CN106966730A - A kind of fine and close TiC materials and preparation method thereof - Google Patents
A kind of fine and close TiC materials and preparation method thereof Download PDFInfo
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- CN106966730A CN106966730A CN201710184692.3A CN201710184692A CN106966730A CN 106966730 A CN106966730 A CN 106966730A CN 201710184692 A CN201710184692 A CN 201710184692A CN 106966730 A CN106966730 A CN 106966730A
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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Abstract
The present invention relates to a kind of fine and close TiC materials and preparation method thereof.Its technical scheme is：It is 100 ︰ (2 ~ 5) dispensing by the mass ratio of ferrotianium Zha ︰ Brown Alundums, ball milling obtains ferrotianium ground-slag end.It is 100 ︰ (5 ~ 10) dispensing by the mass ratio of the ferrotianium ground-slag Mo ︰ coke blackings, mixing obtains mixed-powder.The mixed-powder is added in vacuum arc furnace ignition, under the conditions of less than 0.1Pa and 1930 ~ 2005 DEG C, 0.5 ~ 1 hour is incubated；Upper strata scum silica frost is removed, furnace cooling is crushed, and presoma TiC materials are made.It is 1 ︰ (4 ~ 7) by the mass ratio of the presoma TiC Cai Liao ︰ hydrochloric acid solutions, the hydrochloric acid solution is added into the presoma TiC materials, stir, washing and suction filtration is dried, produce fine and close TiC materials.The present invention has technique simple and the characteristics of low production cost, and fine and close TiC material purities height, advantages of good crystallization and the densification degree prepared with this method is excellent.
Description
Technical field
The invention belongs to TiC field of material technology.Specifically related to a kind of fine and close TiC materials and preparation method thereof.
Background technology
Metal carbides are new non-oxidized substance function ceramics, have the advantages that fusing point height, intensity are big and wear-resistant, such as
A kind of " tabular Cr using ferrochrome slag as major ingredient7C3And preparation method thereof " (CN201510647704.2) patented technology, but prepare work
Skill is more complicated or energy consumption is larger.Therefore, the preparation of inexpensive, high performance carbide material directly affects its application.
TiC belongs to NaCl type face-centred cubic structures, with the characteristic such as fusing point is high, hardness is big and chemical stability is good, answers extensively
For fields such as cermet, hard alloy, high-abrasive material and high-temperature vacuum devices.At present, the method for preparing TiC materials is main
For direct carborization and carbothermic method.
TiC is prepared using direct carborization, typically so that Ti is titanium source or is aided with other metals, in inert gas shielding and height
Under the conditions of temperature, occurs carburizing reagent with carbon black or other carbon sources.TiC is prepared using direct carborization, one side carburizing reagent
Temperature is higher, and energy consumption is big, undoubtedly increases TiC preparation cost；On the other hand, often also need to draw in carbonation reaction
Enter other additives, such as Ni and Co, and then cause to prepare and easily produce new impurities phase during TiC, reduce the pure of TiC
Degree.
TiC is prepared using carbothermic method, mainly with carbon black（Or the carbon source such as nano carbon black, resin）And TiO2For raw material,
It is heat-treated after premix under certain atmospheric condition.TiC is prepared using carbothermic method, using what is discharged in C oxidizing process
Amount of heat and the temperature for reducing reduction reaction, but the accurate control to excessive C is difficult to, it is easily caused TiO2Reduction it is inadequate
Thoroughly form interphase（TiO）, reduce the purity of TiC materials.
The content of the invention
It is contemplated that overcoming prior art defect, it is therefore an objective to provide that a kind of technique is simple and the low densification of production cost
The preparation method of TiC materials.It is excellent with densification TiC material purities height, advantages of good crystallization and densification degree prepared by this method.
To achieve the above object, the technical solution adopted by the present invention is comprised the concrete steps that：
Step 1: being 100 ︰ (2 ~ 5) dispensing by the mass ratio of ferrotianium Zha ︰ Brown Alundums, granularity≤100 μm are milled to, ferrotianium is obtained
Ground-slag end.
Step 2: being 100 ︰ (5 ~ 10) dispensing by the mass ratio of the ferrotianium ground-slag Mo ︰ coke blackings, mix 10 ~ 15 minutes,
Obtain mixed-powder.
Step 3: the mixed-powder is added in vacuum arc furnace ignition, under the conditions of less than 0.1Pa, it is warming up to 1930 ~
2005 DEG C, it is incubated 0.5 ~ 1 hour；Upper strata scum silica frost is removed, room temperature is cooled to the furnace, is crushed to 1 ~ 2mm, presoma TiC materials are made
Material.
