CN105502398A - Method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction - Google Patents
Method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction Download PDFInfo
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- CN105502398A CN105502398A CN201610114041.2A CN201610114041A CN105502398A CN 105502398 A CN105502398 A CN 105502398A CN 201610114041 A CN201610114041 A CN 201610114041A CN 105502398 A CN105502398 A CN 105502398A
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention discloses a method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction. The method includes: using tantalum oxide and carbon black as raw materials, NaCl, KCl and KF as molten salts and magnesium powder as a reductant; weighing the raw materials proportionally; mixing the raw materials well, and filling a graphite crucible with a mixture of the raw materials; performing low-temperature carbothermic reduction in a flowing argon atmosphere to prepare the tantalum carbide superfine powder. The method is simple in process, easy in preparation condition control and low in cost. The tantalum carbide superfine powder prepared by the method can be applied to producing modifiers of ultrahigh-temperature tantalum carbide ceramic and hard alloys.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, be specifically related to the method for a kind of fused salt assisting magnesium thermal reduction synthesis tantalum carbide superfine powder.
Background technology
The high-temperature structural material that tantalum carbide (TaC) is a kind of important high strength, corrosion-resistant and chemical stability is good, its fusing point is up to 3880 DEG C, there is the characteristics such as excellent mechanical behavior under high temperature, the performance of flushing of anti-high velocity air (particle flux), anti-yaw damper performance, hardness are large simultaneously, can be used as high temperature material and Wimet additive.At present, the domestic relevant report preparing tantalum carbide powder mainly with tantalum oxide, tantalum powder be tantalum source, with carbon black etc. for carbon source, prepare tantalum carbide through high temperature cabonization, its synthesis temperature is higher, also needs to grind product to obtain tantalum carbide powder again.
Fused salt assists synthesis method to utilize reactant to have certain solubleness in fused solution salt, reactant can be made to realize the mixing of atomic scale in the liquid phase, and reactant has velocity of diffusion faster in liquid phase medium, because this reducing synthesis temperature; Achieve each component proportion of synthetic product accurate simultaneously, uniform composition, segregation-free, simultaneously in reaction process, melting salt prevents being interconnected between particle, and make the dispersiveness of the powder of synthesis fine, the product after dissolving washing does not almost have agglomeration, the diameter of particle of preparation is less, is conducive to preparing nano-powder and superfine powder.
Still not retrieving with fused salt is at present medium, with tantalum oxide and carbon black be raw material, with Mg powder for reducing agent low temperature prepares the document of tantalum carbide superfine powder aspect and open patent of invention.
Summary of the invention
Object of the present invention just in order to provide a kind of have technical process short, easy to operate, be easy to realize, the method for the fused salt assisting magnesium thermal reduction of save energy synthesis tantalum carbide superfine powder.
The method of fused salt assisting magnesium thermal reduction synthesis tantalum carbide superfine powder of the present invention is with Ta
2o
5be raw material with carbon black, with Mg powder for reductive agent synthesizes tantalum carbide powder, reaction equation is:
Ta
2O
5+5Mg+2C=2TaC+5MgO(1)
MgO+2HCl=MgCl
2+H
2O(2)
The step of the inventive method is as follows:
(1) by Ta
2o
5powder: Mg powder: the mol ratio of carbon black is that 1:5 ~ 6:2 carries out proportioning, mixes and obtains compound 1; Wherein said Mg powder is reductive agent;
(2) fused salt NaCl, KCl, KF are weighed according to mol ratio 1:1:0.1, mix and obtain salt compound 2;
(3) compound 1 and salt compound 2 are weighed according to mass ratio 1:3 ~ 5, mix and obtain powder mix 3;
(4) powder mix 3 is placed in plumbago crucible to add a cover; again crucible is put into tube furnace; then the argon gas of flowing is passed into as protective atmosphere; be that 3 ~ 15 DEG C/min is warmed up to 1150 ~ 1260 DEG C by temperature rise rate; be incubated 2 ~ 6 hours; take out after being cooled to room temperature; be placed in containing 1 ~ 2mol/L hydrochloric acid soln magnetic agitation, 4 ~ 8h; the MgO impurity that solubilizing reaction generates; then washed with de-ionized water is used to remove fused salt; go out powder through centrifugation, dry i.e. obtained TaC superfine powder, its particle diameter is less than 3 microns.
