CN105983688A - Fast preparation method for Ti(C1-x, Nx) (0<=x<=1)-Fe composite powder - Google Patents
Fast preparation method for Ti(C1-x, Nx) (0<=x<=1)-Fe composite powder Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of composite powder in a Ti(C, N) series and provides a method for preparing Ti(C1-x, Nx) (0<=x<=1)-Fe composite powder with titanium concentrate as a main raw material through fast in-situ carbon heat reduction (nitridation). The method specifically includes the steps that firstly, the Ti/C mass ratio is firstly determined according to a target product and titanium concentrate components, and materials are matched; then mechanical high-energy ball milling is performed on raw materials under the Ar gas protective atmosphere till nanocrystalline activated raw material powder which is mixed uniformly is acquired; and finally, a discharging plasma fast in-situ carbon thermal reduction(nitridation) reaction happens to the raw materials in vacuum or in the N2 atmosphere, and the Ti(C1-x, Nx) (0<=x<=1)-Fe composite powder is generated. Compared with conventional carbon thermal reduction(nitridation), the method has the beneficial effects that the temperature rise speed is very high, the synthesis temperature is low and the heat preservation time is short, and product powder smaller in grain size can be acquired more easily.
Description
Technical field
The invention belongs to the preparing technical field of Ti (C, N) series composite granule, more specifically, be a kind of with ilmenite concentrate as primary raw material, prepare Ti (C by plasma discharging quick in situ carbon thermal reduction (nitridation)1 – x ,N x ) (0≤x≤ 1) method of Fe composite granule.
Background technology
Ilmenite concentrate is got by natural titanium iron mine selecting and purchasing, and its resource reserve is big, distribution is wide, and price is comparatively inexpensive.At present, the main utilization ways of ilmenite concentrate has: one is that ilmenite concentrate electric furnace smelting process is made acid-soluble high titanium slag, is subsequently used for sulfate process titanium dioxide and produces；Two is that employing fluidizing chlorination or fused salt chlorimation legal system take TiC1 by ilmenite concentrate after enrichment processing becomes high titanium slag or synthetic rutile4.But, these utilize process all to there are one or more defects such as energy consumption producing level too high, ferrum is low, spent acid mother solution is difficult.To this end, Chinese scholars exploring ilmenite concentrate always utilize new way.In the middle of this, with ilmenite concentrate as primary raw material, making full use of Ti and the Fe two spike-type cultivars in ilmenite concentrate, low cost in-situ reducing synthesizes various titaniferous new materials and has many advantages, thus receives much concern.
At present, the in-situ reducing research of ilmenite concentrate concentrates on following several respects: first, the in-situ carbon thermal reduction of ilmenite concentrate.This method is to add a certain amount of inorganic carbon source laggard row mechanical ball milling batch mixing in ilmenite concentrate, next utilizes in-situ carbon thermal reduction to prepare TiC Fe, Ti (C, N) Fe composite granule or block materials.Second, the active metal in-situ reducing of ilmenite concentrate.This method is to add appropriate active metal in ilmenite concentrate to reduce ilmenite concentrate.Active metal owing to being usually added into is generally Al, Mg, Si etc., because of and be referred to as the aluminothermic reduction of ilmenite concentrate, magnesiothermic reduction, silicothermic reduction etc. respectively.3rd, the composite in-situ reduction of ilmenite concentrate.This method combines the advantage of first two method, reduces ilmenite concentrate by being simultaneously introduced inorganic carbon source and active metal in ilmenite concentrate, thus fabricated in situ contains two kinds of ceramic metal/ceramic composite granules or block materials.
In three of the above in-situ reducing technology, the in-situ carbon thermal reduction of ilmenite concentrate receives much concern owing to having the advantages such as simple, the easy industrial mass manufacture of technics comparing.In recent years, the research by conventional carbon thermal reduction (nitridation) reaction preparation TiC Fe or Ti (C, N) the Fe composite granule between ilmenite concentrate and inorganic carbon source is more.But, conventional carbon thermal reduction (nitridation) method heating rate is relatively slow, reaction temperature is higher, temperature retention time is longer, thus the preparation efficiency of powder body is relatively low, and the particle diameter of product powder body is relatively big, and preparation process power consumption is more.To this end, how to reduce carbon thermal reduction (nitridation) temperature of ilmenite concentrate, shorten temperature retention time, final within a short period of time, prepare thinner Ti (C1 – x ,N x ) (0≤x≤ 1) Fe composite granule or Ti (C1 – x ,N x ) (0≤x≤ 1) ceramic powder, provides suitable feedstock powder body for preparing high-performance metal ceramic composite, it appears extremely important.