Step 4: being 1 ︰ (4 ~ 7) by the mass ratio of presoma TiC Cai Liao ︰ hydrochloric acid solutions, to the presoma TiC materials
It is middle to add the hydrochloric acid solution that concentration is 1 ~ 2mol/L, stir 20 ~ 30 minutes, successively washing and suction filtration 4 ~ 5 times, microwave is done
It is dry, produce fine and close TiC materials.
The ferrotianium slag is smelts the clinker produced by ferro-titanium, and the main chemical compositions of the ferrotianium slag are：Al2O3
Content is 65 ~ 75wt%, TiO2Content is 5 ~ 15wt%, and CaO content is 5 ~ 8wt%.
The Al of the Brown Alundum2O3Content >=96wt%.
Granularity≤100 μm of the coke blacking；C content >=93wt% of the coke blacking.
The hydrochloric acid is pure to analyze.
Due to using above-mentioned technical proposal, the present invention has following good effect compared with prior art：
1st, the present invention is so that solid waste --- ferrotianium slag extracts valuable component and then preparation as primary raw material through carburizing reagent
TiC, can not only effectively utilize waste material, and can significantly reduce the preparation cost of fine and close TiC materials.
2nd, the liquid phase that the present invention is formed under the high temperature conditions using impurity composition in ferrotianium slag, greatly reduces carburizing reagent
Temperature, increase carburizing reagent speed, promote TiC materials crystallization, enhance the consistency of fine and close TiC materials.
3rd, the present invention completely cuts off contacts of the TiC with external environment using " solid-liquid " delaminating deposition in reduction process,
Improve the purity of fine and close TiC materials.
Fine and close TiC materials prepared by the present invention are after measured：Grain size is 4 ~ 7 μm；Real density is 4.33 ~ 4.38g/cm3；Gas
Porosity is 0.2 ~ 0.7%.
Therefore, the present invention has technique simple and the characteristics of low production cost, and the fine and close TiC materials prepared with this method are pure
Degree is high, advantages of good crystallization and densification degree are excellent.
Embodiment
With reference to embodiment, the invention will be further described, not to the limitation of its protection domain：
It is first that the raw material Unify legislation involved by present embodiment is as follows to avoid repeating, repeated no more in embodiment：
The ferrotianium slag is smelts the clinker produced by ferro-titanium, and the main chemical compositions of the ferrotianium slag are：Al2O3Content
For 65 ~ 75wt%, TiO2Content is 5 ~ 15wt%, and CaO content is 5 ~ 8wt%.
The Al of the Brown Alundum2O3Content >=96wt%.
Granularity≤100 μm of the coke blacking；C content >=93wt% of the coke blacking.
The hydrochloric acid is pure to analyze.
Embodiment 1
A kind of fine and close TiC materials and preparation method thereof.Preparation method described in the present embodiment is comprised the concrete steps that：
Step 1: being 100 ︰ (2 ~ 4) dispensing by the mass ratio of ferrotianium Zha ︰ Brown Alundums, granularity≤100 μm are milled to, ferrotianium is obtained
Ground-slag end.
Step 2: being 100 ︰ (5 ~ 7) dispensing by the mass ratio of the ferrotianium ground-slag Mo ︰ coke blackings, mix 10 ~ 15 minutes,
Obtain mixed-powder.
Step 3: the mixed-powder is added in vacuum arc furnace ignition, under the conditions of less than 0.1Pa, it is warming up to 1930 ~
1960 DEG C, it is incubated 0.5 ~ 1 hour；Upper strata scum silica frost is removed, room temperature is cooled to the furnace, is crushed to 1 ~ 2mm, presoma TiC materials are made
Material.
Step 4: being 1 ︰ (4 ~ 6) by the mass ratio of presoma TiC Cai Liao ︰ hydrochloric acid solutions, to the presoma TiC materials
It is middle to add the hydrochloric acid solution that concentration is 1 ~ 2mol/L, stir 20 ~ 30 minutes, successively washing and suction filtration 4 ~ 5 times, microwave is done
It is dry, produce fine and close TiC materials.
Fine and close TiC materials manufactured in the present embodiment are after measured：Grain size is 4 ~ 6 μm；Real density is 4.33 ~ 4.35g/cm3；
The porosity is 0.2 ~ 0.4%.
Embodiment 2
A kind of fine and close TiC materials and preparation method thereof.Preparation method described in the present embodiment is comprised the concrete steps that：
Step 1: being 100 ︰ (2 ~ 4) dispensing by the mass ratio of ferrotianium Zha ︰ Brown Alundums, granularity≤100 μm are milled to, ferrotianium is obtained
Ground-slag end.
