CN101082089A - Preparation method of nitriding vanadium alloy - Google Patents
Preparation method of nitriding vanadium alloy Download PDFInfo
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- CN101082089A CN101082089A CN 200710049495 CN200710049495A CN101082089A CN 101082089 A CN101082089 A CN 101082089A CN 200710049495 CN200710049495 CN 200710049495 CN 200710049495 A CN200710049495 A CN 200710049495A CN 101082089 A CN101082089 A CN 101082089A
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Abstract
The present invention provides process of preparing vanadium nitride alloy. The process includes mixing vanadium oxide, carbon powder and density reinforcer, pressing to form, setting the shaped mixture into a reaction furnace, heating to 650 deg.c while introducing nitrogen or ammonia as the reacting and protecting gas into the furnace, further heating to 1000-1250 deg.c to produce carbonizing and nitriding reaction for 3 hr, cooling to 100 deg.c, and discharging the vanadium nitride alloy. The vanadium nitride alloy contains V 73-80 %, N 12-20 %, C 3-8 % and O 0.5-2.0 %, and has apparent density of 3000-4000 kg/cu m. The process has the features of low reaction temperature, short reaction period, low cost, etc, and the prepared vanadium nitride alloy with high nitrogen content is suitable for use in steel making.
Description
Technical field
The invention belongs to the vanadium alloy technical field, particularly relate to a kind of preparation method of alloy of vanadium nitride.
Background technology
Vanadium nitride is a kind of important vanadium alloy additive.Existing studies show that: add vanadium nitride in the steel and can improve wear resistance, rotproofness, toughness, ductility and the comprehensive mechanical performances such as hardness and thermal fatigue resistance of steel, and make steel have good weldability, and play effects such as eliminating the inclusion extension.The increase of nitrogen content has reduced grow up trend with alligatoring of precipitated phase in the vanadium steel, and the precipitated phase particle attenuates, more give full play to the effect of vanadium.Compare with using vanadium iron, the alloy of vanadium nitride additive can be saved 20%～40% vanadium in high-strength low-alloy steel, thereby reduces production costs.
To the development of vanadium nitride, company and scientific research institutions have carried out a large amount of research both at home and abroad:
The method that U.S. combinating carbide company prepares vanadium nitride has following three kinds:
(1) with V
2O
3, iron powder and the carbon dust back compound stalk forming that is mixed, in vacuum oven, obtain vanadium carbide behind the insulation 60h down in 1385 ℃, nitriding 2 hours and 6 hours respectively when cooling the temperature to 1100 ℃ and 1000 ℃ again makes and contains V78.7%, N7.3%, the vanadium nitride of C10.5%.
(2) use V
2O
5With carbon mixture in vacuum oven internal heating to 1100～1500 ℃, vacuumize and feed the nitrogen nitriding, repeat such process for several times, obtain carbon containing, oxygen at last and all be lower than 2% vanadium nitride.
(3) with high price barium oxide V
2O
5Or NH
4VO
3Deng being raw material, with mixed gas (N
2+ NH
3Or N
2+ H
2) be reductive agent and nitridizing agent, earlier at 675～700 ℃ of following prereduction 1h, low-melting high price barium oxide is reduced into dystectic low price barium oxide, under 950 ℃, reduce simultaneously afterwards and nitriding 3～4h, can obtain to contain the oxygen massfraction and be 3%～20% nitrogen vanadyl product, it is mixed with carbonaceous material, 1400 ℃ of pyroprocessing obtain basic composition is of vanadium nitride: 80%V-7%C-12%oN-2%O at last under inertia or nitrogen atmosphere or in the vacuum oven again.
