CN103130506A - Method for preparing superfine titanium carbonitride - Google Patents
Method for preparing superfine titanium carbonitride Download PDFInfo
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- CN103130506A CN103130506A CN2013100815510A CN201310081551A CN103130506A CN 103130506 A CN103130506 A CN 103130506A CN 2013100815510 A CN2013100815510 A CN 2013100815510A CN 201310081551 A CN201310081551 A CN 201310081551A CN 103130506 A CN103130506 A CN 103130506A
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Abstract
The invention belongs to the field of metal ceramic material preparation, and provides a method for preparing superfine titanium carbonitride. The method comprises the following steps of: firstly, ball-milling and mixing nano TiO2 with an organic carbon source, and preparing into a piece material in a cold pressing mode; feeding the piece material into a vacuum sensing furnace, vacuumizing till the pressure inside the furnace is less than or equal to 50Pa, increasing the temperature to 300-800 DEG C and preserving the temperature for 0.5-2h; subsequently increasing the temperature to be 1000-1900 DEG C and preserving the temperature for 0.5-2h, wherein vacuumizing is constantly performed in the temperature preservation process; stopping vacuumizing after the temperature preservation is accomplished, introducing nitrogen so as to make the pressure in the furnace be of 1.1-1.2 atmosphere pressures; preserving the temperature for 1-4h to sufficiently nitridize the raw material; and subsequently decreasing the temperature, taking out the piece material, crushing, ball-milling and grading so as to obtain the superfine titanium carbonitride of which the Fisher particle size is less than 1mm. A TiCN powder material prepared by using the method is high in purity, few in impurities, small in particle size, uniform in particle size distribution and spherical in morphology, and can be used as a raw material of a cutting tool, a metal ceramic, a spraying material and the like.
Description
Technical field
The invention belongs to the cermet material field, relate to a kind of method for preparing super fine titanium carbonitride.
Background technology
In recent years, because Ti (C, N) based ceramic metal has good wear resistance, high hot hardness, better oxidation-resistance and high temperature creep-resisting energy, be subject to people and more and more paid close attention to.In addition, the main raw material of making traditional Wimet is WC and Co, they are all rare strategic resources, and Ti (C, N) main raw material of based metal ceramic cutter material is Ti, Ti reserves on earth are 70 times 131 of W, therefore compare with traditional Wimet to have great cost and resources advantage.But the intensity of Ti (C, N) based ceramic metal and toughness but lower than traditional WC-Co series hard metal, have seriously limited ceramic-metallic application.If we can improve its intensity and toughness in the situation that do not reduce Ti (C, N) based ceramic metal premium properties, Ti (C, N) based ceramic metal will become the good cutting material that substitutes of traditional WC-Co series hard metal so.Therefore, according to Hall-Petch formula, utilize ultrafine powder to prepare superfine Ti (C, N) based ceramic metal is more and more with the research of the obdurability of raising material, but the technology of existing preparation TiCN powder is not that raw materials cost is high at present, the equipment complexity is exactly that quality product is low, is difficult to obtain that purity is high, even-grained high quality superfine Ti CN powder.
At present, the method for preparing the TiCN powder body material comprises: by carbodynamite at 1100 ℃ of pyrolytic decompositions; Utilize nano TiN and carbon black to react in the argon gas stream of 1300 ℃; Adopt sodium Metal 99.5 at 600 ℃ of reduction C
3N
3Cl
3And TiCl
4Mixture; Unite sol-gel technique and the carbothermic reduction technology (1550 ℃) used; Utilize gac to reduce TiO in the nitrogen of 900～1500 ℃
2Utilize titanium and carbon to carry out the self-propagating high-temperature reaction in nitrogen; Ball milling TiO in nitrogen for a long time
2, graphite and aluminium powder.And the existing method for preparing the TiCN powder is all one section reaction, and raw materials cost is high, and equipment complexity or quality product are low, is difficult to obtain that purity is high, granularity is little, the high quality TiCN powder of even particle size distribution.