Step 2: being 100 ︰ (6 ~ 8) dispensing by the mass ratio of the ferrotianium ground-slag Mo ︰ coke blackings, mix 10 ~ 15 minutes,
Obtain mixed-powder.
Step 3: the mixed-powder is added in vacuum arc furnace ignition, under the conditions of less than 0.1Pa, it is warming up to 1945 ~
1975 DEG C, it is incubated 0.5 ~ 1 hour；Upper strata scum silica frost is removed, room temperature is cooled to the furnace, is crushed to 1 ~ 2mm, presoma TiC materials are made
Material.
Step 4: being 1 ︰ (4 ~ 6) by the mass ratio of presoma TiC Cai Liao ︰ hydrochloric acid solutions, to the presoma TiC materials
It is middle to add the hydrochloric acid solution that concentration is 1 ~ 2mol/L, stir 20 ~ 30 minutes, successively washing and suction filtration 4 ~ 5 times, microwave is done
It is dry, produce fine and close TiC materials.
Fine and close TiC materials manufactured in the present embodiment are after measured：Grain size is 4 ~ 6 μm；Real density is 4.34 ~ 4.36g/cm3；
The porosity is 0.3 ~ 0.5%.
Embodiment 3
A kind of fine and close TiC materials and preparation method thereof.Preparation method described in the present embodiment is comprised the concrete steps that：
Step 1: being 100 ︰ (3 ~ 5) dispensing by the mass ratio of ferrotianium Zha ︰ Brown Alundums, granularity≤100 μm are milled to, ferrotianium is obtained
Ground-slag end.
Step 2: being 100 ︰ (7 ~ 9) dispensing by the mass ratio of the ferrotianium ground-slag Mo ︰ coke blackings, mix 10 ~ 15 minutes,
Obtain mixed-powder.
Step 3: the mixed-powder is added in vacuum arc furnace ignition, under the conditions of less than 0.1Pa, it is warming up to 1960 ~
1990 DEG C, it is incubated 0.5 ~ 1 hour；Upper strata scum silica frost is removed, room temperature is cooled to the furnace, is crushed to 1 ~ 2mm, presoma TiC materials are made
Material.
Step 4: being 1 ︰ (5 ~ 7) by the mass ratio of presoma TiC Cai Liao ︰ hydrochloric acid solutions, to the presoma TiC materials
It is middle to add the hydrochloric acid solution that concentration is 1 ~ 2mol/L, stir 20 ~ 30 minutes, successively washing and suction filtration 4 ~ 5 times, microwave is done
It is dry, produce fine and close TiC materials.
Fine and close TiC materials manufactured in the present embodiment are after measured：Grain size is 5 ~ 7 μm；Real density is 4.35 ~ 4.37g/cm3；
The porosity is 0.4 ~ 0.6%.
Embodiment 4
A kind of fine and close TiC materials and preparation method thereof.Preparation method described in the present embodiment is comprised the concrete steps that：
Step 1: being 100 ︰ (3 ~ 5) dispensing by the mass ratio of ferrotianium Zha ︰ Brown Alundums, granularity≤100 μm are milled to, ferrotianium is obtained
Ground-slag end.
Step 2: being 100 ︰ (8 ~ 10) dispensing by the mass ratio of the ferrotianium ground-slag Mo ︰ coke blackings, mix 10 ~ 15 minutes,
Obtain mixed-powder.
Step 3: the mixed-powder is added in vacuum arc furnace ignition, under the conditions of less than 0.1Pa, it is warming up to 1975 ~
2005 DEG C, it is incubated 0.5 ~ 1 hour；Upper strata scum silica frost is removed, room temperature is cooled to the furnace, is crushed to 1 ~ 2mm, presoma TiC materials are made
Material.
Step 4: being 1 ︰ (5 ~ 7) by the mass ratio of presoma TiC Cai Liao ︰ hydrochloric acid solutions, to the presoma TiC materials
It is middle to add the hydrochloric acid solution that concentration is 1 ~ 2mol/L, stir 20 ~ 30 minutes, successively washing and suction filtration 4 ~ 5 times, microwave is done
It is dry, produce fine and close TiC materials.
Fine and close TiC materials manufactured in the present embodiment are after measured：Grain size is 5 ~ 7 μm；Real density is 4.36 ~ 4.38g/cm3；
The porosity is 0.5 ~ 0.7%.
Due to using above-mentioned technical proposal, present embodiment has following good effect compared with prior art：
1st, present embodiment is so that solid waste --- ferrotianium slag extracts valuable component as primary raw material, through carburizing reagent and entered
And TiC is prepared, waste material can not only be effectively utilized, and the preparation cost of fine and close TiC materials can be significantly reduced.