Wang Gong in 1988 is thick to wait the people in " laboratory study of vanadium carbide, carbon vanadium nitride manufacturing condition ", and " steel vanadium titanium ", 1988, P.19 No.2 in the document, has proposed the preparation method of vanadium nitride, promptly uses V
2O
5With the gac compound stalk forming, under experiment condition, carry out carbothermic reduction, reduction generates VC earlier under 1673K and 1.333Pa vacuum, feeds nitrogen subsequently, at P
N2Nitriding is 1.5 hours under the=101325Pa, can obtain (the sample of 86%V-7%C-9.069～9.577%N-2%O).In order to improve the intensity of vanadium nitride, in raw material, add 3% iron powder.
The main drawback that above-mentioned several method exists is: 1, need vacuum system, facility investment height, complicated operation; 2, intermittent type one stove one stove ground produces, and the production cycle is long, and efficiency is low; 3, temperature of reaction height, long reaction time, production cost height.
Calendar year 2001, the preparation method of the vanadium nitride that proposes in patent CN1194888C of Panzhihua Iron was; with pulverous barium oxide; carbonaceous pulvis and binding agent mix the back briquetting; moulding; again the material after the moulding is added continuously in the preparation stove; feed nitrogen or reaction of ammonia do and shielding gas to the preparation stove simultaneously; the preparation stove need be heated to 1000 ℃～1800 ℃; material is at this temperature province generation carbonization and nitrogenizing reaction; time length is less than 6h; to under protective atmosphere, be cooled to 100～250 ℃ before coming out of the stove; promptly obtain the vanadium nitride product after coming out of the stove; this product is bulk or particulate state, and its apparent density is greater than 3000kg/m
3
Aforementioned production method has lot of advantages, if can produce in enormous quantities, and production efficiency is high.But part also comes with some shortcomings: raw materials used scope is narrower, only is suitable for V
2O
3Or V
2O
3With VO
2, VO mixture, cost of material is higher; Real reaction temperature higher (～1500 ℃) has increased energy consumption, has reduced the work-ing life of sintering oven, and production cost is higher.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of alloy of vanadium nitride; vanadium resource is a raw material to this method to originate widely; after compacting, moulding; directly send in the Reaktionsofen; before 650 ℃ of insulations, feed nitrogen or ammonia as reaction and shielding gas; before 1250 ℃ of denitrification temperature, carry out carbonization and nitrogenizing reaction,, can in material, add a spot of density reinforcer in order to promote liquid phase sintering, to improve density.These method raw material sources are extensive, and temperature of reaction is low, and the reaction times is short, and carbonization, nitrogenizing reaction carry out simultaneously, and technology is simple, can be continuously produced, and production cost reduces significantly.
The objective of the invention is to be achieved through the following technical solutions:
With oxide compound, carbonaceous pulvis and the density reinforcer of vanadium mix, compression moulding is placed in the Reaktionsofen; in 650 ℃ of insulation forward reaction stoves, feed nitrogen or ammonia as reaction and shielding gas; Reaktionsofen is heated to 1000～1250 ℃; material is at this temperature range generation carbonization and nitrogenizing reaction; reaction times is less than 3h; be cooled to subsequently come out of the stove below 100 ℃, finally obtain alloy of vanadium nitride.
Further be that the oxide compound of described vanadium is V
2O
5, VO
2, V
2O
3Or VO a kind of or their mixture.
Further be that described carbonaceous pulvis is carbon black, gac, graphite or wood charcoal powder.
Further be that described density reinforcer is Fe, Co, Ni, Cr simple substance or its compound.
Further be that described Reaktionsofen is carbon tube furnace, tube furnace, induction furnace, microwave agglomerating furnace, rotary kiln, shaft furnace, grate, pushed bat kiln or tunnel furnace.
Further be that described carbonization and nitrogenizing reaction are in 1000～1250 ℃ of temperature ranges.