Summary of the invention
Instant invention overcomes the technical disadvantages such as conventional carbon thermal reduction (nitridation) reaction temperature is higher, heating rate is relatively slow, temperature retention time is longer, provide a kind of with ilmenite concentrate as primary raw material, prepare fine Ti (C by relatively low temperature quick in situ carbon thermal reduction (nitridation)1 – x ,N x ) (0≤x≤ 1) method of Fe composite granule.
In order to solve above-mentioned technical problem, the present invention is achieved by the following technical solutions:
A kind of Ti (C1 – x ,N x ) (0≤x≤ 1) fast preparation method of Fe composite granule, it is characterised in that comprise the technical steps that:
(1) preparation of material powder and dispensing
According to prepared Ti (C1 – x ,N x ) (0≤x≤ 1) Fe target product composition, and combine the chemical composition of ilmenite concentrate, determines initial feed Ti/C mass proportioning, by ilmenite concentrate and carbon source powder body according to determining that proportioning weighs dispensing；
(2) mechanical ball milling of material powder activates
Preparing raw material and hard alloy abrading-ball is put in ball grinder by above-mentioned, high energy ball mill carrying out mechanical ball milling to raw material under Ar gas shielded atmosphere, until obtaining mixed uniformly nanocrystalline activation material powder；
(3) the quick preparation of product composite granule
After above-mentioned ball milling is activated powder body loading graphite jig, it is placed in discharge plasma sintering system heating intracavity, at vacuum or N2Being rapidly heated under atmospheric condition, raw material generation in-situ carbon thermal reduction (nitridation) reacts, and generates Ti (C1 – x ,N x ) (0≤x≤ 1) Fe composite granule.
The ratio of grinding media to material that described raw material mechanical ball milling activates is 10:1 30:1, and Ball-milling Time is 10 40h.
The process conditions that TiC Fe composite granule is prepared in described plasma discharging in-situ carbon thermal reduction are as follows:
System pressure 1 3KN, initial depression < 1Pa, 100 400 DEG C/min of heating rate, synthesis temperature 1,250 1400 DEG C, temperature retention time 5 15min.
The process conditions that described plasma discharging carbothermal reduction-nitridation in situ prepares Ti (C, N) Fe composite granule are as follows:
System pressure 1 3KN, N2Pressure 0.1 1KPa, 100 400 DEG C/min of heating rate, synthesis temperature 1,200 1350 DEG C, temperature retention time 5 15min.
The process conditions that described plasma discharging carbothermal reduction-nitridation in situ prepares TiN Fe composite granule are as follows:
System pressure 1 3KN, N2Pressure 1 2KPa, 100 400 DEG C/min of heating rate, synthesis temperature 1,150 1300 DEG C, temperature retention time 5 15min.
Described product Ti (C1 – x ,N x ) (0≤x≤ 1) Fe composite granule is put in diluted acid and is soaked, and can obtain Ti (C further through filtration drying1 – x ,N x ) (0≤x≤ 1) powder body.
Compared to existing technology, the present invention has a following outstanding advantages:
1. titanium source used by the present invention is ilmenite selecting and purchasing ilmenite concentrate out, and its source is very wide, price is at a fairly low, has bigger cost of material advantage in industrial mass manufacture.
2. the present invention utilizes high-energy ball milling that raw material carries out pretreatment, not only can obtain mixed uniformly nanocrystalline material powder, and mechanical activation can improve raw material reaction driving force and diffusivity, and the reactivity of reinforcing component reduces follow-up synthesis temperature.
3. the present invention takes full advantage of the technical characterstic of discharge plasma sintering, and relatively conventional carbon thermal reduction (nitridation) is reacted, have heating rate quickly, the advantage such as synthesis temperature is relatively low, temperature retention time is the shortest, it is easier to obtain the product powder body that particle diameter is thinner.
Detailed description of the invention
Below with FeTiO3The mass fraction ilmenite concentrate more than 97% is primary raw material, and the invention will be further described in conjunction with specific embodiments, but embodiments of the present invention are not limited to this.
