CN108910885A - A kind of spherical shape TiC powder and preparation method thereof - Google Patents
A kind of spherical shape TiC powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of spherical shape TiC powder, which is characterized in that used raw material is the irregular TiC powder of shape, and the preparation process of spherical TiC powder is radio frequency plasma nodularization method, and preparation flow comprises the steps of：(1) it sieves；(2) nodularization；(3) it cleans；(4) dry.Radio frequency plasma nodularization system model TekSphero-40 KW SY165 used in radio frequency plasma nodularization method.The carbonized titanium powder for the original irregular pattern that the present invention uses by plasma spheroidization equipment can be obtained high Oxygen potential (>90%), high sphericity, high-bulk-density, hypoxic spherical carbide titanium valve, binary, ternary, quaternary compound solid solution can be formed with tungsten carbide, tantalum carbide, niobium carbide, chromium carbide, titanium nitride, be applied to sprayed on material, welding material, hard thin film material, military aviation material, hard alloy and cermet.
Description
Technical field
The present invention relates to metal powder preparation technical field, in particular to a kind of spherical shape TiC powder and preparation method thereof.
Background technique
Material, information, the energy, biology are that 21 century fast development has revolutionary industry, wherein the material of various characteristics
Material has been widely applied in daily life and high-tech industry, therefore it is current material that research and development, which prepare the various materials haveing excellent performance,
Expect the key of development in science and technology.TiC powder is due to the property such as high temperature resistant, wear-resisting, corrosion-resistant, high-intensitive, high rigidity, thermal conductivity
Can and be widely used in making the fields such as ceramics, cutting tool, wearing-proof refractory material, aviation and metallurgy.One kind is explored at present
Efficient energy-saving method be prepared purity is high, even particle size distribution, particle agglomeration it is small, close to the TiC powder of stoichiometry be state
Inside and outside vast investigation of materials person's focus of attention.
It is widely used in steel hard alloy.Have high intensity, high rigidity, height resistance to the steel bonded carbide of TiC production
Mill property can carry out machining and cheap feature, and annual demand is all being continuously increased both at home and abroad, the scope of application
Expanding.The main hard phase of such alloy is titanium boride, relatively high to titanium boride requirement, and especially carbon content, oxygen content, nitrogen contain
It is tighter to measure three norm controllings.
It is widely used in ceramal.Due to the inherent characteristic of TiC powder, it is widely used in ceramal, and titanium
The oxide that can generate a variety of valence states is reacted with oxygen, and most of oxides are unstable, therefore titanium carbide too high oxygen level
It is easy to cause the unstable and compactness of alloy structure poor.Therefore the powder also requires oxygen content low；
It is widely used in wear-resistant material.Wear-resisting and hard material is to develop faster industry in nearly 2 years, is wanted to TiC powder
Ask also required in addition to physics and chemical index are up to standard particle intensity will well and uniform particle sizes concentrate.
The TiC powder of 6-30% is added in the hard alloy of tungsten-cobalt carbide system, the solid solution of titanium carbide-titanium carbide tungsten can be formed
The performances such as alloy red hardness, wearability, inoxidizability corrosion resistance can be improved in body, are more suitable for processing steel than WC-Co hard alloy
Material.It is widely used in carbide alloy cutting tool product；Tungsten-free cemented carbide is made as binder applied to alloys such as Ni-Mo,
Precision, the finish of turning speed and workpiece can be improved.
As additive for making thermistor, wearability is improved.
With the continuous development that spherical carbide titanium valve is applied, the demand of spherical carbide titanium valve is quicklyd increase.It is high-purity, low
Cost and stabilized spherical carbide titanium valve production technology have become the hot spot of domestic and international Preparation Technique of Powders exploitation.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of micron-size spherical TiC powder and its preparation sides
Method, the present invention use following technical scheme：
A kind of preparation method of spherical shape TiC powder, which is characterized in that used raw material is the irregular TiC powder of shape,
The preparation process of spherical TiC powder is radio frequency plasma nodularization method, and preparation flow comprises the steps of：
(1) in screening system, to starting powder TiC dressing sieve point；
(2) in plasma spheroidization system, nodularization is carried out to starting powder；
(3) in cleaning equipment, the powder after nodularization is cleaned；
(4) in drying system, the powder after cleaning is dried, final products are obtained.
Preferably, screening plant model Artech used in preparation step (1), powder diameter after screening is 15~
45μm。
Preferably, radio frequency plasma nodularization system model used in the radio frequency plasma nodularization method
TekSphero-40KW SY165。
Preferably, the radio frequency plasma nodularization system powder feeder revolving speed is set as 2~6r/min, between powder feeder powder feeding
Gap is set as 0.6~1mm, powder feeder probe model SI792, and powder feeder probe height is set as -12~0mm, argon gas sheath gas
Flow 45~50splm of flow, hydrogen sheath 6~15splm of air flow rate, argon gas center gas 17~23splm of air flow rate, powder feeding gas
Body flow is 2.5~5splm.