Summary of the invention
For deficiency of the prior art, the present invention aims to provide a kind of method for preparing super fine titanium carbonitride, the principal feature of the method is to adopt organic carbon source, vacuum reducing carbonization fast in vacuum oven, prepared superfine Ti CN powder body material purity is high, impurity is few, granularity is less than 1 micron, and pattern is spherical, even particle size distribution, and cost is low, and technique is simple.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of method for preparing super fine titanium carbonitride, concrete steps are:
(1) with nano-TiO
2Mix with the organic carbon source ball milling, wherein nano-TiO
2With the mass ratio of contained C in organic carbon source be 10:1～4.8, then cold pressing and make the piece material;
(2) described block of material packed in vacuum induction furnace, be evacuated to furnace pressure less than or equal to 50Pa, then the heat-up rate with 5 ℃/min-8 ℃/min is warming up to 300 ℃-800 ℃, insulation 0.5 h-3h; Be warming up to 1000 ℃～1900 ℃, insulation 0.5 h～3h constantly vacuumizes in insulating process again;
After (3) (2) steps finish, pass into nitrogen, making furnace pressure is 1.1-1.2 normal atmosphere, continuation is incubated 1 h～4h under 1000 ℃～1900 ℃, make the abundant nitrogenize of raw material, then be cooled to 150 ℃～350 ℃, take out the piece material, fragmentation, ball milling, classification obtain Fisher particle size less than the carbon titanium nitride powder material of 1 micron.
The described nano-TiO of step (1)
2Preferred Fisher particle size is less than 100 nanometers, TiO
2Content is greater than 99%.
The carbon source of the described carbon source of step (1) is selected from polyvinyl alcohol, sucrose, starch, tartrate, oxalic acid or glucose.
The described nano-TiO of step (1)
2Be preferably 10:2～4 with the mass ratio of contained C in carbon source.
In preferred steps (2), described block of material packed in vacuum induction furnace, be evacuated to furnace pressure less than or equal to 50Pa, then the heat-up rate with 5 ℃/min-8 ℃/min is warming up to 350 ℃-650 ℃, insulation 0.5 h-2h; Be warming up to again 1100 ℃～1700 ℃, insulation 0.5 h～2h.
The speed that heats up again of step (2) does not have particular requirement, so that 3 ℃/min-8 ℃/min is better.
The described nitrogen gas purity of step (3) is preferably greater than 99%.
The below does further explanation and explanation to the present invention:
Principle of the present invention comprises decomposes coating, reduction and nitrogenize three phases: the 1st, and the decomposition of organic carbon source coats, being about to described block of material packs in vacuum induction furnace, be evacuated to furnace pressure less than or equal to 50Pa, then the heat-up rate with 5 ℃/min-8 ℃/min is warming up to 300 ℃-800 ℃, insulation 0.5 h-3h.The 2nd, step of reaction namely is warming up to 1000 ℃～1900 ℃ again, and insulation 0.5 h～3h constantly vacuumizes in insulating process.The 3rd, the nitrogenize stage, i.e. insulation stops vacuumizing after finishing, and passes into nitrogen, and making furnace pressure is 1.1-1.2 normal atmosphere, and insulation 1 h～4h makes the abundant nitrogenize of raw material, then is cooled to 150 ℃～350 ℃, takes out the piece material.
Decomposition at organic carbon source coats the stage, and organic carbon source melts, decomposes under vacuum state, generates fine carbon black, is enclosed in uniformly TiO
2Particle surface can play the effect of foaming when organic carbon fusing, decomposition, be that the material piece is loose, is conducive to the mass transfer of nitrogen; When decomposing, organic carbon produces superfine carbon granule, surround uniformly around the Nanometer Titanium Dioxide particle, not only can make the reaction fully fast at lower temperature of carbon and titanium white, the more important thing is that coating function due to carbon makes between the titanium white particle can directly not contact, thereby suppressed growing up of particle.
At reduction phase, be warming up to 1000 ℃～1900 ℃, with titanium white (TiO
2) fully reduction, excess carbon reduction TiO under vacuum state
2Chemical equation be TiO
2+ (2+x) C=Ti
y+ Ti
(1-y)C
x+ 2CO, wherein 0≤y≤1,0≤x≤1.The CO that generates due to reaction simultaneously is pumped rapidly, has also promoted carrying out rapidly and thoroughly of reaction, and O content wherein is reduced to less than 1%.
In the nitrogenize stage, work as TiO
2After fully being reduced by carbon, stop vacuumizing, pass into nitrogen, and make furnace pressure be slightly larger than a normal atmosphere, the metal Ti that at this moment reduction generates begins rapidly and the nitrogen reaction, generates titanium nitride, and its reaction formula is 2Ti+N
2The Ti that=2TiN, TiN generate with reduction phase again simultaneously
(1-y)C
x, wherein solid solution reaction, occur, thereby generate single-phase TiCN material in 0≤y≤1,0≤x≤1.