Embodiment 1
The fast preparation method of the TiC Fe composite granule of the present embodiment, comprises the following steps and process conditions:
(1) preparation of material powder and dispensing
According to prepared TiC Fe target product, and combine the chemical composition of ilmenite concentrate, determine that initial feed Ti/C mass proportioning is 3:1, ilmenite concentrate and carbon black are weighed dispensing according to this proportioning.
(2) mechanical ball milling of material powder activates
The above-mentioned raw material for preparing is put in stainless steel jar mill, and puts into hard alloy abrading-ball by ratio of grinding media to material 10:1, high-energy ball milling machine carries out mechanical ball milling 30h to raw material under Ar gas shielded atmosphere, it is thus achieved that mixed uniformly nanocrystalline activation material powder.
(3) the quick preparation of product composite granule
After above-mentioned 10g ball milling is activated powder body loading Φ 50 graphite jig, it is placed in discharge plasma sintering system heating intracavity, carry out plasma discharging in-situ carbon thermal reduction reaction, process conditions are as follows: system pressure 2KN, initial depression < 1Pa, 350 DEG C/min of heating rate, synthesis temperature 1350 DEG C, temperature retention time 10min.
By method made above, final acquisition particle diameter TiC Fe composite granule about 0.5 μm；This composite granule is put into immersion 15h in 20% dilute hydrochloric acid solution, after filtration drying, obtains submicron TiC powder.
Embodiment 2
Ti (the C of the present embodiment0.7,N0.3) fast preparation method of Fe composite granule, comprise the following steps and process conditions:
(1) preparation of material powder and dispensing
According to prepared Ti (C0.7,N0.3) Fe target product, and combine the chemical composition of ilmenite concentrate, determine that initial feed Ti/C mass proportioning is 3.3:1, ilmenite concentrate and carbon black are weighed dispensing according to this proportioning.
(2) mechanical ball milling of material powder activates
The above-mentioned raw material for preparing is put in stainless steel jar mill, and puts into hard alloy abrading-ball by ratio of grinding media to material 20:1, high-energy ball milling machine carries out mechanical ball milling 20h to raw material under Ar gas shielded atmosphere, it is thus achieved that mixed uniformly nanocrystalline activation material powder.
(3) the quick preparation of product composite granule
After above-mentioned 10g ball milling activates powder body loading Φ 50 graphite jig, being placed in discharge plasma sintering system heating intracavity, carry out plasma discharging in-situ carbon thermal reduction nitridation reaction, process conditions are as follows: system pressure 1KN, N2Pressure 0.3KPa, 300 DEG C/min of heating rate, synthesis temperature 1320 DEG C, temperature retention time 10min.
By method made above, final acquisition particle diameter Ti (C about 0.5 μm0.7,N0.3) Fe composite granule；This composite granule is put into immersion 15h in 20% dilute hydrochloric acid solution, after filtration drying, obtains submicron Ti (C0.7,N0.3) powder body.
Embodiment 3
Ti (the C of the present embodiment0.5,N0.5) fast preparation method of Fe composite granule, comprise the following steps and process conditions:
(1) preparation of material powder and dispensing
According to prepared Ti (C0.5,N0.5) Fe target product, and combine the chemical composition of ilmenite concentrate, determine that initial feed Ti/C mass proportioning is 3.5:1, ilmenite concentrate and carbon black are weighed dispensing according to this proportioning.
(2) mechanical ball milling of material powder activates
The above-mentioned raw material for preparing is put in stainless steel jar mill, and puts into hard alloy abrading-ball by ratio of grinding media to material 15:1, high-energy ball milling machine carries out mechanical ball milling 25h to raw material under Ar gas shielded atmosphere, it is thus achieved that mixed uniformly nanocrystalline activation material powder.
(3) the quick preparation of product composite granule
After above-mentioned 10g ball milling activates powder body loading Φ 50 graphite jig, being placed in discharge plasma sintering system heating intracavity, carry out plasma discharging in-situ carbon thermal reduction nitridation reaction, process conditions are as follows: system pressure 1KN, N2Pressure 0.5KPa, 250 DEG C/min of heating rate, synthesis temperature 1280 DEG C, temperature retention time 12min.
By method made above, final acquisition particle diameter Ti (C below 0.5 μm0.5,N0.5) Fe composite granule；This composite granule is put into immersion 15h in 20% dilute hydrochloric acid solution, after filtration drying, obtains superfine Ti (C0.5,N0.5) powder body.