Preferably, the time of cleaning described in step (3) be 2~7min, 500~600r/min of revolving speed, wash number 2~
3 times, cleansing medium is deionized water.
Preferably, in step (4), the vacuum drying, temperature is set as 60~100 DEG C, and soaking time is set as 0.5
~2h.
A kind of spherical shape TiC powder, is prepared by any of the above-described preparation method.
Protective gas uses 99.99% high-purity argon and 99.99% height when the radio frequency plasma nodularization equipment works
Pure hydrogen.
Plasma nodularization equipment operation process of the present invention is as follows：System switching is opened, manual mode is selected, opens master
Power supply determines powder feeder probe height and powder feeding gap, sets powder feeder revolving speed, and cooling system booting selects water cooling and probe
It is cooling, powder feeder and reaction chamber connection switch are opened, purification system (beating) is opened, and after purification, closes powder feeder and reaction chamber
Switch, adjusting reaction room pressure to 2.0psi are opened vacuum system and argon gas switch, purification reaction room and receipts powder device, are adjusted
Whole argon gas sheath air flow rate adjusts argon gas center gas air flow rate, after aforesaid operations, opens radio frequency plasma power supply,
Radio frequency plasma system steady operation is waited, dispersion gas is adjusted to 1.5psi, adjusts hydrogen sheath air flow rate, regulation power is extremely
40kw adjusts chamber pressure to 15psi, adjusts powder feeding gas flow, open powder feeder valve, open ultrasound, equipment starts
Into production procedure.
The working principle and advantage of plasma spheroidization equipment：Irregular carbonized titanium powder is sent into pdp body torch, in spoke
Penetrate, convection current, under the transmission mechanism effect of heat transfer, in a very short period of time, metallic particles is melt into droplet, on surface
The very high particle of sphericity is shrunk under the action of power, high temperature drop is quickly cooled down, and forms micro-sized metal carbonized titanium powder.Plasma
Body nodularization is a kind of processing method of high-efficiency and economic, it can improve the physics and chemical characteristic of processing powder, is mainly manifested in
Following several aspects：Improve powder flowbility, it is not in clogging that spheroidized particle, which guarantees powder feeding Uniform Flow,；Subtract
The porosity of small powder, the molten condition during powder-processed can eliminate hole, it is possible thereby in powder metallurgy and densification
Better characteristics is obtained in coating application；Improve powder density；Nodularization particle can be improved powder and using after such powder
Coating and component total body density；Reduce powder brittleness：Behind the surface of nodularization powder spray to components, hair can be reduced
Thorn, reduces dusting, flaking and broken；Improve particle surface finish；Individual particles impulse- free robustness can greatly improve micro-
Finish.It is largely effective in requiring the application that coefficient of friction is low and gas transport does not pollute pipeline.
Beneficial effects of the present invention：The carbonized titanium powder for the original irregular pattern that the present invention uses passes through plasma spheroidization
Equipment can be obtained high Oxygen potential (>90%), high sphericity, high-bulk-density, hypoxic spherical carbide titanium valve, Ke Yiyu
Tungsten carbide, tantalum carbide, niobium carbide, chromium carbide, titanium nitride form binary, ternary, quaternary compound solid solution, are applied to spraying material
Material, welding material, hard thin film material, military aviation material, hard alloy and cermet.Carbonized titanium powder in the method for the present invention
Ingredient, partial size, sphericity are controllable, and spherical TiC powder sphericity height, good fluidity, the partial size prepared are small, and are evenly distributed, are miscellaneous
Matter is few, compactness is high, technique more rapidly, simple and direct, one-pass molding, it is at low cost, have good industrial prospect.
Detailed description of the invention
Fig. 1 TekSphero-40KW SY165 nodularization equipment drawing.
Fig. 2 TiC powder raw material pattern.
Spherical TiC powder pattern prepared by Fig. 3 embodiment 1.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Unless otherwise indicated, raw material additional amount percentage employed in the following example of the present invention is mass percent.
Embodiment 1：
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm.(1) in screening system, to starting powder TiC dressing sieve point, the screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 1mm, probe height -10mm, powder feeder revolving speed 2r/min, argon gas sheath air flow rate 50splm,
Hydrogen sheath air flow rate 6splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 3splm.(3) in cleaning equipment
In, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：Water is added to rinse
2min, dehydrating speed 500r/min, second dehydration parameter are：Water is added to rinse 3min, dehydrating speed 500r/min.(4) exist
In drying system, the powder after cleaning is dried, slurry is put into 100 DEG C of heat preservation 1h of vacuum oven, obtains final products.
Product Oxygen potential is up to 85%.
