CN103979566B - A kind of vanadium diboride raw powder's production technology - Google Patents
A kind of vanadium diboride raw powder's production technology Download PDFInfo
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- CN103979566B CN103979566B CN201410219036.9A CN201410219036A CN103979566B CN 103979566 B CN103979566 B CN 103979566B CN 201410219036 A CN201410219036 A CN 201410219036A CN 103979566 B CN103979566 B CN 103979566B
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- powder
- fused salt
- obtains
- vanadate
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- 239000000843 powder Substances 0.000 title claims abstract description 67
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000005516 engineering process Methods 0.000 title claims abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 9
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 20
- 150000003839 salts Chemical class 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- 238000007669 thermal treatment Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000009837 dry grinding Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 239000011833 salt mixture Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 abstract 2
- 239000006227 byproduct Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 230000002110 toxicologic effect Effects 0.000 abstract 1
- 231100000027 toxicology Toxicity 0.000 abstract 1
- 239000012153 distilled water Substances 0.000 description 10
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 238000003828 vacuum filtration Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Landscapes
- Battery Electrode And Active Subsutance (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of vanadium diboride raw powder's production technology, belong to ceramic powder preparing technical field.This preparation method is that after the ammonium meta-vanadate of 3:11 and pure boron powder and a certain amount of fused salt mix, under protection of inert gas, at 800 ~ 1100 DEG C, thermal treatment 0.5 ~ 4h obtains vanadium diboride powder by mol ratio.The by product boron trioxide that reaction produces and fused salt are removed by infiltrating the method for dissolving with hot water.The vanadium source toxicological harmless that the inventive method adopts, production technique is simple, is applicable to batch production.The melting salt environment that the inventive method is introduced accelerates the velocity of diffusion of solid matter, and make synthesis temperature low, synthesis cycle is short, and synthesized powder has the features such as purity is high, particle diameter is little.
Description
Technical field
The invention belongs to ceramic powder preparing technical field, be specifically related to a kind of vanadium diboride (VB
2) raw powder's production technology, it can be used for preparing superhigh temperature ceramics, high-abrasive material and alkaline cell electrode materials.
Background technology
VB
2have that fusing point is high, hardness is large, electrical and thermal conductivity performance is good, can resist the features such as molten metal attack, can be used for making ultrahigh-temperature structured material, at the extreme environment such as ultrahigh-temperature, Metal smelting, there is important application.In addition, VB
2having larger loading capacity as alkaline cell electrode materials, is a kind of novel energy and material.
Current VB
2raw powder's production technology mainly contains following several, and comprise (1) and adopt metal simple-substance V and simple substance B direct heating or mechanical alloy method to synthesize, this method technique is simple, and temperature is low, but expensive starting materials, synthetic powder particle size is large and homogeneity is poor; (2) reductive agent reduction V is adopted
2o
5, the diameter of particle prepared by this method is even, but synthesis temperature higher (> 1300 DEG C), and the raw material V used
2o
5for highly toxic substance; (3) VCl is adopted
4, NaBH
4be raw material with Mg, in a kettle. by solid state reaction kinetics VB
2, this method synthesis temperature low (650 DEG C), gained powder granule size can reach nano level, but expensive starting materials, production technique needs specific installation, is not suitable for producing in enormous quantities.As can be seen here, a kind of advantages of nontoxic raw materials is studied and price is relatively inexpensive, production technique is simple, synthesis temperature is lower, synthetic powder particle size is little and the VB be evenly distributed
2raw powder's production technology has very important significance.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provide a kind of technique simple, with low cost, VB can be prepared in batches
2the method of powder.
In order to solve above technical problem, the present invention is achieved by the following technical programs, comprises the following steps:
(1) first by ammonium meta-vanadate (NH
4vO
3), pure boron (B) powder and fused salt carry out proportioning in proportion, and put into ball mill for dry grinding mixing; Described fused salt is NaCl, KCl, LiCl, MgCl
2in one or more mixing; NH
4vO
3be 3:11 with the plain mol ratio of simple substance B powder; The quality of fused salt is NH
4vO
3with 5 ~ 20 times of simple substance B powder total mass;
(2) mixed powder that step (1) obtains is put into alumina crucible, under protection of inert gas, naturally cooling after thermal treatment for some time, obtains VB
2, B
2o
3and molten salt mixture; Described thermal treatment temp is 800 ~ 1100 DEG C, and the treatment time is 0.5 ~ 4h;
(3) mixture that step (2) obtains is put into the deionized water of 60 ~ 90 DEG C and stirred, as the B that reaction generates
2o
3and after fused salt dissolving, be precipitated by filtering separation, precipitate and can obtain VB after the techniques such as washing, alcohol wash, drying
2powder.