Utilize the alloy of vanadium nitride of technical scheme preparation of the present invention to contain 73～80%V, 12～20%N, 3～8%C, 0.5～2.0%O, its apparent density reaches 3000～4000kg/m
3
Compared with the prior art, the present invention has following tangible advantage:
(1) raw materials used is V
2O
5, VO
2, V
2O
3, VO, VC or VN a kind of or their mixture, raw material sources are extensive, cheap; Do not need binding agents such as polyvinyl alcohol, saved cost, simplified operating procedure.
(2) temperature of reaction is low, and the reaction times is short, and energy consumption is low.
(3) technology is simple.The present invention can once finish carbonization, nitrogenizing reaction, and the production efficiency height can be continuously produced, and is fit to industrialized mass.
(4) Zhi Bei alloy of vanadium nitride nitrogen content height reaches 12～20%, is more suitable in the Iron And Steel Industry steel-making requirements.
Embodiment
Now specify technical solution of the present invention in conjunction with the embodiments:
Embodiment 1:
After 48g carbon black, 152g Vanadium Pentoxide in FLAKES and 2g iron powder mixed, be pressed, pressure is 57MPa, and pressed compact is of a size of Φ 1.5cm * 1.0cm.Pressed compact is put into Reaktionsofen to be heated, before 650 ℃ of insulation 0.5h, feed high pure nitrogen, nitrogen pressure is 101325Pa, and at 1100 ℃ of insulation 1h, carbonization and nitrogenizing reaction take place, be cooled to subsequently come out of the stove below 100 ℃, finally obtain the alloy of vanadium nitride of 76.58%V-5.41%C-16.20%N-1.46%O, its apparent density is 3310kg/m
3
Embodiment 2:
After 48g carbon black, 152g Vanadium Pentoxide in FLAKES and 6g ferric oxide powder mixed, be pressed, pressure is 57MPa, and pressed compact is of a size of Φ 1.5cm * 1.0cm.Pressed compact is put into Reaktionsofen to be heated, before 650 ℃ of insulation 0.5h, feed high pure nitrogen, nitrogen pressure is 101325Pa, and at 1100 ℃ of insulation 1h, carbonization and nitrogenizing reaction take place, be cooled to subsequently come out of the stove below 100 ℃, finally obtain the alloy of vanadium nitride of 74.06%V-4.55%C-19.20%N-1.71%O, its apparent density is 3450kg/m
3
Embodiment 3:
After 50g carbon black, 150g Vanadium Pentoxide in FLAKES and 2g iron powder mixed, be pressed, pressure is 57MPa, and pressed compact is of a size of Φ 1.5cm * 1.0cm.Pressed compact is put into Reaktionsofen to be heated, before 650 ℃ of insulation 0.5h, feed high pure nitrogen, nitrogen pressure is 101325Pa, and at 1100 ℃ of insulation 1h, carbonization and nitrogenizing reaction take place, be cooled to subsequently come out of the stove below 100 ℃, finally obtain the alloy of vanadium nitride of 76.98%V-6.48%C-15.10%N-1.41%O, its apparent density is 3300kg/m
3
Embodiment 4:
After 50g carbon black, 150g Vanadium Pentoxide in FLAKES and 6g ferric oxide powder mixed, be pressed, pressure is 57MPa, and pressed compact is of a size of Φ 1.5cm * 1.0cm.Pressed compact is put into Reaktionsofen to be heated, before 650 ℃ of insulation 0.5h, feed high pure nitrogen, nitrogen pressure is 101325Pa, and at 1100 ℃ of insulation 1h, carbonization and nitrogenizing reaction take place, be cooled to subsequently come out of the stove below 100 ℃, finally obtain the alloy of vanadium nitride of 74.18%V-5.54%C-18.50%N-1.42%O, its apparent density is 3400kg/m
3
Embodiment 5:
