while the protective gas of nitrogen from radio frequency plasma equipment is entered
It is passed through at mouthful；The operating voltage for controlling radio frequency plasma equipment is 5~15kV, and power is 30~200kW, wherein, ionized gas
Flow is 1~10m3/ h, the nitrogen flow being passed through at gas atmosphere inlet are 1~10m3/h；
B, feeding：After arc stabilization, titanium valve is sent by feed device, obtains spherical titanium nitride.
Preferably, in a steps, after arc stabilization, ionized gas is become into nitrogen.
Preferably, the flow of ionized gas is 3~4m3/ h, the nitrogen flow being passed through at gas atmosphere inlet are 3
~6m3/h。
Preferably, in b step, the grain size of titanium valve is 1~150 μm.
Preferably, the titanium valve is fed using vibration, and amplitude is 10~80%.
Second technical problem that the present invention solves is to provide a kind of equipment for preparing spherical titanium nitride powder.
The equipment that the present invention prepares spherical titanium nitride powder, including atomization storehouse (2), the plasma being connect with atomization storehouse (2)
Torch (1), gas powder separator (8), is connect with gas powder separator (8) feed device (3) to plasmatorch (1) feeding
Air extractor (9) and receipts powder cabin two (7), it is characterised in that：Described atomization storehouse (2) bottom, which is connected with, receives powder cabin one (5), the mist
Change storehouse (2) bulkhead and be connected with exhaust pipe (10), the exhaust pipe (10) connect with gas powder separator (8)；The receipts powder cabin one
(5) and receipts powder cabin two (7) is equipped with heating unit.
Preferably, the heating unit is heating wire, and the receipts powder cabin one (5) and receipts powder cabin two (7) housing are inside and outside
Double-layer structure, the heater strip are arranged between inner and outer shell.
Preferably, the exhaust pipe (10) is in reverse V-shaped.
Preferably, the plasmatorch (1) is high frequency plasma torch.
Preferably, the high frequency plasma torch includes distribution seat (17), feed pipe (13), middle pipe (14) and discharge tube
(15)；The distribution seat (17) is equipped with ionized gas entrance (12) and gas atmosphere inlet (11), the feed pipe (13), middle pipe
(14) and discharge tube (15) is coaxially mounted to distribution seat (17) center from inside to outside successively, and the feed pipe (13) is through distribution seat
(17), the discharge tube (15) is externally provided with inductance coil (16), and the cavity of the middle pipe (14) is ionized gas channel, described to put
Cavity between fulgurite (15) and middle pipe (14) is protective gas channel, the ionized gas entrance (12) and ionized gas channel
It communicates；The gas atmosphere inlet (11) communicates with protective gas channel；The feed pipe (13) connect with feed device (3).
Compared with prior art, the present invention has the advantages that：
The method of the present invention, using titanium valve as raw material, using nitrogen as reaction gas, titanium nitride powder, work is prepared in a step
Skill flow is short, the reaction time is extremely short, substantially increases production efficiency, the product free from admixture pollution of acquisition, preparation process is simple, right
Ingredient requirement is relatively low, and the industrialized production to realize spherical titanium nitride powder is laid a good foundation.The spherical titanium nitride being prepared
Powder, Oxygen potential and nitriding rate are all very high.It prepares raw material and does not need to be largely broken, particle size is small.
The equipment of the present invention, receives powder cabin one and receipts powder cabin two is equipped with heating unit, not sufficiently reactive ball after cooling
Shape raw material powder continues to react with nitrogen after entering receipts powder cabin, and reaction is more abundant, improves the nitriding rate of raw material.Meanwhile receive powder cabin
One, for collecting the slightly larger nitridation titanium valve of particle, receives powder cabin two for collecting thinner nitridation titanium valve, so as to fulfill nitridation titanium valve
Coarse and fine separation.Plasmatorch is high frequency plasma torch, and high frequency plasma torch center is equipped with feed pipe, the spherical TiN prepared
Powder particles are thin, free from admixture pollution.Equipment using the present invention has been greatly improved the efficiency for preparing nitridation titanium valve, preparation process
Simply, relatively low to ingredient requirement, Oxygen potential and nitriding rate all increase.