Ta described in the present invention
2o
5granularity is less than 0.5 μm, Ta
2o
5purity is greater than 99.5%(weight percent); Carbon black purity is greater than 98.5%(weight percent); Magnesium Powder Particle Size is less than 0.074mm, and magnesium powder purity is greater than 98.5%(weight percent).
Beneficial effect of the present invention is as follows:
1, preparation technology is simple, without the need to processing unit and the technological process of complexity.
2, the present invention utilizes the advantage of molten-salt growth method, adopts magnesiothermic reduction tantalum oxide, not only reduces synthesis temperature, can control the size of tantalum carbide powder simultaneously.
3, preparation temperature is low, powder granularity is little, purity is higher, and in prepared powder, the mass percent of TaC phase is greater than 95%.
4, the tantalum carbide superfine powder that prepared by the present invention can be used for the properties-correcting agent preparing TaC system superhigh temperature ceramics and Wimet.
Embodiment
The present invention is further described below with reference to embodiment:
embodiment 1
By Ta
2o
5powder: Mg powder: the mol ratio of carbon black is that 1:6:2 carries out proportioning and mixes and obtain compound 1; Fused salt NaC, KCl, KF are weighed to mix according to mol ratio 1:1:0.1 and obtains salt compound 2; Mix after compound 1 and salt compound 2 are weighed according to mass ratio 1:3, obtain powder mix 3; Powder mix 3 is placed in plumbago crucible add a cover, then crucible is put into tube furnace, be that 3 DEG C/min is warmed up to 1150 DEG C by temperature rise rate under flowing argon gas atmosphere, be incubated 6 hours, take out after being cooled to room temperature; Product is placed in containing 2mol/L hydrochloric acid soln magnetic agitation 4h, then fused salt is removed by washed with de-ionized water, separated from solution by tantalum carbide powder with whizzer (8000 turns/min), dry 8h i.e. obtained TaC superfine powder at 110 DEG C, its particle diameter is less than 3 μm.
embodiment 2
By Ta
2o
5powder: Mg powder: the mol ratio of carbon black is that 1:5.5:2 carries out proportioning and mixes and obtain compound 1; Fused salt NaCl, KCl, KF are weighed to mix according to mol ratio 1:1:0.1 and obtains salt compound 2; Mix after compound 1 and salt compound 2 are weighed according to mass ratio 1:5, obtain powder mix 3; Powder mix 3 is placed in plumbago crucible add a cover, then crucible is put into tube furnace, flowing argon gas atmosphere under by temperature rise rate be 10 DEG C/min be warmed up to 1200 DEG C insulation 4 hours, take out after being cooled to room temperature; Product is placed in containing 1.5mol/L hydrochloric acid soln magnetic agitation 4h, then fused salt is removed by washed with de-ionized water, separated from solution by tantalum carbide powder with whizzer (11000 turns/min), dry 8h i.e. obtained TaC superfine powder at 110 DEG C, its particle diameter is less than 3 μm.
embodiment 3
By Ta
2o
5powder: Mg powder: the mol ratio of carbon black is that 1:5.25:2 carries out proportioning and mixes and obtain compound 1; Fused salt NaCl, KCl, KF are weighed to mix according to mol ratio 1:1:0.1 and obtains salt compound 2; Mix after compound 1 and salt compound 2 are weighed according to mass ratio 1:5, obtain powder mix 3; Powder mix 3 is placed in plumbago crucible add a cover, then crucible is put into tube furnace, be that 15 DEG C/min is warmed up to 1230 DEG C by temperature rise rate under flowing argon gas atmosphere, be incubated 3 hours, take out after being cooled to room temperature; Product is placed in containing 1mol/L hydrochloric acid soln magnetic agitation 8h, then fused salt is removed by washed with de-ionized water, separated from solution by tantalum carbide powder with whizzer (9000 turns/min), dry 8h i.e. obtained TaC superfine powder at 110 DEG C, its particle diameter is less than 3 μm.