Compared with prior art, advantage of the present invention is:
1, method of the present invention comprises decomposition coating, reduction and nitrogenize three phases, the quality product that obtains is high, prepared superfine Ti CN powder body material purity tall and big in equal 99%, O content lower than 1%, few, the Fisher particle size of impurity is less than 1um, pattern is spherical, even particle size distribution.
2, method technique of the present invention is simple, and equipment requirements is low, cost is low, energy expenditure is less, be convenient to the advantage of large-scale commercial production.
Description of drawings
Fig. 1 and Fig. 2 are the SEM figure of the prepared product of the embodiment of the present application 1;
Fig. 3 and Fig. 4 are the SEM figure of German Stratco Inc. like product.
Embodiment
The present invention is described further below in conjunction with embodiment.
Embodiment 1:
A kind of method for preparing super fine titanium carbonitride adopts TiO
2With starch be raw material, with 100kg TiO
2Evenly mix (nano-TiO wherein with 87.5kg starch
2Mass ratio 10:3.85 with institute's carbon containing in organic carbon source), cold pressing and make the piece material, in the vacuum oven of packing into, speed with 5 ℃/min heats up rapidly, and vacuumizes simultaneously, makes vacuum tightness less than 50pa, after temperature rose to 700 ℃, then insulation 1h when continuing to rise to 1500 ℃, then insulation 2h stops vacuumizing, and passes into continuously nitrogen, making furnace pressure is 1.1 normal atmosphere, in the time of 1500 ℃, after nitrogenize 2h, stopped heating makes the product furnace cooling.Product TiCN content is that 99.2%, O content is 0.9%, and Fisher particle size is 0.93um, and the SEM pattern is spherical, and even particle size distribution is seen Fig. 1, Fig. 2.Fig. 3 and Fig. 4 are the SEM figure of German Stratco Inc. like product.With Fig. 1 and Fig. 3 contrast, Fig. 2 and Fig. 4 contrast, as can be known, the prepared product SEM pattern of the present invention is spherical, size-grade distribution is more even.
Embodiment 2:
A kind of method for preparing super fine titanium carbonitride adopts TiO
2With polyvinyl alcohol be raw material, with 100kg TiO
2With contain the 76.8kg polyvinyl alcohol and evenly mix (nano-TiO wherein
2Mass ratio 10:4 with institute's carbon containing in organic carbon source), cold pressing and make the piece material, in the vacuum oven of packing into, speed with 5 ℃/min heats up rapidly, and vacuumizes simultaneously, makes vacuum tightness less than 50pa, after temperature rose to 650 ℃, then insulation 1h when continuing to rise to 1520 ℃, then insulation 2h stops vacuumizing, and passes into continuously nitrogen, making furnace pressure is 1.1 normal atmosphere, after 1520 ℃ of nitrogenize 3h, stopped heating makes the product furnace cooling.Product TiCN content is that 99.1%, O content is 0.8%, and Fisher particle size is 0.96um.
Claims (6)
1. a method for preparing super fine titanium carbonitride, is characterized in that, concrete steps are:
(1) with nano-TiO
2Mix with the organic carbon source ball milling, wherein nano-TiO
2With the mass ratio of contained C in organic carbon source be 10:1～4.8, then cold pressing and make the piece material;
(2) described block of material packed in vacuum induction furnace, be evacuated to furnace pressure less than or equal to 50Pa, then the heat-up rate with 5 ℃/min-8 ℃/min is warming up to 300 ℃-800 ℃, insulation 0.5 h-3h; Be warming up to 1000 ℃～1900 ℃, insulation 0.5 h～3h constantly vacuumizes in insulating process again;
After (3) (2) steps finish, pass into nitrogen, making furnace pressure is 1.1-1.2 normal atmosphere, continuation is incubated 1 h～4h under 1000 ℃～1900 ℃, make the abundant nitrogenize of raw material, then be cooled to 150 ℃～350 ℃, take out the piece material, fragmentation, ball milling, classification obtain Fisher particle size less than the carbon titanium nitride powder material of 1 micron.
