CN108163821A - The preparation method of spherical titanium nitride - Google Patents
The preparation method of spherical titanium nitride Download PDFInfo
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- CN108163821A CN108163821A CN201810089384.7A CN201810089384A CN108163821A CN 108163821 A CN108163821 A CN 108163821A CN 201810089384 A CN201810089384 A CN 201810089384A CN 108163821 A CN108163821 A CN 108163821A
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The present invention relates to the preparation methods of spherical titanium nitride, and in particular to the method that spherical titanium nitride is prepared using radio frequency plasma powder production equipment.The technical problem to be solved by the present invention is to provide a kind of preparation methods of the high spherical titanium nitride of Oxygen potential.The method of the present invention uses radio frequency plasma equipment as reaction unit, using hydride powder as raw material, using nitrogen as reaction gas, titanium nitride powder is prepared in one step, and technological process is short, the reaction time is extremely short, substantially increases production efficiency, the product free from admixture pollution of acquisition, preparation process is simple, relatively low to ingredient requirement, and 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 preparation methods of spherical titanium nitride, and in particular to utilizes radio frequency plasma powder production equipment system
The method of standby spherical shape titanium nitride.
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 needs pure titanium valve for raw material, needs to prepare not in advance
With the titanium powder particle of grain size, then to be nitrogenized.Preparation process is complicated, and equipment requirement is high.Importantly, pure titanium valve is in sky
It is oxidizable in gas, form titanium oxide.This is unfavorable for nitridation.In addition, the spontaneous combustion danger of pure titanium valve is much bigger,
The safety requirements higher of production.Titanium valve powder is sent to enter flame stream, during spraying and collecting into the container being filled with water, energy damage
It loses big.And obtained titanium nitride sphericity is bad, 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 ball of Oxygen potential
The preparation method of shape titanium nitride.
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；
B, feeding：After arc stabilization, it is 1 to control the flow-rate ratio of the argon gas being passed through and nitrogen:20~10:1, then by feeding
Device is sent into hydride powder, obtains spherical titanium nitride.
Preferably, in a steps, after arc stabilization, ionized gas is become to the mixed gas of argon gas and nitrogen.
Preferably, in the mixed gas of the argon gas and nitrogen, the volume ratio of argon gas and nitrogen is 1:5~10:1.
It is further preferred that in the mixed gas of the argon gas and nitrogen, preferably the volume ratio of argon gas and nitrogen is 1:2~
3:1。
Preferably, in b step, the grain size of hydride powder is 10~400 μm.
It is further preferred that the hydride powder is fed using vibration, amplitude is 10~80%.
Compared with prior art, the present invention has the advantages that：
The present invention uses radio frequency plasma equipment as reaction unit, using hydride powder as raw material, using nitrogen as reaction gas
Titanium nitride powder is prepared in body, a step, and technological process is short, the reaction time is extremely short, substantially increases production efficiency, acquisition
Product free from admixture pollutes, and preparation process is simple, relatively low to ingredient requirement, and the industrialized production to realize spherical titanium nitride powder is established
Basis is determined.
The spherical titanium nitride powder being prepared using the method for the present invention, Oxygen potential and nitriding rate are all very high.Prepare raw material
Do not need to be largely broken, particle size is small.
The present invention is applicable not only to the preparation of spherical nitridation titanium valve, is also applied for spherical nitridation zirconium powder and other nitridation ball powder
Preparation.
Description of the drawings
Fig. 1 is the XRD diagram of titanium nitride prepared by the present invention.
Fig. 2 is the SEM figures of titanium nitride 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；
B, feeding：After arc stabilization, it is 1 to control the flow-rate ratio of the argon gas being passed through and nitrogen:20~10:1, then by feeding
Device is sent into hydride powder, and Direct-Nitridation while hydride powder dehydrogenation, nodularization, obtains the nitrogen of half melt in plasma torch
Change titanium；
C, nodularization：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 hydride powder dehydrogenation, nodularization, obtains spherical titanium nitride in gas ions torch.Its reaction principle is：
TiH2=Ti+H2
2Ti+N2=2TiN
The method of the present invention, above-mentioned two-step reaction are being passed through the radio frequency plasma high-temperature field condition of argon gas and nitrogen in next step
It carries out.First, argon gas is passed through from radio frequency plasma equipment center, i.e. ionized gas inlet is passed through, and nitrogen is from radio frequency etc.
Gas ions device end is passed through, i.e., is passed through at gas atmosphere inlet.Argon gas stream is easy to generate plasma jet in this way, by titantium hydride object
Material carries out pyrolytic.Nitrogen is passed through from radio frequency plasma powder production device end can make nitridation reaction more complete.It should
The titanium nitride Oxygen potential and nitriding rate that method obtains are higher, and 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 to the mixed gas of argon gas and nitrogen, at this point, argon gas nitrogen arc will be formed.In plasma torch
Nitrogen ionization as heat source for reaction while again be used as reactant, reacted at high temperature with titanium valve and directly obtain 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 in the mixed gas of the argon gas and nitrogen, the volume ratio of argon gas and nitrogen is 1:5~10:1, more
Preferably, the volume ratio of argon gas and nitrogen is 1:2~3:1.When ionized gas is mixed gas, total argon that control is passed through is still needed to
The flow-rate ratio of gas and total nitrogen is 1:20~10:1.In the present invention, nitrogen or argon gas, the unit of flow use
m3/h。
The grain size of common hydride powder is suitable for the present invention, it is preferred that in b step, the grain size of hydride powder is 40
~100 μm.
Preferably, the hydride powder is fed using vibration, and amplitude is 10~80%, can cause hydrogen in this way
The reaction for changing titanium valve is more complete, improves nitriding rate.