embodiment 4
By Ta
2o
5powder: Mg powder: the mol ratio of carbon black is that 1:5.3:2 carries out proportioning and mixes and obtain compound 1; Fused salt NaCl, KCl, KF are weighed to mix according to mol ratio 1:1:0.1 and obtains salt compound 2; Mix after compound 1 and salt compound 2 are weighed according to mass ratio 1:5, obtain powder mix 3; Powder mix 3 is placed in plumbago crucible add a cover, then crucible is put into tube furnace, be that 5 DEG C/min is warmed up to 1260 DEG C by temperature rise rate under flowing argon gas atmosphere, be incubated 2 hours, take out after being cooled to room temperature; Product is placed in containing 2mol/L hydrochloric acid soln magnetic agitation 4h, then fused salt is removed by washed with de-ionized water, separated from solution by tantalum carbide powder with whizzer (11000 turns/min), at 110 DEG C, dry 8h obtains TaC superfine powder, and its particle diameter is less than 3 μm.
Claims (2)
1. a method for fused salt assisting magnesium thermal reduction synthesis tantalum carbide superfine powder, is characterized in that: described method steps is as follows:
(1) by Ta
2o
5powder: Mg powder: the mol ratio of carbon black is that 1:5 ~ 6:2 carries out proportioning, mixes and obtains compound 1; Wherein said Mg powder is reductive agent;
(2) fused salt NaCl, KCl, KF are weighed according to mol ratio 1:1:0.1, mix and obtain salt compound 2;
(3) compound 1 and salt compound 2 are weighed according to mass ratio 1:3 ~ 5, mix and obtain powder mix 3;
(4) powder mix 3 is placed in plumbago crucible to add a cover; again crucible is put into tube furnace; then the argon gas of flowing is passed into as protective atmosphere; be that 3 ~ 15 DEG C/min is warmed up to 1150 ~ 1260 DEG C by temperature rise rate; be incubated 2 ~ 6 hours; take out after being cooled to room temperature; be placed in containing 1 ~ 2mol/L hydrochloric acid soln magnetic agitation, 4 ~ 8h; the MgO impurity that solubilizing reaction generates; then washed with de-ionized water is used to remove fused salt; go out powder through centrifugation, dry i.e. obtained TaC superfine powder, its particle diameter is less than 3 microns.
2. the method for the fused salt assisting magnesium thermal reduction synthesis tantalum carbide superfine powder according to claims 1, is characterized in that: described Ta
2o
5granularity is less than 0.5 μm, Ta
2o
5purity is greater than 99.5%; Carbon black purity is greater than 98.5%; Magnesium Powder Particle Size is less than 0.074mm, and magnesium powder purity is greater than 98.5%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2639797C1 (en) * | 2016-08-11 | 2017-12-22 | Федеральное государственное бюджетное учреждение науки Институт металлургии Уральского отделения Российской академии наук (ИМЕТ УрО РАН) | Method of producing carbide powder |
| CN109019625A (en) * | 2018-09-30 | 2018-12-18 | 成都先进金属材料产业技术研究院有限公司 | The preparation method of powders of titanium boride |
| CN109574014A (en) * | 2018-10-22 | 2019-04-05 | 西安建筑科技大学 | A kind of B4Fiber C felt and preparation method thereof |
| CN111874907A (en) * | 2020-08-18 | 2020-11-03 | 四川轻化工大学 | Preparation method of spherical nanometer VC powder |
| CN111926183A (en) * | 2020-08-12 | 2020-11-13 | 昆明理工大学 | Method for preparing low-oxygen metal by using rare earth to assist magnesiothermic reduction of metal oxide |
| CN112267017A (en) * | 2020-09-18 | 2021-01-26 | 昆明理工大学 | Method for preparing metal alloy powder by magnesiothermic reduction |
| CN114853018A (en) * | 2022-04-13 | 2022-08-05 | 广东先导稀材股份有限公司 | Method for preparing tantalum carbide powder |
| CN114959905A (en) * | 2022-03-07 | 2022-08-30 | 西北工业大学 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