Description of the drawings
Fig. 1 is the structure diagram of the equipment of the spherical titanium nitride powder of preparation of the present invention；
Fig. 2 is high frequency plasma torch structure diagram；
Shown in figure：1. plasmatorch, 2. atomization storehouses, 3. feed devices, 4. butterfly valves, 5. receive powder cabin one, and 7. receive powder cabin two,
8. gas powder separator, 9. air extractors, 10. exhaust pipes, 11. gas atmosphere inlets, 12. ionized gas entrances, 13. feedings
Pipe, 14. middle pipes, 15. discharge tubes, 16. inductance coils, 17. distribution seats, 18. plasma jets, 21. cooling gas mouths, 51. electricity
Heated filament.
Fig. 3 is the SEM figures of spherical titanium nitride powder prepared by the present invention.
Fig. 4 is the XRD diagram of spherical titanium nitride powder prepared by the present invention.
Specific embodiment
The preparation method of spherical shape titanium nitride of the invention, is prepared using radio frequency plasma equipment, specifically included as follows
Step：
A, the starting the arc：Using argon gas as the ionized gas starting the arc, while the protective gas of nitrogen from radio frequency plasma equipment is entered
It is passed through at mouthful；The operating voltage for controlling radio frequency plasma equipment is 5~15kV, and power is 30~200kW；Wherein, ionized gas
Flow is 1~10m3/h, and the nitrogen flow being passed through at gas atmosphere inlet is 1~10m3/h；
B, feeding：After arc stabilization, titanium valve is sent by feed device, it is direct while titanium valve nodularization in plasma torch
Nitridation, obtains the titanium nitride of half melt；Then the titanium nitride of half melt is under the action of surface tension, and cooled and solidified is into spherical shape.
Radio frequency plasma spheroidizing of powder technology is existing technology, and principle is the indifferent gas under high frequency electric source effect
Body is ionized, and forms stable high temperature inert gas plasma；And raw material in irregular shape through feed device be sent into etc. from
In daughter torch, a large amount of heat is absorbed in high-temperature plasma, surface is melted rapidly, and enters reactor with high speed,
It is quickly cooled down under an inert atmosphere, in the effect of surface tension, cooled and solidified is into spherical powder.And the present invention is by controlling radio frequency
The voltage of plasma apparatus, power and the parameters such as particular kind of gas and specific gas flow are passed through, realize and waiting
Direct-Nitridation while titanium valve nodularization, obtains spherical titanium nitride in gas ions torch.Its reaction principle is：
2Ti+N2=2TiN
The method of the present invention, above-mentioned reaction carry out under the conditions of the radio frequency plasma high-temperature field of argon gas and nitrogen is passed through.It is first
First, argon gas is passed through from radio frequency plasma equipment center, i.e. ionized gas inlet is passed through, and nitrogen is set from radio frequency plasma
Standby edge is passed through, i.e., is passed through at gas atmosphere inlet.Argon gas stream is easy to generate plasma jet in this way, and titanium material is carried out high temperature point
Solution.Nitrogen is passed through from radio frequency plasma powder production device end can make nitridation reaction more complete.The nitrogen that this method obtains
Change titanium Oxygen potential and nitriding rate is higher, nodularization and nitridation are carried out at the same time, and substantially increase production efficiency.
In order to improve Oxygen potential, it is preferred that in a steps, using argon gas as the ionized gas starting the arc, obtain argon arc, treat that argon arc is steady
After fixed, ionized gas is become into nitrogen, at this point, nitrogen arc will be formed.Nitrogen ionization in plasma torch is as reaction heat
It is reacted at high temperature with titanium valve as reactant again while source and directly obtains spherical titanium nitride powder, can not only save reaction
Energy consumption, moreover it is possible to improve product purity and Oxygen potential.
It is furthermore preferred that ionized gas flow is 3~4m3/ h, the nitrogen flow being passed through at gas atmosphere inlet are 3~4m3/
h。
The grain size of common titanium valve is suitable for the present invention, it is preferred that in b step, the grain size of titanium valve is 1~150 μm.
Preferably, the titanium valve is fed using vibration, and amplitude is 10~80%, can cause titanium valve in this way
Reaction is more complete, improves nitriding rate.