2. a kind of method for preparing super fine titanium carbonitride according to claim 1, is characterized in that the described nano-TiO of step (1)
2Fisher particle size less than 100 nanometers, TiO
2Content is greater than 99%.
3. a kind of described method for preparing super fine titanium carbonitride according to claim 1 and 2, is characterized in that, the described carbon source of step (1) is selected from polyvinyl alcohol, sucrose, starch, tartrate, oxalic acid or glucose.
4. a kind of described method for preparing super fine titanium carbonitride according to claim 1 and 2, is characterized in that the described nano-TiO of step (1)
2With the mass ratio of contained C in carbon source be 10:2～4.
5. a kind of described method for preparing super fine titanium carbonitride according to claim 1 and 2, it is characterized in that, in step (2), described block of material packed in vacuum induction furnace, be evacuated to furnace pressure less than or equal to 50Pa, then the heat-up rate with 5 ℃/min-8 ℃/min is warming up to 350 ℃-650 ℃, insulation 0.5 h-2h; Be warming up to again 1100 ℃～1700 ℃, insulation 0.5 h～2h.
6. a kind of described method for preparing super fine titanium carbonitride according to claim 1 and 2, is characterized in that, the described nitrogen gas purity of step (3) is greater than 99%.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387215A (en) * | 2013-07-28 | 2013-11-13 | 桂林理工大学 | Method for preparing TiCN powder by using tetrabutyl titanate and starch as Ti source and C source respectively |
| CN103387216A (en) * | 2013-07-28 | 2013-11-13 | 桂林理工大学 | Method for preparing TiCN powder by using TiOSO4 and starch as Ti source and C source respectively |
| CN103395755A (en) * | 2013-08-04 | 2013-11-20 | 桂林理工大学 | Method used for preparing TiCN powder by using tetrabutyl titanate as titanium source and phenolic resin as carbon source |
| CN103395753A (en) * | 2013-08-04 | 2013-11-20 | 桂林理工大学 | Method used for preparing TiCN powder by using tetrabutyl titanate as titanium source and pentaerythritol as carbon source |
| CN103435355A (en) * | 2013-08-28 | 2013-12-11 | 桂林理工大学 | Method for preparing TiCN powder by respectively taking butyl titanate and sucrose as titanium source and carbon source |
| CN103449387A (en) * | 2013-08-28 | 2013-12-18 | 桂林理工大学 | Method for preparing TiCN powder by using TiOSO4 as titanium source and cane sugar as carbon source |
| CN103787407A (en) * | 2013-12-25 | 2014-05-14 | 河北科技大学 | Method for preparing nano TiCN/Al2O3 composite powder through reactive ball milling |
| CN103979508A (en) * | 2014-05-04 | 2014-08-13 | 华中科技大学 | Preparation method of nano-Ti(C,N) solid solution powder |
| CN105621378A (en) * | 2015-12-27 | 2016-06-01 | 北京工业大学 | Preparation method for TiN (1-x) Cx daltonide powder |
| CN106430286A (en) * | 2016-09-18 | 2017-02-22 | 河南师范大学 | Method for preparing ZnO/g-C3N4 composite of core-shell structure |
| CN108424147A (en) * | 2018-02-12 | 2018-08-21 | 吉林长玉特陶新材料技术股份有限公司 | A kind of method that Rapid Nitriding produces titanium carbonitride, nitrogenizes titanium valve |
| CN109437917A (en) * | 2018-12-19 | 2019-03-08 | 北京科技大学 | A kind of method that two sections of reduction nitridations produce titanium nitride and titanium carbonitride |
| CN109536811A (en) * | 2018-12-26 | 2019-03-29 | 河源普益硬质合金厂有限公司 | A kind of Ti(CN) base TN18 cermet and its preparation process |
| CN110357637A (en) * | 2019-07-29 | 2019-10-22 | 株洲红日新材料科技有限公司 | Super fine titanium carbonitride powder end and preparation method thereof |
| CN110357639A (en) * | 2019-07-29 | 2019-10-22 | 株洲红芯新材料科技有限公司 | Super fine titanium carbonitride powder end and preparation method thereof |
| CN111547724A (en) * | 2020-05-20 | 2020-08-18 | 蓬莱市超硬复合材料有限公司 | Superfine titanium carbide powder and preparation method thereof |