As one optimization, the fused salt in described step (1) be NaCl and KCl in molar ratio 1:1 carry out the mixture that proportioning obtains, the quality of this fused salt is 10 times of ammonium meta-vanadate and pure boron powder total mass; Described step (2) thermal treatment temp is 900 DEG C, and heat treatment time is 1h; Deionized water temperature in described step (3) is 60 DEG C.
Compared with prior art, the present invention has following technique effect.
(1) present invention process is simple, without the need to the moulding process needed for conventional solid-state method, without the need to specific installation, is applicable to batch production.
(2) the present invention adopts NH
4vO
3as vanadium source, nontoxic, cheap, cost is lower.
(3) the present invention introduces melting salt in building-up process, accelerates material velocity of diffusion, NH
4vO
3decomposes release gas and generate B
2o
3volatilization can also stir molten salt system, accelerate further diffusion.The inventive method synthesis temperature is low, and synthesis cycle is short, significantly reduces production energy consumption.In addition, the adding generated VB of fused salt
2particle has certain iris action, and grain growth receives suppression, prepared VB
2diameter of particle is little, and median size is lower than 0.5 μm.
Accompanying drawing explanation
Fig. 1 is the VB that embodiment 1 obtains
2x-ray diffraction (XRD) collection of illustrative plates.
Fig. 2 is the VB that embodiment 1 obtains
2scanning electronic microscope (SEM) photo.
Embodiment
In order to understand technology contents of the present invention further, below in conjunction with drawings and Examples in detail the present invention is described in detail, but the present invention is not limited to following embodiment.
Embodiment 1
By NH
4vO
3the ratio being 3:11 in molar ratio with simple substance B powder is carried out proportioning and is obtained powder 1; NaCl and KCl is obtained powder 2 for the ratio of 1:1 carries out proportioning in molar ratio; The ratio of powder 1 and powder 2 1:10 is in mass ratio obtained powder 3 after ball mill for dry grinding mixes 1h; Powder 3 is placed in alumina crucible, under flowing Ar gas shielded, is heated to 900 DEG C and is incubated 1h, after naturally cooling to room temperature, obtaining powder 4; Powder 4 to be immersed in 60 DEG C of distilled water and Keep agitation 0.5h, be separated through vacuum filtration and be precipitated thing; By throw out with after 60 DEG C of distilled water washs twice with washing with alcohol once, obtain VB after drying
2powder.
The nanometer VB of Fig. 1 prepared by the present embodiment
2the XRD figure spectrum of powder, this collection of illustrative plates shows, prepared VB
2powder is pure phase, does not have other impurity phase.
VB prepared by Fig. 2 the present embodiment
2the SEM collection of illustrative plates of powder, collection of illustrative plates shows, prepared VB
2the particle size uniformity of powder, median size is lower than 0.5 μm.
Embodiment 2
By NH
4vO
3the ratio being 3:11 in molar ratio with simple substance B powder is carried out proportioning and is obtained powder 1; The ratio of powder 1 and NaCl 1:10 is in mass ratio obtained powder 2 after ball mill for dry grinding mixes 1h; Powder 2 is placed in alumina crucible, under flowing Ar gas shielded, is heated to 800 DEG C and is incubated 4h, after naturally cooling to room temperature, obtaining powder 3; Powder 3 to be immersed in 70 DEG C of distilled water and Keep agitation 0.5h, be separated through vacuum filtration and be precipitated thing; By throw out with after 80 DEG C of distilled water washs twice with washing with alcohol once, obtain VB after drying
2powder.
Embodiment 3
By NH
4vO
3the ratio being 3:11 in molar ratio with simple substance B powder is carried out proportioning and is obtained powder 1; The ratio of powder 1 and KCl 1:5 is in mass ratio obtained powder 2 after ball mill for dry grinding mixes 1h; Powder 2 is placed in alumina crucible, under flowing Ar gas shielded, is heated to 1100 DEG C and is incubated 0.5h, after naturally cooling to room temperature, obtaining powder 3; Powder 3 to be immersed in 80 DEG C of distilled water and Keep agitation 1.5h, be separated through vacuum filtration and be precipitated thing; By throw out with after 80 DEG C of distilled water washs twice with washing with alcohol once, obtain VB after drying
2powder.