A kind of equipment for preparing spherical TiN powder, as shown in Figure 1, including atomization storehouse 2, the plasmatorch being connect with atomization storehouse 2
1st, the feed device 3 to 1 feeding of plasmatorch, gas powder separator 8, the air extractor 9 being connect with gas powder separator 8 and receipts
Powder cabin 27, atomization 2 bottom of storehouse, which is connected with, receives powder cabin 1, and atomization 2 bulkhead of storehouse is connected with exhaust pipe 10, the exhaust
Pipe 10 is connect with gas powder separator 8；The receipts powder cabin 1 and receipts powder cabin 27 are equipped with heating unit.
1 optional DC plasma torch of plasmatorch or high frequency plasma torch etc., plasmatorch 1 can be one or more.Deng
Ion torch 1 is connect with atomization storehouse 2, i.e., plasmatorch 1 can be mounted in atomization storehouse 2 or 1 jet orifice of plasmatorch is direct
Connection atomization storehouse 2.Gas powder separator 8 can select cyclone separator, bag filter etc., preferably cyclone separator.Pumping dress
Air pump, wind turbine etc. can be selected by putting 9, and atomization 2 bottom of storehouse, which is connected with, receives powder cabin 1, for collecting the larger spherical TiN powder of particle.
In Fig. 1, the tapered setting in 2 bottom of storehouse is atomized, powder cabin 1 is received and is located at 1 lower section of atomization storehouse, in order to the collection of powder.It is atomized storehouse 2
Bulkhead is connected with exhaust pipe 10, and atomization storehouse 2 is connected with gas powder separator 8 by exhaust pipe 10, and exhaust pipe 10 is in reverse V-shaped.Row
Tracheae 10 is in reverse V-shaped, can prevent TiN powder deposition in the duct.When equipment works, raw material is sent into plasmatorch by feed device 3
1, raw material atomized molten is simultaneously reacted with nitrogen, and being passed through cooling nitrogen from atomization storehouse cooling gas mouth 21 is quickly cooled down, the spherical shape of system
TiN powder.Larger TiN powder, which sinks to entering, to be received in powder cabin 1, and thinner TiN powder enters gas powder separator 8 through exhaust pipe 10 and divides
It is collected from after by receipts powder cabin 27.By the above-mentioned means, it can realize the coarse and fine separation to TiN powder.It receives powder cabin 1 and receives powder cabin 27
Equipped with heating unit, powder cabin 1 is kept by heating devices heat and receives 27 temperature of powder cabin equal to or higher than 800 DEG C, so as to make
Enter from the unreacted raw material of atomization 2 nodularization postcooling of storehouse after receiving powder cabin, generation can be reacted with nitrogen again in receiving warehouse
TiN, so as to improve raw material nitriding rate.Heating unit can be air blower, and people's High Temperature Gas is roused to 5 housing of moist closet using air blower
Body heats, and also optional heating wire, utilizes electrical heating.
Using air blower to receiving the drum people high-temperature gas heating of powder cabin housing, large quantity of exhaust gas can be generated, it is preferred that heating unit
For heating wire 51, it is interior outer double-layer structure to receive powder cabin one and receive two housing of powder cabin, and heater strip 51 is arranged between inner and outer shell.
It is interior outer double-layer structure to receive powder cabin housing, and heater strip 51 is arranged between inner and outer shell, can prevent from receiving the powder attachment in powder cabin
On heating wire 51.
Since high frequency plasma torch has, electrodeless pollution, arc area is big, temperature is relatively uniform, can provide pure heat source, material
Material processing is fast, especially shows unique advantage in terms of high-melting-point spheroidizing of powder.Preferably, plasmatorch is high frequency plasma
Torch.