| CN116332678A (en) * | 2023-05-30 | 2023-06-27 | 中南大学 | Method for preparing tantalum carbide coating on surface of carbon material |
| CN116444296A (en) * | 2023-05-04 | 2023-07-18 | 中南大学 | Method for preparing tantalum carbide coating on graphite substrate by molten salt method |
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| CN102225764A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of tantalum carbide powder |
| CN102491328A (en) * | 2011-12-08 | 2012-06-13 | 武汉科技大学 | Titanium carbide powder and preparation method thereof |
| CN103253670A (en) * | 2013-05-17 | 2013-08-21 | 航天材料及工艺研究所 | Method for preparing TaC powder at low temperature by carbothermic method |
| CN103265031A (en) * | 2013-05-17 | 2013-08-28 | 航天材料及工艺研究所 | Method for low-temperature preparation of ZrC-WC or ZrC-TaC mixed powder through carbothermic method |
-
2016
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Patent Citations (4)
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|---|---|---|---|---|
| CN102225764A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of tantalum carbide powder |
| CN102491328A (en) * | 2011-12-08 | 2012-06-13 | 武汉科技大学 | Titanium carbide powder and preparation method thereof |
| CN103253670A (en) * | 2013-05-17 | 2013-08-21 | 航天材料及工艺研究所 | Method for preparing TaC powder at low temperature by carbothermic method |
| CN103265031A (en) * | 2013-05-17 | 2013-08-28 | 航天材料及工艺研究所 | Method for low-temperature preparation of ZrC-WC or ZrC-TaC mixed powder through carbothermic method |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2639797C1 (en) * | 2016-08-11 | 2017-12-22 | Федеральное государственное бюджетное учреждение науки Институт металлургии Уральского отделения Российской академии наук (ИМЕТ УрО РАН) | Method of producing carbide powder |
| CN109019625B (en) * | 2018-09-30 | 2021-07-20 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing titanium boride powder |
| CN109019625A (en) * | 2018-09-30 | 2018-12-18 | 成都先进金属材料产业技术研究院有限公司 | The preparation method of powders of titanium boride |
| CN109574014A (en) * | 2018-10-22 | 2019-04-05 | 西安建筑科技大学 | A kind of B4Fiber C felt and preparation method thereof |
| CN109574014B (en) * | 2018-10-22 | 2022-04-19 | 西安建筑科技大学 | B4C fiber felt and preparation method thereof |
| CN111926183A (en) * | 2020-08-12 | 2020-11-13 | 昆明理工大学 | Method for preparing low-oxygen metal by using rare earth to assist magnesiothermic reduction of metal oxide |
| CN111874907A (en) * | 2020-08-18 | 2020-11-03 | 四川轻化工大学 | Preparation method of spherical nanometer VC powder |
| CN112267017A (en) * | 2020-09-18 | 2021-01-26 | 昆明理工大学 | Method for preparing metal alloy powder by magnesiothermic reduction |
| CN114959905A (en) * | 2022-03-07 | 2022-08-30 | 西北工业大学 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
| CN114853018A (en) * | 2022-04-13 | 2022-08-05 | 广东先导稀材股份有限公司 | Method for preparing tantalum carbide powder |
| CN114853018B (en) * | 2022-04-13 | 2024-03-26 | 广东先导稀材股份有限公司 | Preparation method of tantalum carbide powder |
| CN116444296A (en) * | 2023-05-04 | 2023-07-18 | 中南大学 | Method for preparing tantalum carbide coating on graphite substrate by molten salt method |
| CN116444296B (en) * | 2023-05-04 | 2024-02-02 | 中南大学 | Method for preparing tantalum carbide coating on graphite substrate by molten salt method |
| CN116332678A (en) * | 2023-05-30 | 2023-06-27 | 中南大学 | Method for preparing tantalum carbide coating on surface of carbon material |
| CN116332678B (en) * | 2023-05-30 | 2023-08-11 | 中南大学 | Method for preparing tantalum carbide coating on surface of carbon material |
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Application publication date: 20160420 |