CN108274012A - A kind of method that aerosolization prepares spherical shape TiN - Google Patents
A kind of method that aerosolization prepares spherical shape TiN Download PDFInfo
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- CN108274012A CN108274012A CN201810089349.5A CN201810089349A CN108274012A CN 108274012 A CN108274012 A CN 108274012A CN 201810089349 A CN201810089349 A CN 201810089349A CN 108274012 A CN108274012 A CN 108274012A
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- tin
- aerosolization
- titanium
- spherical shape
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/02—Nitrogen
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The present invention relates to a kind of methods that aerosolization prepares spherical shape TiN, belong to the preparing technical field of titanium nitride powder.The technical problem to be solved by the present invention is to provide a kind of methods that aerosolization prepares spherical shape TiN.This method comprises the following steps：A, raw material titanium melts in a vacuum, after fusing, is filled with argon gas, vacuum degree is made to reach 1 × 103~5 × 104Pa obtains stable titanium liquid；B, titanium liquid is passed through the atomizer of aerosolizing device, while being passed through nitrogenous gas, and aerosolization forms fine droplet, then cools down, obtains spherical TiN.Spherical TiN is directly prepared using aerosolization in the present invention, and the preparation for spherical titanium nitride powder provides a kind of new preparation method.The spherical TiN beaten is prepared into using this method, Oxygen potential and nitriding rate are all higher, and this method reaction time is short, production efficiency is substantially increased, the product free from admixture of acquisition pollutes, and preparation process is simple, it is relatively low to ingredient requirement, to realize that the industrialized production of spherical titanium nitride powder is laid a good foundation.
Description
Technical field
The present invention relates to a kind of methods that aerosolization prepares spherical shape TiN, belong to the preparing technical field of 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 hardness 1990 (× 9.8N/mm2).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
The excellent properties that degree and depth are possessed with it are extremely unbecoming, need people and research and develop, can indicate, titanium nitride powder will
As century new material.
As that studies TiN 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 cover the solution of problem above.
And compared with aspherical titanium nitride powder, the mechanical performance of spherical titanium nitride is the same in all directions,
The product haveing excellent performance more 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
The preparation method of high spherical shape titanium nitride.
Invention content
The present invention in view of the foregoing drawbacks, provides a kind of method preparing spherical shape TiN using aerosolization stove, titanium valve is in aerosolization
Direct-Nitridation while nodularization in stove.
The method that aerosolization of the present invention prepares spherical shape TiN, is prepared spherical TiN, including as follows using aerosolizing device
Step：
A, raw material titanium melts in a vacuum, ensures that vacuum degree is 1 × 10-4~1Pa after fusing, is filled with argon gas, makes vacuum degree
Reach 1 × 103~5 × 104Pa obtains titanium liquid；
B, titanium liquid is passed through the atomizer of aerosolizing device, while being passed through nitrogenous gas, and aerosolization forms fine droplet, so
Postcooling obtains spherical TiN, wherein the nitrogenous gas is the mixed gas or pure nitrogen gas of nitrogen and inert gas.
Preferably, the raw material titanium is at least one of stud, titanium plate.
It is further preferred that in a steps, the temperature of the titanium liquid is 1600~1800 DEG C.
Preferably, in b step, the flow velocity of titanium liquid is 20~500g/s；It is further preferred that in b step, the flow velocity of titanium liquid
For 100~300g/s.
Preferably, in b step, the flow of nitrogenous gas is 3~20m3/h；It is further preferred that in b step, contain nitrogen
The flow of body is 6~12m3/h。
Preferably, in the nitrogenous gas of b step, the percent by volume of nitrogen is 50% or more.
It is further preferred that b step, inert gas is helium, argon gas, neon or Krypton.
Preferably, the cooling described in b step carries out in a vacuum chamber.
Compared with prior art, the present invention has the advantages that：
Spherical TiN is directly prepared using aerosolization in the present invention, and the preparation for spherical titanium nitride powder provides one kind
New preparation method.The spherical titanium nitride powder beaten is prepared into using this method, Oxygen potential and nitriding rate are all higher, and this method
Reaction time is short, substantially increases production efficiency, and the product free from admixture pollution of acquisition, preparation process is simple, to ingredient requirement compared with
It is low, to realize that the industrialized production of spherical titanium nitride powder is laid a good foundation.
Specific implementation mode
The technical problem to be solved by the present invention is to provide a kind of methods that aerosolization prepares spherical shape TiN.
The method that aerosolization of the present invention prepares spherical shape TiN, includes the following steps：
A, raw material titanium melts in a vacuum, ensures that vacuum degree is 1 × 10-4~1Pa after fusing, is filled with argon gas, makes vacuum degree
Reach 1 × 103~5 × 104Pa obtains stable titanium liquid；
B, titanium liquid is passed through the atomizer of aerosolizing device, while being passed through nitrogenous gas, and aerosolization forms fine droplet, so
Postcooling obtains spherical TiN, wherein the nitrogenous gas is the mixed gas or pure nitrogen gas of nitrogen and inert gas.