A kind of high frequency plasma torch structure diagram as shown in Figure 2, in figure：High frequency plasma torch include distribution seat 17,
Feed pipe 13, middle pipe 14 and discharge tube 15；Distribution seat 17 is equipped with ionized gas entrance 12 and gas atmosphere inlet 11, the feeding
Pipe 13, middle pipe 14 and discharge tube 15 are coaxially mounted to 17 center of distribution seat from inside to outside successively, and 13 pipe of feed pipe wears distribution seat 17,
Discharge tube 15 is externally provided with inductance coil 16, and the cavity of middle pipe 14 is ionized gas channel, the chamber between discharge tube 15 and middle pipe 14
Body is protective gas channel, and ionized gas entrance 12 is communicated with ionized gas channel；Gas atmosphere inlet 11 leads to protective gas
Road communicates；Feed pipe 13 is connect with feed device 3.Feed pipe 13 is arranged on high frequency plasma torch center, is conducive to raw material and is sent to
Plasma arcs core high-temperature region conducive to the harmonious and nodularization of raw material, is also reacted conducive to raw material with nitrogen, improves raw material nitridation
Rate.By adjusting the air inflow of ionized gas, the enthalpy of plasma jet and injection intensity is adjusted, so as to fulfill different-effect
Melting and nodularization effect.Gas atmosphere inlet 11 can be passed through nitrogen, cold in one layer of 14 tube wall of high frequency plasma torch discharge tube formation
Air film is cooled down and is prevented the raw material of melted by heating and TiN to be adhered on 14 inner wall of discharge tube to discharge tube 14.
The specific embodiment of the present invention is further described with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment shown in FIG. 1.Set radio frequency etc. from
The amplitude of the feed arrangement of daughter powder production equipment is 20%, operating voltage 10.5KV, power 32kW." side gas " (is protected
Gas access) nitrogen is passed through, " middle gas " (i.e. ionized gas entrance) is passed through argon gas, nitrogen flow 3m3/ h, argon flow amount are
3m3/ h, wherein nitrogen are reaction gas, and argon gas is ionization of gas.5min rewindings are reacted in feeding, and spherical nitridation titanium valve is prepared
End.Its SEM schemes as shown in figure 3, its XRD spectrum is shown in Fig. 4, and the curve above Fig. 4 is the final products TiN that is prepared in embodiment 1,
Following curve is the TiN powder containing Ti.This method Oxygen potential reaches 91%, nitriding rate 87%.
Wherein, Oxygen potential carries out the acquisition of morphology observation nodularization quantity using scanning electron microscope.Nitriding rate is measured using energy disperse spectroscopy
Sample surfaces simultaneously combine the acquisition of X-ray diffractometer analysis result.
Embodiment 2
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment shown in FIG. 1.Set radio frequency etc. from
The amplitude of the feed arrangement of daughter powder production equipment is 22%, operating voltage 11.5kV, power 54kW." side gas " (is protected
Gas access) nitrogen is passed through, " middle gas " (i.e. ionized gas entrance) is first passed through the argon gas starting the arc, and closing argon gas after arc stabilization is passed through
Nitrogen, adjusting " middle gas " flow are 3m3/ h, " side gas " flow are 3m3/ h, feeding reaction 5min rewindings, measures titanium nitride powder matter
It measures as 27g.Its SEM figures are similar with Fig. 3, and XRD spectrum is similar with the curve above Fig. 4.This method Oxygen potential reaches 92%, nitrogen
Rate is 86%.
Embodiment 3
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment shown in FIG. 1.Set radio frequency etc. from
The amplitude of the feed arrangement of daughter powder production equipment is 24%, operating voltage 13kV, power 62kW." side gas " is passed through nitrogen,
" middle gas " is first passed through the argon gas starting the arc, and argon gas is closed after arc stabilization and is passed through nitrogen, adjusting " middle gas " flow is 4m3/ h, " side gas "
Flow is 4m3/ h, feeding reaction 5min rewindings, measures titanium nitride powder quality as 28g.Its SEM schemes, XRD diagram similar with Fig. 3
Spectrum is similar with the curve above Fig. 4.This method Oxygen potential reaches 90%, nitriding rate 85%.
Embodiment 4
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment shown in FIG. 1.Set radio frequency etc. from
The amplitude of the feed arrangement of daughter powder production equipment is 80%, operating voltage 5kV, power 30kW." side gas " is passed through nitrogen,
" middle gas " is first passed through the argon gas starting the arc, and argon gas is closed after arc stabilization and is passed through nitrogen, adjusting " middle gas " flow is 4m3/ h, " side gas "
Flow is 4m3/ h, feeding reaction 5min rewindings, measures titanium nitride powder quality as 28g.Its SEM schemes, XRD diagram similar with Fig. 3
Spectrum is similar with the curve above Fig. 4.This method Oxygen potential reaches 77%, nitriding rate 83%.