Embodiment 2
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm, and (1) divides starting powder TiC dressing sieve in screening system；The screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 1mm, probe height -10mm, powder feeder revolving speed 2r/min, argon gas sheath air flow rate 50splm,
Hydrogen sheath air flow rate 9splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 3splm.(3) in cleaning equipment
In, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：Water is added to rinse
2min, dehydrating speed 500r/min, second dehydration parameter are：Water is added to rinse 3min, dehydrating speed 500r/min.(4) exist
In drying system, the powder after cleaning is dried, slurry is put into 100 DEG C of heat preservation 1h of vacuum oven, obtains final products.
Product Oxygen potential is up to 93%.
Embodiment 3：
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm.(1) in screening system, to starting powder TiC dressing sieve point；The screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 1mm, probe height -10mm, powder feeder revolving speed 2r/min, argon gas sheath air flow rate 50splm,
Hydrogen sheath air flow rate 12splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 3splm.(3) in cleaning equipment
In, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：Water is added to rinse
2min, dehydrating speed 500r/min, second dehydration parameter are：Water is added to rinse 3min, dehydrating speed 500r/min.(4) exist
In drying system, the powder after cleaning is dried, slurry is put into 100 DEG C of heat preservation 1h of vacuum oven, obtains final products.
Oxygen potential is up to 98%.
Embodiment 4：
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm.(1) in screening system, to starting powder TiC dressing sieve point；The screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 0.6mm, probe height -10mm, powder feeder revolving speed 4r/min, argon gas sheath air flow rate
50splm, hydrogen sheath air flow rate 15splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 3splm.(3) exist
In cleaning equipment, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：Add
Water rinses 4min, dehydrating speed 500r/min, and second dehydration parameter is：Water is added to rinse 6min, dehydrating speed 600r/min.
(4) in drying system, the powder after cleaning is dried, slurry is put into 80 DEG C of heat preservation 1h of vacuum oven, obtains final
Product.Oxygen potential up to 98%,
Embodiment 5：
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm.(1) in screening system, to starting powder TiC dressing sieve point；The screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 0.6mm, probe height -10mm, powder feeder revolving speed 5r/min, argon gas sheath air flow rate
50splm, hydrogen sheath air flow rate 15splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 3splm.(3) exist
In cleaning equipment, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：Add
Water rinses 2min, dehydrating speed 500r/min, and second dehydration parameter is：Water is added to rinse 3min, dehydrating speed 500r/min.
(4) in drying system, the powder after cleaning is dried, slurry is put into 100 DEG C of heat preservation 0.5h of vacuum oven, obtains most
Finished product.Oxygen potential up to 98%,
Embodiment 6：
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm.(1) in screening system, to starting powder TiC dressing sieve point；The screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 0.6mm, probe height -10mm, powder feeder revolving speed 6r/min, argon gas sheath air flow rate
50splm, hydrogen sheath air flow rate 15splm, argon gas central fluidizing gas flow 20splm, powder feeding gas flow are 3splm.(3) exist
In cleaning equipment, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：Add
Water rinses 2min, dehydrating speed 500r/min, and second dehydration parameter is：Water is added to rinse 3min, dehydrating speed 500r/min.
(4) in drying system, the powder after cleaning is dried, slurry is put into 60 DEG C of heat preservation 2h of vacuum oven, obtains final
Product.Oxygen potential up to 98%,
Embodiment 7：
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm.(1) in screening system, to starting powder TiC dressing sieve point；The screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 0.8mm, probe height 0mm, powder feeder revolving speed 5r/min, argon gas sheath air flow rate 48splm,
Hydrogen sheath air flow rate 6splm, argon gas central fluidizing gas flow 17splm, powder feeding gas flow are 5splm.(3) in cleaning equipment
In, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：Water is added to rinse
7min, dehydrating speed 600r/min, second dehydration parameter are：Water is added to rinse 3min, dehydrating speed 600r/min takes off three times
Water parameter is：Water is added to rinse 6min, dehydrating speed 600r/min.(4) in drying system, the powder after cleaning is dried
Dry, slurry is put into 100 DEG C of heat preservation 1h of vacuum oven, obtains final products.Oxygen potential is up to 98%.