After 50g carbon black, 150g Vanadium Pentoxide in FLAKES and 6g ferric oxide powder mixed, be pressed, pressure is 57MPa, and pressed compact is of a size of Φ 1.5cm * 1.0cm.Pressed compact is put into Reaktionsofen to be heated, before 650 ℃ of insulation 0.5h, feed high pure nitrogen, nitrogen pressure is 101325Pa, and at 1150 ℃ of insulation 1h, carbonization and nitrogenizing reaction take place, be cooled to subsequently come out of the stove below 100 ℃, finally obtain the alloy of vanadium nitride of 74.29%V-5.32%C-18.60%N-1.49%O, its apparent density is 3840kg/m
3
Embodiment 6:
After 48g carbon black, 152g Vanadium Pentoxide in FLAKES and 6g ferric oxide powder mixed, be pressed, pressure is 57MPa, and pressed compact is of a size of Φ 1.5cm * 1.0cm.Pressed compact is put into Reaktionsofen to be heated, before 650 ℃ of insulation 0.5h, feed high pure nitrogen, nitrogen pressure is 101325Pa, and at 1100 ℃ of insulation 1.5h, carbonization and nitrogenizing reaction take place, be cooled to subsequently come out of the stove below 100 ℃, finally obtain the alloy of vanadium nitride of 73.57%V-4.78%C-19.90%N-1.39%O, its apparent density is 3560kg/m
3
Claims (6)
1, a kind of preparation method of alloy of vanadium nitride; it is characterized in that: with oxide compound, carbonaceous pulvis and the density reinforcer of vanadium mix, compression moulding is placed in the Reaktionsofen; in 650 ℃ of insulation forward reaction stoves, feed nitrogen or ammonia as reaction and shielding gas; Reaktionsofen is heated to 1000～1250 ℃; material is at this temperature range generation carbonization and nitrogenizing reaction; reaction times is cooled to come out of the stove below 100 ℃ less than 3h subsequently, finally obtains alloy of vanadium nitride.Described alloy of vanadium nitride contains 73～80%V, 12～20%N, 3～8%C, 0.5～2.0%O, and its apparent density reaches 3000～4000kg/m
3
2, the preparation method of alloy of vanadium nitride as claimed in claim 1, the oxide compound that it is characterized in that described vanadium is V
2O
5, VO
2, V
2O
3Or VO a kind of or their mixture.
3, the preparation method of alloy of vanadium nitride as claimed in claim 1 is characterized in that described carbonaceous pulvis is carbon black, gac, graphite or wood charcoal powder.
4, the preparation method of alloy of vanadium nitride as claimed in claim 1 is characterized in that described density reinforcer is Fe, Co, Ni, Cr simple substance or its compound.
5, the preparation method of alloy of vanadium nitride as claimed in claim 1 is characterized in that described Reaktionsofen is carbon tube furnace, tube furnace, induction furnace, microwave agglomerating furnace, rotary kiln, shaft furnace, grate, pushed bat kiln or tunnel furnace.
6, the preparation method of alloy of vanadium nitride as claimed in claim 1 is characterized in that described carbonization and nitrogenizing reaction are in 1000～1250 ℃ of temperature ranges.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603132B (en) * | 2009-07-16 | 2011-05-11 | 钢铁研究总院 | Method and device for producing vanadium-nitrogen alloy |
| CN102465226A (en) * | 2010-11-16 | 2012-05-23 | 安阳昱千鑫冶金耐材有限公司 | Method for utilizing carbon-nitrogen-oxygen vanadium to prepare vanadium-nitrogen alloy |
| CN103255302A (en) * | 2013-05-06 | 2013-08-21 | 南通汉瑞实业有限公司 | Process for producing vanadium-nitrogen alloy by plasma nitrogen gas |