2nd, present embodiment utilizes the liquid phase that impurity composition is formed under the high temperature conditions in ferrotianium slag, greatly reduces
The temperature of carburizing reagent, increases carburizing reagent speed, promotes the crystallization of TiC materials, enhances the consistency of fine and close TiC materials.
3rd, present embodiment utilizes " solid-liquid " delaminating deposition in reduction process, isolation TiC and external environment
Contact, improve the purity of fine and close TiC materials.
Fine and close TiC materials prepared by present embodiment are after measured：Grain size is 4 ~ 7 μm；Real density be 4.33 ~
4.38g/cm3；The porosity is 0.2 ~ 0.7%.
Therefore, present embodiment has technique simple and the characteristics of production cost is low, the densification prepared with this method
TiC material purities are high, advantages of good crystallization and densification degree are excellent.
Claims (6)
1. a kind of preparation method of fine and close TiC materials, it is characterised in that the preparation method is comprised the concrete steps that：
Step 1: being 100 ︰ (2~5) dispensing by the mass ratio of ferrotianium Zha ︰ Brown Alundums, granularity≤100 μm are milled to, ferrotianium is obtained
Ground-slag end；
Step 2: being 100 ︰ (5~10) dispensing by the mass ratio of the ferrotianium ground-slag Mo ︰ coke blackings, mix 10~15 minutes, obtain
To mixed-powder；
Step 3: the mixed-powder is added in vacuum arc furnace ignition, under the conditions of less than 0.1Pa, 1930~2005 are warming up to
DEG C, it is incubated 0.5~1 hour；Upper strata scum silica frost is removed, room temperature is cooled to the furnace, is crushed to 1~2mm, presoma TiC materials are made；
Step 4: being 1 ︰ (4~7) by the mass ratio of presoma TiC Cai Liao ︰ hydrochloric acid solutions, add into the presoma TiC materials
Enter the hydrochloric acid solution that concentration is 1~2mol/L, stir 20~30 minutes, successively washing and suction filtration 4~5 times, microwave drying,
Produce fine and close TiC materials.
2. the preparation method of fine and close TiC materials according to claim 1, it is characterised in that the ferrotianium slag is smelting ferrotianium
Clinker produced by alloy, the main chemical compositions of the ferrotianium slag are：Al2O3Content is 65~75wt%, TiO2Content is 5
~15wt%, CaO content is 5~8wt%.
3. the preparation method of fine and close TiC materials according to claim 1, it is characterised in that the Al of the Brown Alundum2O3Content
>=96wt%.
4. the preparation method of fine and close TiC materials according to claim 1, it is characterised in that the granularity of the coke blacking≤
100μm；C content >=93wt% of the coke blacking.
5. the preparation method of fine and close TiC materials according to claim 1, it is characterised in that the hydrochloric acid is pure to analyze.
6. a kind of fine and close TiC materials, it is characterised in that the fine and close TiC materials are according to any one of Claims 1 to 5 institute
Fine and close TiC materials prepared by the preparation method for the fine and close TiC materials stated.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558417A (en) * | 2018-01-09 | 2018-09-21 | 武汉科技大学 | A kind of titanium calcium aluminate fireclay insulating refractory and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152652A (en) * | 2015-10-09 | 2015-12-16 | 武汉科技大学 | Plate-shaped Cr with ferrochrome slag as main material7C3And method for preparing the same |
| CN105567970A (en) * | 2016-01-05 | 2016-05-11 | 北京科技大学 | Titanium carbide prepared by adopting ilmenite and smelting process and application of titanium carbide |
| CN106315584A (en) * | 2016-08-29 | 2017-01-11 | 重庆大学 | Method for preparing carbon-doped titanium oxide or/and titanium carbide from titanium-containing mineral or slag |
-
2017
- 2017-03-24 CN CN201710184692.3A patent/CN106966730A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152652A (en) * | 2015-10-09 | 2015-12-16 | 武汉科技大学 | Plate-shaped Cr with ferrochrome slag as main material7C3And method for preparing the same |
| CN105567970A (en) * | 2016-01-05 | 2016-05-11 | 北京科技大学 | Titanium carbide prepared by adopting ilmenite and smelting process and application of titanium carbide |
| CN106315584A (en) * | 2016-08-29 | 2017-01-11 | 重庆大学 | Method for preparing carbon-doped titanium oxide or/and titanium carbide from titanium-containing mineral or slag |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558417A (en) * | 2018-01-09 | 2018-09-21 | 武汉科技大学 | A kind of titanium calcium aluminate fireclay insulating refractory and preparation method thereof |
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Application publication date: 20170721 |