| CN115093233A (en) * | 2022-07-12 | 2022-09-23 | 吉林长玉特陶新材料技术股份有限公司 | Preparation method of high-purity superfine transition metal carbonitride high-entropy ceramic powder suitable for industrial mass production |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387216A (en) * | 2013-07-28 | 2013-11-13 | 桂林理工大学 | Method for preparing TiCN powder by using TiOSO4 and starch as Ti source and C source respectively |
| CN103387215A (en) * | 2013-07-28 | 2013-11-13 | 桂林理工大学 | Method for preparing TiCN powder by using tetrabutyl titanate and starch as Ti source and C source respectively |
| CN103395755B (en) * | 2013-08-04 | 2015-09-23 | 桂林理工大学 | The method that titanium source and carbon source prepare TiCN powder is respectively with tetrabutyl titanate and resol |
| CN103395755A (en) * | 2013-08-04 | 2013-11-20 | 桂林理工大学 | Method used for preparing TiCN powder by using tetrabutyl titanate as titanium source and phenolic resin as carbon source |
| CN103395753A (en) * | 2013-08-04 | 2013-11-20 | 桂林理工大学 | Method used for preparing TiCN powder by using tetrabutyl titanate as titanium source and pentaerythritol as carbon source |
| CN103435355A (en) * | 2013-08-28 | 2013-12-11 | 桂林理工大学 | Method for preparing TiCN powder by respectively taking butyl titanate and sucrose as titanium source and carbon source |
| CN103449387A (en) * | 2013-08-28 | 2013-12-18 | 桂林理工大学 | Method for preparing TiCN powder by using TiOSO4 as titanium source and cane sugar as carbon source |
| CN103787407B (en) * | 2013-12-25 | 2016-04-20 | 河北科技大学 | Reaction ball milling legal system is for nano TiC N/Al 2o 3the method of composite powder |
| CN103787407A (en) * | 2013-12-25 | 2014-05-14 | 河北科技大学 | Method for preparing nano TiCN/Al2O3 composite powder through reactive ball milling |
| CN103979508B (en) * | 2014-05-04 | 2015-07-08 | 华中科技大学 | Preparation method of nano-Ti(C,N) solid solution powder |
| CN103979508A (en) * | 2014-05-04 | 2014-08-13 | 华中科技大学 | Preparation method of nano-Ti(C,N) solid solution powder |
| CN105621378A (en) * | 2015-12-27 | 2016-06-01 | 北京工业大学 | Preparation method for TiN (1-x) Cx daltonide powder |
| CN106430286A (en) * | 2016-09-18 | 2017-02-22 | 河南师范大学 | Method for preparing ZnO/g-C3N4 composite of core-shell structure |
| CN108424147A (en) * | 2018-02-12 | 2018-08-21 | 吉林长玉特陶新材料技术股份有限公司 | A kind of method that Rapid Nitriding produces titanium carbonitride, nitrogenizes titanium valve |
| CN109437917A (en) * | 2018-12-19 | 2019-03-08 | 北京科技大学 | A kind of method that two sections of reduction nitridations produce titanium nitride and titanium carbonitride |
| CN109536811A (en) * | 2018-12-26 | 2019-03-29 | 河源普益硬质合金厂有限公司 | A kind of Ti(CN) base TN18 cermet and its preparation process |
| CN110357637A (en) * | 2019-07-29 | 2019-10-22 | 株洲红日新材料科技有限公司 | Super fine titanium carbonitride powder end and preparation method thereof |
| CN110357639A (en) * | 2019-07-29 | 2019-10-22 | 株洲红芯新材料科技有限公司 | Super fine titanium carbonitride powder end and preparation method thereof |
| CN111547724A (en) * | 2020-05-20 | 2020-08-18 | 蓬莱市超硬复合材料有限公司 | Superfine titanium carbide powder and preparation method thereof |
| CN115093233A (en) * | 2022-07-12 | 2022-09-23 | 吉林长玉特陶新材料技术股份有限公司 | Preparation method of high-purity superfine transition metal carbonitride high-entropy ceramic powder suitable for industrial mass production |
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Address after: 410205 No. 38 Lugu Lutian Road, Changsha High-tech Development Zone, Hunan Province Patentee after: Changsha Wei Hui hi tech new material Co., Ltd. Address before: 410205 Hunan province Changsha City Lugu high tech Zone Lu Tin Road No. 38 Patentee before: Changsha Wing High High-tech New Materials Co.,Ltd. |