Embodiment 5
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment shown in FIG. 1.Set radio frequency etc. from
The amplitude of the feed arrangement of daughter powder production equipment is 10%, operating voltage 11kV, power 48kW." side gas " is passed through nitrogen,
" middle gas " is first passed through the argon gas starting the arc, and argon gas is closed after arc stabilization and is passed through nitrogen, adjusting " middle gas " flow is 4m3/ h, " side gas "
Flow is 4m3/ h, feeding reaction 5min rewindings, measures titanium nitride powder quality as 28g.Its SEM schemes, XRD diagram similar with Fig. 3
Spectrum is similar with the curve above Fig. 4.This method Oxygen potential reaches 91%, nitriding rate 89%.
Claims (10)
1. prepare the method for spherical titanium nitride powder, it is characterised in that：It is prepared using radio frequency plasma equipment, it is specific to wrap
Include following steps：
A, the starting the arc：Using argon gas as the ionized gas starting the arc, while by nitrogen at the gas atmosphere inlet of radio frequency plasma equipment
It is passed through；The operating voltage for controlling radio frequency plasma equipment is 5~15kV, and power is 30~200kW, wherein, ionized gas flow
For 1~10m3/ h, the nitrogen flow being passed through at gas atmosphere inlet are 1~10m3/h；
B, feeding：After arc stabilization, titanium valve is sent by feed device, obtains spherical titanium nitride.
2. the method according to claim 1 for preparing spherical titanium nitride powder, it is characterised in that：In a steps, treat that arc is stablized
Afterwards, ionized gas is become into nitrogen.
3. the method according to claim 2 for preparing spherical titanium nitride powder, it is characterised in that：The flow of ionized gas is
3~4m3/ h, the nitrogen flow being passed through at gas atmosphere inlet are 3~6m3/h。
4. the method for spherical titanium nitride powder is prepared according to claims 1 to 3 any one of them, it is characterised in that：B step
In, the grain size of titanium valve is 1~150 μm.
5. the method for spherical titanium nitride powder is prepared according to Claims 1 to 4 any one of them, it is characterised in that：The titanium
Powder is fed using vibration, and amplitude is 10~80%.
6. a kind of equipment for preparing spherical titanium nitride powder, including atomization storehouse (2), the plasmatorch being connect with atomization storehouse (2)
(1), to the feed device (3), gas powder separator (8), the pumping being connect with gas powder separator (8) of plasmatorch (1) feeding
Device of air (9) and receipts powder cabin two (7), it is characterised in that：Described atomization storehouse (2) bottom, which is connected with, receives powder cabin one (5), the atomization
Storehouse (2) bulkhead is connected with exhaust pipe (10), and the exhaust pipe (10) connect with gas powder separator (8)；The receipts powder cabin one (5)
Heating unit is equipped with powder cabin two (7) is received.
7. the equipment according to claim 6 for preparing spherical titanium nitride powder, it is characterised in that：The heating unit is electricity
Heated filament, the receipts powder cabin one (5) and receipts powder cabin two (7) housing are interior outer double-layer structure, and the heater strip is arranged on inside and outside shell
Between body.
8. the equipment of the spherical titanium nitride powder of preparation described according to claim 6 or 7, it is characterised in that：The exhaust pipe
(10) in reverse V-shaped.
9. the equipment according to claim 8 for preparing spherical titanium nitride powder, it is characterised in that：The plasmatorch (1)
For high frequency plasma torch.
10. the equipment according to claim 9 for preparing spherical titanium nitride powder, it is characterised in that：The high frequency plasma
Torch includes distribution seat (17), feed pipe (13), middle pipe (14) and discharge tube (15)；The distribution seat (17) enters equipped with ionized gas
Mouth (12) and gas atmosphere inlet (11), the feed pipe (13), middle pipe (14) and discharge tube (15) are coaxial from inside to outside successively
Mounted on distribution seat (17) center, the feed pipe (13) is externally provided with inductor wire through distribution seat (17), the discharge tube (15)
It encloses (16), the cavity of the middle pipe (14) is ionized gas channel, and the cavity between the discharge tube (15) and middle pipe (14) is
Protective gas channel, the ionized gas entrance (12) communicate with ionized gas channel；The gas atmosphere inlet (11) is with protecting
Shield gas passage communicates；The feed pipe (13) connect with feed device (3).
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