The method that aerosolization of the present invention prepares spherical shape TiN is passed through nitrogenous gas using the method for aerosol powder, in nodularization
While nitrogenized, simple for process, the reaction time is short, substantially increases production efficiency.
Raw material titanium commonly used in the art is suitable for the present invention.Preferably, the raw material titanium be stud, in titanium plate at least
It is a kind of.
The temperature of titanium liquid influences atomizing effect, it is preferred that the temperature of the titanium liquid is 1600~1800 DEG C, as preferred side
The temperature of case, titanium liquid is 1700~1800 DEG C.
In order to improve Oxygen potential and nitriding rate, it is preferred that the flow velocity of titanium liquid is 20~500g/s, preferably, titanium
The flow velocity of liquid is 100~300g/s.
The flow of nitrogenous gas has a certain impact to nodularization and nitridation, and the flow of nitrogenous gas is too small, and Oxygen potential is not high,
And nitridation reaction also can be incomplete；And the flow of nitrogenous gas is excessive, not only results in the waste of raw material, can also cause nodularization
The grain size of TiN is uneven, and Oxygen potential declines instead.Therefore, in order to improve nitriding rate and Oxygen potential, it is preferred that the stream of nitrogenous gas
Amount is 3~20m3/h；The flow of more preferable nitrogenous gas is 6~12m3/h。
In order to improve nitriding rate, nitrogen content in nitrogenous gas cannot be too low.Preferably, the nitrogen and argon gas is mixed
It closes in gas, the percent by volume of nitrogen is 50% or more.
Common inert gas is suitable for the present invention, it is preferred that the inert gas is helium, argon gas, neon or krypton
Gas.
Preferably, the cooling of b step carries out in a vacuum chamber.
Spherical titanium nitride is directly obtained by the reaction in the method for the present invention in aerosolizing device.Aerosolization commonly used in the art is set
It is standby to be suitable for the present invention.Preferably, the aerosolizing device includes atomizer, the atomizer be equipped with fluid course with
And the gas channel around fluid course setting, titanium liquid is imported from fluid course, and nitrogenous gas is passed through from gas channel.
Method using the present invention, the spherical TiN grain sizes being prepared are 5~250 μm.
The specific implementation mode 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
Setting aerosolization stove melting voltage 30kV, soak voltage 20kV, vacuum degree 1Pa make stud and titanium plate in aerosol
Change and is melted in stove.It after fusing, is passed through and is filled with argon gas, vacuum degree is made to reach 1 × 103Pa obtains stable titanium liquid, is by temperature
The titanium liquid of 1700 DEG C of stabilization pours into nozzle, is flowed down by nozzle, coutroi velocity 200g/s.It is passed through nitrogen, adjusts flow
For 6m3/ h, titanium liquid are blown for fine droplet, are then cooled down, and it is 120g that rewinding, which measures titanium nitride powder quality,.Its Oxygen potential is
83%, nitriding rate 54%, powder diameter is 10~220 μm.
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 X-ray diffractometer analysis result to obtain.
Embodiment 2
Aerosolization stove melting voltage 30kV is set, and soak voltage 20kV, vacuum degree is 1 × 10-4Pa makes stud and titanium plate exist
It is melted in aerosolization stove.It after fusing, is passed through and is filled with argon gas, vacuum degree is made to reach 5 × 104Pa obtains stable titanium liquid, by temperature
Nozzle is poured into for the titanium liquid of 1750 DEG C of stabilizations, is flowed down by nozzle, coutroi velocity 100g/s.It is passed through nitrogen and argon gas
The percent by volume of gaseous mixture, nitrogen is 80%, and adjusting flow is 10m3/ h, it is 164g that rewinding, which measures titanium nitride powder quality,.
Its Oxygen potential is 71%, nitriding rate 66%, and powder diameter is 12~220 μm.
Embodiment 3
Aerosolization stove melting voltage 30kV is set, and soak voltage 20kV, vacuum degree is 1 × 10-2Pa makes stud and titanium plate exist
It is melted in aerosolization stove.It after fusing, is passed through and is filled with argon gas, vacuum degree is made to reach 1 × 104Pa obtains stable titanium liquid, by temperature
Nozzle is poured into for the titanium liquid of 1800 DEG C of stabilizations, is flowed down by nozzle, coutroi velocity 200g/s.It is passed through nitrogen and argon gas
The percent by volume of gaseous mixture, nitrogen is 50%, and adjusting flow is 12m3/ h, it is 120g that rewinding, which measures titanium nitride powder quality,.