Embodiment 4
Ti (the C of the present embodiment0.3,N0.7) fast preparation method of Fe composite granule, comprise the following steps and process conditions:
(1) preparation of material powder and dispensing
According to prepared Ti (C0.3,N0.7) Fe target product, and combine the chemical composition of ilmenite concentrate, determine that initial feed Ti/C mass proportioning is 3.7:1, ilmenite concentrate and carbon black are weighed dispensing according to this proportioning.
(2) mechanical ball milling of material powder activates
The above-mentioned raw material for preparing is put in stainless steel jar mill, and puts into hard alloy abrading-ball by ratio of grinding media to material 25:1, high-energy ball milling machine carries out mechanical ball milling 15h to raw material under Ar gas shielded atmosphere, it is thus achieved that mixed uniformly nanocrystalline activation material powder.
(3) the quick preparation of product composite granule
After above-mentioned 10g ball milling activates powder body loading Φ 50 graphite jig, being placed in discharge plasma sintering system heating intracavity, carry out plasma discharging in-situ carbon thermal reduction nitridation reaction, process conditions are as follows: system pressure 1KN, N2Pressure 0.7KPa, 200 DEG C/min of heating rate, synthesis temperature 1240 DEG C, temperature retention time 8min.
By method made above, final acquisition particle diameter Ti (C below 0.5 μm0.3,N0.7) Fe composite granule；This composite granule is put into immersion 15h in 20% dilute hydrochloric acid solution, after filtration drying, obtains superfine Ti (C0.3,N0.7) powder body.
Embodiment 5
The fast preparation method of the TiN Fe composite granule of the present embodiment, comprises the following steps and process conditions:
(1) preparation of material powder and dispensing
According to prepared TiN Fe target product, and combine the chemical composition of ilmenite concentrate, determine that initial feed Ti/C mass proportioning is 4.1:1, ilmenite concentrate and carbon black are weighed dispensing according to this proportioning.
(2) mechanical ball milling of material powder activates
The above-mentioned raw material for preparing is put in stainless steel jar mill, and puts into hard alloy abrading-ball by ratio of grinding media to material 25:1, high-energy ball milling machine carries out mechanical ball milling 10h to raw material under Ar gas shielded atmosphere, it is thus achieved that mixed uniformly nanocrystalline activation material powder.
(3) the quick preparation of product composite granule
After above-mentioned 10g ball milling activates powder body loading Φ 50 graphite jig, being placed in discharge plasma sintering system heating intracavity, carry out plasma discharging in-situ carbon thermal reduction nitridation reaction, process conditions are as follows: system pressure 1KN, N2Pressure 1.5KPa, 150 DEG C/min of heating rate, synthesis temperature 1210 DEG C, temperature retention time 10min.
By method made above, final acquisition particle diameter TiN Fe composite granule below 0.4 μm；This composite granule is put into immersion 15h in 20% dilute hydrochloric acid solution, after filtration drying, obtains superfine Ti N powder body.
Claims (6)
1. a Ti (C1 –x,Nx ) (0≤x≤ 1) fast preparation method of Fe composite granule, it is characterised in that comprise the technical steps that:
(1) preparation of material powder and dispensing
According to prepared Ti (C1 –x,Nx ) (0≤x≤ 1) Fe target product composition, and combine the chemical composition of ilmenite concentrate, determines initial feed Ti/C mass proportioning, by ilmenite concentrate and carbon source powder body according to determining that proportioning weighs dispensing；
(2) mechanical ball milling of material powder activates
Preparing raw material and hard alloy abrading-ball is put in ball grinder by above-mentioned, high energy ball mill carrying out mechanical ball milling to raw material under Ar gas shielded atmosphere, until obtaining mixed uniformly nanocrystalline activation material powder；
(3) the quick preparation of product composite granule
After above-mentioned ball milling is activated powder body loading graphite jig, it is placed in discharge plasma sintering system heating intracavity, at vacuum or N2Being rapidly heated under atmospheric condition, raw material generation in-situ carbon thermal reduction (nitridation) reacts, and generates Ti (C1 –x,Nx ) (0≤x≤ 1) Fe composite granule.
A kind of Ti (C the most according to claim 11 –x,Nx ) (0≤x≤ 1) fast preparation method of Fe composite granule, it is characterised in that the ratio of grinding media to material that described raw material mechanical ball milling activates is 10:1 30:1, and Ball-milling Time is 10 40h.