| CN103305739A (en) * | 2013-07-09 | 2013-09-18 | 高博 | High-nitrogen vanadium-nitrogen alloy VN18 and production method thereof |
| CN103834905A (en) * | 2012-11-27 | 2014-06-04 | 大连经济技术开发区圣洁真空技术开发有限公司 | New method for gas nitriding of tiny workpiece in rotary furnace |
| CN106048284A (en) * | 2016-06-13 | 2016-10-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium-nitrogen alloy and preparation method thereof |
| CN106636866A (en) * | 2015-11-02 | 2017-05-10 | 陕西华银科技有限公司 | Utilization method for heat and material in vanadium-nitrogen alloy preparation |
| CN107012385A (en) * | 2017-04-10 | 2017-08-04 | 攀钢集团研究院有限公司 | The preparation method of high nitrogen VN alloy |
| CN108545707A (en) * | 2018-04-23 | 2018-09-18 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on liquid phase carbothermy |
| CN109023028A (en) * | 2018-08-30 | 2018-12-18 | 成都锦钛精工科技有限公司 | Carbon chromium nitride hardening agent and preparation method thereof |
| CN109234602A (en) * | 2018-08-30 | 2019-01-18 | 成都锦钛精工科技有限公司 | Carbon chromium nitride vanadium alloy and preparation method thereof |
| CN112342421A (en) * | 2020-10-20 | 2021-02-09 | 长安大学 | Vanadium nitride multi-field coupling preparation process and device |
-
2007
- 2007-07-12 CN CN 200710049495 patent/CN101082089A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603132B (en) * | 2009-07-16 | 2011-05-11 | 钢铁研究总院 | Method and device for producing vanadium-nitrogen alloy |
| CN102465226A (en) * | 2010-11-16 | 2012-05-23 | 安阳昱千鑫冶金耐材有限公司 | Method for utilizing carbon-nitrogen-oxygen vanadium to prepare vanadium-nitrogen alloy |
| CN103834905A (en) * | 2012-11-27 | 2014-06-04 | 大连经济技术开发区圣洁真空技术开发有限公司 | New method for gas nitriding of tiny workpiece in rotary furnace |
| CN103255302A (en) * | 2013-05-06 | 2013-08-21 | 南通汉瑞实业有限公司 | Process for producing vanadium-nitrogen alloy by plasma nitrogen gas |
| CN103305739A (en) * | 2013-07-09 | 2013-09-18 | 高博 | High-nitrogen vanadium-nitrogen alloy VN18 and production method thereof |
| CN103305739B (en) * | 2013-07-09 | 2015-10-21 | 高博 | A kind of high nitrogen VN alloy VN18 and production method thereof |
| CN106636866A (en) * | 2015-11-02 | 2017-05-10 | 陕西华银科技有限公司 | Utilization method for heat and material in vanadium-nitrogen alloy preparation |
| CN106048284B (en) * | 2016-06-13 | 2018-11-30 | 四川攀研技术有限公司 | A kind of VN alloy and preparation method thereof |
| CN106048284A (en) * | 2016-06-13 | 2016-10-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium-nitrogen alloy and preparation method thereof |
| CN107012385A (en) * | 2017-04-10 | 2017-08-04 | 攀钢集团研究院有限公司 | The preparation method of high nitrogen VN alloy |
| CN108545707A (en) * | 2018-04-23 | 2018-09-18 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on liquid phase carbothermy |
| CN109023028A (en) * | 2018-08-30 | 2018-12-18 | 成都锦钛精工科技有限公司 | Carbon chromium nitride hardening agent and preparation method thereof |
| CN109234602A (en) * | 2018-08-30 | 2019-01-18 | 成都锦钛精工科技有限公司 | Carbon chromium nitride vanadium alloy and preparation method thereof |
| CN109023028B (en) * | 2018-08-30 | 2020-01-07 | 成都锦钛精工科技有限公司 | Chromium carbonitride reinforcer and preparation method thereof |
| CN109234602B (en) * | 2018-08-30 | 2020-02-21 | 成都锦钛精工科技有限公司 | Chromium vanadium carbonitride alloy and preparation method thereof |
| CN112342421A (en) * | 2020-10-20 | 2021-02-09 | 长安大学 | Vanadium nitride multi-field coupling preparation process and device |
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