Embodiment 8：
The preparation method of micron-size spherical carbonized titanium powder, raw material use original silicon carbide titanium valve in irregular shape, powder rule
Lattice are 15~53 μm.(1) in screening system, to starting powder TiC dressing sieve point；The screening plant model Artech used,
Powder diameter after screening is 15~45 μm.(2) in plasma spheroidization system, nodularization is carried out to starting powder；It is used
Radio frequency plasma nodularization device model be TekSphero-40KW SY165.Nodularization parameter setting is：Powder feeder probe type
Number be SI792, powder feeding gap be 0.6mm, probe height -12mm, powder feeder revolving speed 6r/min, argon gas sheath air flow rate
45splm, hydrogen sheath air flow rate 15splm, argon gas central fluidizing gas flow 23splm, powder feeding gas flow are 2.5splm.(3)
In cleaning equipment, cleaning classification is carried out to the powder after nodularization；Nodularization powder cleaning process is as follows, and primary dewatering parameter is：
Water is added to rinse 2min, dehydrating speed 550r/min, second dehydration parameter is：Water is added to rinse 5min, dehydrating speed 550r/
min.(4) in drying system, the powder after cleaning is dried, slurry is put into 90 DEG C of heat preservation 1h of vacuum oven, obtains
Final products.Oxygen potential is up to 98%.
Performance test：
TiC powder mobility, tap density, pine before and after the spherical TiC powder prepared in above-described embodiment 1 progress nodularization are filled close
Degree test, test result such as table one：
Table one：Carbonized titanium powder mobility, tap density, apparent density before and after nodularization
Above-described embodiment is merely illustrative of the technical solution of the present invention and is not intended to limit it, all without departing from the present invention
Any modification of spirit and scope or equivalent replacement should all cover the range in technical solution of the present invention.
Claims (7)
1. a kind of preparation method of spherical shape TiC powder, which is characterized in that used raw material is the irregular TiC powder of shape, ball
The preparation process of shape TiC powder is radio frequency plasma nodularization method, and preparation flow comprises the steps of：
(1) in screening system, to starting powder TiC dressing sieve point；
(2) in plasma spheroidization system, nodularization is carried out to starting powder；
(3) in cleaning equipment, the powder after nodularization is cleaned；
(4) in drying system, the powder after cleaning is dried, final products are obtained.
2. a kind of preparation method of spherical shape TiC powder according to claim 1, which is characterized in that used in preparation step (1)
Screening plant model Artech, powder diameter after screening is 15~45 μm.
3. a kind of preparation method of spherical shape TiC powder according to claim 1, which is characterized in that the radio frequency plasma
Radio frequency plasma nodularization system model TekSphero-40KW SY165 used in nodularization method.
4. a kind of preparation method of spherical shape TiC powder according to claim 1, which is characterized in that the radio frequency plasma ball
Change system powder feeder revolving speed is set as 2~6r/min, and powder feeder powder feeding gap is set as 0.6~1mm, powder feeder probe model
SI792, powder feeder, which is popped one's head in, is highly set as -12~0mm, argon gas sheath 45~50splm of air flow rate, and hydrogen sheath air flow rate 6~
15splm, argon gas center gas 17~23splm of air flow rate, powder feeding gas flow are 2.5~5splm.
5. a kind of preparation method of micron-size spherical TiC powder according to claim 1, which is characterized in that institute in step (3)
The time for stating cleaning is 2~7min, and 500~600r/min of revolving speed, wash number 2~3 times, cleansing medium is deionized water.
6. a kind of preparation method of micron-size spherical TiC powder according to claim 1, which is characterized in that in step (4),
The vacuum drying, temperature are set as 60~100 DEG C, and soaking time is set as 0.5~2h.
7. a kind of spherical shape TiC powder, which is characterized in that spherical TiC powder be by the preparation of any one of claim 1 to 6 preparation method and
At.
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| CN109702189A (en) * | 2019-03-14 | 2019-05-03 | 上海海事大学 | A kind of production method of cochrome base spherical carbide niobium powder body |
| CN111422874A (en) * | 2020-03-27 | 2020-07-17 | 上海海事大学 | Method for producing spherical titanium carbide powder by one-step method |
| CN113800522A (en) * | 2021-09-27 | 2021-12-17 | 星尘科技(广东)有限公司 | Method for preparing high-purity compact tungsten carbide-cobalt composite spherical powder material |
| 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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| CN109368645B (en) * | 2018-12-26 | 2021-11-23 | 吉林大学 | Preparation method of array Z-shaped niobium carbide microcrystal |
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| CN111422874A (en) * | 2020-03-27 | 2020-07-17 | 上海海事大学 | Method for producing spherical titanium carbide powder by one-step method |
| CN113800522A (en) * | 2021-09-27 | 2021-12-17 | 星尘科技(广东)有限公司 | Method for preparing high-purity compact tungsten carbide-cobalt composite spherical powder material |
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| CN114920218B (en) * | 2022-04-28 | 2024-01-05 | 湖南天际智慧材料科技有限公司 | Preparation process of nitride nano or submicron powder material |
| CN116023125A (en) * | 2022-12-29 | 2023-04-28 | 武汉理工大学 | High-hardness transparent ceramic microsphere and preparation method thereof |
| CN116023125B (en) * | 2022-12-29 | 2024-02-27 | 武汉理工大学 | High-hardness transparent ceramic microsphere and preparation method thereof |
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