Embodiment 4
By NH
4vO
3the ratio being 3:11 in molar ratio with simple substance B powder is carried out proportioning and is obtained powder 1; By powder 1 and MgCl
2the ratio of 1:15 obtains powder 2 after ball mill for dry grinding mixing 1h in mass ratio; Powder 2 is placed in alumina crucible, under flowing Ar gas shielded, is heated to 1050 DEG C and is incubated 1h, after naturally cooling to room temperature, obtaining powder 3; Powder 3 to be immersed in 80 DEG C of distilled water and Keep agitation 0.5h, be separated through vacuum filtration and be precipitated thing; By throw out with after 80 DEG C of distilled water washs twice with washing with alcohol once, obtain VB after drying
2powder.
Embodiment 5
By NH
4vO
3the ratio being 3:11 in molar ratio with simple substance B powder is carried out proportioning and is obtained powder 1; The ratio of powder 1 and LiCl 1:20 is in mass ratio obtained powder 2 after ball mill for dry grinding mixes 1h; Powder 2 is placed in alumina crucible, under flowing Ar gas shielded, is heated to 950 DEG C and is incubated 1h, after naturally cooling to room temperature, obtaining powder 3; Powder 3 to be immersed in 90 DEG C of distilled water and Keep agitation 0.5h, be separated through vacuum filtration and be precipitated thing; By throw out with after 90 DEG C of distilled water washs twice with washing with alcohol once, obtain VB after drying
2powder.
Claims (2)
1. a vanadium diboride raw powder's production technology, is characterized in that, the method comprises the following steps:
(1) first ammonium meta-vanadate, pure boron powder and fused salt are carried out proportioning by a certain percentage, and put into ball mill for dry grinding mixing; Described fused salt is NaCl, KCl, LiCl, MgCl
2in one or more mixing; The mol ratio of described ammonium meta-vanadate and pure boron powder is 3:11; The quality of described fused salt is 5 ~ 20 times of ammonium meta-vanadate and pure boron powder total mass;
(2) mixed powder that step (1) obtains is put into alumina crucible, under protection of inert gas, naturally cooling after thermal treatment, obtains VB
2, B
2o
3and molten salt mixture; Described thermal treatment temp is 800 ~ 1100 DEG C, and the treatment time is 0.5 ~ 4h;
(3) mixture that step (2) obtains is put into the deionized water of 60 ~ 90 DEG C and stirred, as the B that reaction generates
2o
3and after fused salt dissolving, be precipitated thing by filtering separation, this throw out can be obtained VB after washing, alcohol wash, drying
2powder.
2. vanadium diboride raw powder's production technology as claimed in claim 1, it is characterized in that, fused salt in described step (1) be NaCl and KCl in molar ratio 1:1 carry out the mixture that proportioning obtains, the quality of this fused salt is 10 times of ammonium meta-vanadate and pure boron powder total mass; Described step (2) thermal treatment temp is 900 DEG C, and heat treatment time is 1h; Deionized water temperature in described step (3) is 60 DEG C.
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|---|---|---|---|
| CN201410219036.9A CN103979566B (en) | 2014-05-22 | 2014-05-22 | A kind of vanadium diboride raw powder's production technology |
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| CN103979566B true CN103979566B (en) | 2015-12-09 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2638396C2 (en) * | 2016-05-16 | 2017-12-13 | Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Новосибирский Государственный Технический Университет" | Method of producing vanadium diboride |
| CN108584972A (en) * | 2018-04-20 | 2018-09-28 | 华南理工大学 | A kind of TiB2Raw powder's production technology |
| CN115403051A (en) * | 2022-09-16 | 2022-11-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of vanadium diboride |
| CN116239386A (en) * | 2023-02-03 | 2023-06-09 | 山西大同大学 | Preparation method of high-purity vanadium boride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5551797A (en) * | 1978-10-05 | 1980-04-15 | Agency Of Ind Science & Technol | Production of vanadium diboride and tantalum diboride single crystal from aluminum bath |
| JPH0778727A (en) * | 1993-09-09 | 1995-03-20 | Toshiba Corp | Thin film capacitor |
| US8404199B2 (en) * | 2010-08-06 | 2013-03-26 | Empire Technology Development Llc | Fluorine based vanadium boride nanoparticle synthesis |
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