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.The life of radio frequency plasma powder is set
The amplitude for producing the feed arrangement of equipment is 20%, operating voltage 10.5kV, power 48kW." side gas " (i.e. gas atmosphere inlet) is logical
Enter nitrogen, " middle gas " (i.e. ionized gas entrance) is first passed through the argon gas starting the arc, is passed through the mixing of argon gas and nitrogen again after arc stabilization
Gas, it is 2 to control nitrogen flow and argon flow amount ratio:1, spherical titanium nitride powder is prepared in feeding reaction 5min rewindings.Its
XRD spectrum is shown in Fig. 1, and SEM spectrum is shown in Fig. 2.Oxygen potential reaches 80%, nitriding rate 83%.
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.The life of radio frequency plasma powder is set
The amplitude for producing the feed arrangement of equipment is 22%, operating voltage 11.5kV, power 55kW." side gas " (i.e. gas atmosphere inlet) is logical
Enter nitrogen, " middle gas " (i.e. ionized gas entrance) is passed through the argon gas starting the arc, and nitrogen flow and argon flow amount ratio are 1：1.Treat that arc is steady
Titantium hydride is sent into after fixed, feeding reaction 5min rewindings measure titanium nitride powder quality as 27g.Its XRD spectrum is similar with Fig. 1,
SEM spectrum is similar with Fig. 2.Oxygen potential reaches 82%, nitriding rate 76%.
Embodiment 3
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment.The life of radio frequency plasma powder is set
The amplitude for producing the feed arrangement of equipment is 24%, operating voltage 8kV, power 40kW." side gas " (i.e. gas atmosphere inlet) is passed through
Nitrogen, " middle gas " (i.e. ionized gas entrance) are first passed through the argon gas starting the arc, are passed through the mixed air of argon gas and nitrogen again after arc stabilization,
Nitrogen flow and argon flow amount ratio are 3:2, feeding reaction 5min rewindings measure titanium nitride powder quality as 28g.Its XRD diagram
Spectrum is similar with Fig. 1, and SEM spectrum is similar with Fig. 2.Oxygen potential reaches 88%, nitriding rate 78%.
Embodiment 4
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment.The life of radio frequency plasma powder is set
The amplitude for producing the feed arrangement of equipment is 10%, operating voltage 15kV, power 200kW." side gas " (i.e. gas atmosphere inlet) is logical
Enter nitrogen, " middle gas " (i.e. ionized gas entrance) is first passed through the argon gas starting the arc, is passed through the mixing of argon gas and nitrogen again after arc stabilization
Gas, nitrogen flow and argon flow amount ratio are 3:20, feeding reaction 5min rewindings measure titanium nitride powder quality as 19g.Its
XRD spectrum is similar with Fig. 1, and SEM spectrum is similar with Fig. 2.Oxygen potential reaches 91%, nitriding rate 56%.
Embodiment 5
Spherical titanium nitride powder is produced using radio frequency plasma powder production equipment.The life of radio frequency plasma powder is set
The amplitude for producing the feed arrangement of equipment is 80%, operating voltage 12kV, power 60kW." side gas " (i.e. gas atmosphere inlet) is passed through
Nitrogen, " middle gas " (i.e. ionized gas entrance) are first passed through the argon gas starting the arc, are passed through the mixed air of argon gas and nitrogen again after arc stabilization,
Nitrogen flow and argon flow amount ratio are 9:10, feeding reaction 5min rewindings measure titanium nitride powder quality as 42g.Its XRD diagram
Spectrum is similar with Fig. 1, and SEM spectrum is similar with Fig. 2.Oxygen potential reaches 81%, nitriding rate 68%.
Claims (6)
1. the preparation method of spherical titanium nitride, it is characterised in that：Be prepared using radio frequency plasma equipment, specifically include as
Lower step：
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；
B, feeding：After arc stabilization, it is 1 to control the flow-rate ratio of the argon gas being passed through and nitrogen:20~10:1, then by feed device
Hydride powder is sent into, obtains spherical titanium nitride.
2. the preparation method of spherical shape titanium nitride according to claim 1, it is characterised in that：In a steps, after arc stabilization,
Ionized gas is become to the mixed gas of argon gas and nitrogen.
3. the preparation method of spherical shape titanium nitride according to claim 2, it is characterised in that：The mixing of the argon gas and nitrogen
In gas, the volume ratio of argon gas and nitrogen is 1:5~10:1.
4. the preparation method of spherical shape titanium nitride according to claim 3, it is characterised in that：The mixing of the argon gas and nitrogen
In gas, preferably the volume ratio of argon gas and nitrogen is 1:2~3:1.
5. according to the preparation method of Claims 1 to 4 any one of them spherical shape titanium nitride, it is characterised in that：In b step, hydrogen
The grain size for changing titanium valve is 10~400 μm.
6. according to the preparation method of Claims 1 to 5 any one of them spherical shape titanium nitride, it is characterised in that：The titantium hydride
Powder is fed using vibration, and amplitude is 10~80%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109437132A (en) * | 2018-12-14 | 2019-03-08 | 中信锦州金属股份有限公司 | A kind of production method nitrogenizing titanium valve |
| CN110157937A (en) * | 2019-04-09 | 2019-08-23 | 中国科学院金属研究所 | A kind of titanium nitride block preparation method that ingredient is controllable |
| CN111620313A (en) * | 2020-06-09 | 2020-09-04 | 合肥中航纳米技术发展有限公司 | Process for preparing nano titanium nitride powder by chemical vapor deposition method |
| CN114920218A (en) * | 2022-04-28 | 2022-08-19 | 湖南天际智慧材料科技有限公司 | Process for preparing nitride nano or and submicron powder material |
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