Its Oxygen potential is 74%, nitriding rate 61%, and powder diameter is 10~250 μm.
Claims (8)
1. a kind of method that aerosolization prepares spherical shape TiN, which is characterized in that spherical TiN is prepared using aerosolizing device, wraps
Include following steps：
A, raw material titanium melts in a vacuum, ensures that vacuum degree is 1 × 10-4~1Pa after fusing, is filled with argon gas, vacuum degree is made to reach
1×103~5 × 104Pa obtains titanium liquid；
B, titanium liquid is passed through the atomizer of aerosolizing device, while being passed through nitrogenous gas, and aerosolization forms fine droplet, then cold
But, spherical TiN is obtained, wherein the nitrogenous gas is the mixed gas or pure nitrogen gas of nitrogen and inert gas.
2. the method that aerosolization according to claim 1 prepares spherical shape TiN, it is characterised in that：The raw material titanium be stud,
At least one of titanium plate.
3. the method that aerosolization according to claim 1 prepares spherical shape TiN, it is characterised in that：In a steps, the titanium liquid
Temperature be 1600~1800 DEG C.
4. the method that aerosolization according to claim 1 prepares spherical shape TiN, it is characterised in that：In b step, the stream of titanium liquid
Speed is 20~500g/s；It is preferred that in b step, the flow velocity of titanium liquid is 100~300g/s.
5. the method that aerosolization according to claim 1 prepares spherical shape TiN, it is characterised in that：In b step, nitrogenous gas
Flow be 3~20m3/h；It is preferred that in b step, the flow of nitrogenous gas is 6~12m3/h。
6. the method that aerosolization according to claim 1 prepares spherical shape TiN, it is characterised in that：The nitrogenous gas of b step
In, the percent by volume of nitrogen is 50% or more.
7. the method that aerosolization according to claim 1 prepares spherical shape TiN, it is characterised in that：B step, inert gas are
Helium, argon gas, neon or Krypton.
8. the method that aerosolization according to claim 1 prepares spherical shape TiN, it is characterised in that：Cooling described in b step exists
It is carried out in vacuum chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810089349.5A CN108274012A (en) | 2018-01-30 | 2018-01-30 | A kind of method that aerosolization prepares spherical shape TiN |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810089349.5A CN108274012A (en) | 2018-01-30 | 2018-01-30 | A kind of method that aerosolization prepares spherical shape TiN |
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| CN108274012A true CN108274012A (en) | 2018-07-13 |
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| CN201810089349.5A Pending CN108274012A (en) | 2018-01-30 | 2018-01-30 | A kind of method that aerosolization prepares spherical shape TiN |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112024899A (en) * | 2020-09-04 | 2020-12-04 | 上海大学 | TiN-Ti composite powder and preparation method and application thereof |
| CN112475309A (en) * | 2020-12-15 | 2021-03-12 | 江苏金物新材料有限公司 | Method for preparing spherical titanium nitride powder by reaction atomization method |
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| JPS6168311A (en) * | 1984-09-10 | 1986-04-08 | Chugai Ro Kogyo Kaisha Ltd | Process and apparatus for preparing aluminum nitride powder |
| JPS61132505A (en) * | 1984-12-01 | 1986-06-20 | Daido Steel Co Ltd | Production of tin powder |
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| CN103769594A (en) * | 2013-11-25 | 2014-05-07 | 王利民 | Technological method and device for preparing high-purity spherical superfine/nanoscale powdered materials in plasma atomization mode |
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| GB2048955B (en) * | 1979-04-05 | 1983-01-26 | Atomic Energy Authority Uk | Titanium nitride strengthened alloys |
| JPS6168311A (en) * | 1984-09-10 | 1986-04-08 | Chugai Ro Kogyo Kaisha Ltd | Process and apparatus for preparing aluminum nitride powder |
| JPS61132505A (en) * | 1984-12-01 | 1986-06-20 | Daido Steel Co Ltd | Production of tin powder |
| DE19623351A1 (en) * | 1996-06-12 | 1997-12-18 | Geesthacht Gkss Forschung | Production of metal nitride powders |
| CN103769594A (en) * | 2013-11-25 | 2014-05-07 | 王利民 | Technological method and device for preparing high-purity spherical superfine/nanoscale powdered materials in plasma atomization mode |
| CN105883731A (en) * | 2015-01-22 | 2016-08-24 | 南京杰博宏镓新型材料有限公司 | Preparation method of compound powder material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112024899A (en) * | 2020-09-04 | 2020-12-04 | 上海大学 | TiN-Ti composite powder and preparation method and application thereof |
| CN112475309A (en) * | 2020-12-15 | 2021-03-12 | 江苏金物新材料有限公司 | Method for preparing spherical titanium nitride powder by reaction atomization method |
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Application publication date: 20180713 |
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