A kind of Ti (C the most according to claim 11 –x,Nx ) (0≤x≤ 1) fast preparation method of Fe composite granule, it is characterised in that the process conditions that TiC Fe composite granule is prepared in described plasma discharging in-situ carbon thermal reduction are as follows:
System pressure 1 3KN, initial depression < 1Pa, 100 400 DEG C/min of heating rate, synthesis temperature 1,250 1400 DEG C, temperature retention time 5 15min.
A kind of Ti (C the most according to claim 11 –x,Nx ) (0≤x≤ 1) fast preparation method of Fe composite granule, it is characterised in that the process conditions that described plasma discharging carbothermal reduction-nitridation in situ prepares Ti (C, N) Fe composite granule are as follows:
System pressure 1 3KN, N2Pressure 0.1 1KPa, 100 400 DEG C/min of heating rate, synthesis temperature 1,200 1350 DEG C, temperature retention time 5 15min.
A kind of Ti (C the most according to claim 11 –x,Nx ) (0≤x≤ 1) fast preparation method of Fe composite granule, it is characterised in that the process conditions that described plasma discharging carbothermal reduction-nitridation in situ prepares TiN Fe composite granule are as follows:
System pressure 1 3KN, N2Pressure 1 2KPa, 100 400 DEG C/min of heating rate, synthesis temperature 1,150 1300 DEG C, temperature retention time 5 15min.
A kind of Ti (C the most according to claim 11 –x,Nx ) (0≤x≤ 1) fast preparation method of Fe composite granule, it is characterised in that described product Ti (C1 –x,Nx ) (0≤x≤ 1) Fe composite granule is put in diluted acid and is soaked, and can obtain Ti (C further through filtration drying1 –x,Nx ) (0≤x≤ 1) powder body.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108080648A (en) * | 2017-12-18 | 2018-05-29 | 北京科技大学 | A kind of method that Fe/TiC composite granules are prepared in situ in vacuum carbothermal reduction |
| CN109338196A (en) * | 2018-11-30 | 2019-02-15 | 肖水清 | Ti (C, N) based ceramic metal and its preparation method and application |
| CN110467160A (en) * | 2019-09-25 | 2019-11-19 | 攀钢集团钒钛资源股份有限公司 | Carbothermal reduction-nitridation prepares the feedstock composition of titanium nitride and the preparation method of titanium nitride |
| CN115353145A (en) * | 2022-08-26 | 2022-11-18 | 中国矿业大学 | Preparation of Sn (Ba, ca) TiO by using vacuum plasma field assisted sol-gel technology 3 Method for producing powder |
| CN115518627A (en) * | 2022-09-21 | 2022-12-27 | 四川师范大学 | Preparation method and application of defect perovskite type catalyst |
| CN116393705A (en) * | 2023-05-11 | 2023-07-07 | 宝鸡市永盛泰钛业有限公司 | Titanium alloy material for 3D printing and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108080648A (en) * | 2017-12-18 | 2018-05-29 | 北京科技大学 | A kind of method that Fe/TiC composite granules are prepared in situ in vacuum carbothermal reduction |
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| CN110467160A (en) * | 2019-09-25 | 2019-11-19 | 攀钢集团钒钛资源股份有限公司 | Carbothermal reduction-nitridation prepares the feedstock composition of titanium nitride and the preparation method of titanium nitride |
| CN115353145A (en) * | 2022-08-26 | 2022-11-18 | 中国矿业大学 | Preparation of Sn (Ba, ca) TiO by using vacuum plasma field assisted sol-gel technology 3 Method for producing powder |
| CN115353145B (en) * | 2022-08-26 | 2023-11-24 | 中国矿业大学 | Sn (Ba, ca) TiO prepared by vacuum plasma field assisted sol-gel technology 3 Method for preparing powder |
| CN115518627A (en) * | 2022-09-21 | 2022-12-27 | 四川师范大学 | Preparation method and application of defect perovskite type catalyst |
| CN115518627B (en) * | 2022-09-21 | 2023-10-13 | 四川师范大学 | Preparation method and application of defect perovskite type catalyst |
| CN116393705A (en) * | 2023-05-11 | 2023-07-07 | 宝鸡市永盛泰钛业有限公司 | Titanium alloy material for 3D printing and preparation method thereof |
| CN116393705B (en) * | 2023-05-11 | 2023-09-08 | 宝鸡市永盛泰钛业有限公司 | Titanium alloy material for 3D printing and preparation method thereof |
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Application publication date: 20161005 |