CN110304653A - A kind of surface modifying method of titanium carbide granule - Google Patents
A kind of surface modifying method of titanium carbide granule Download PDFInfo
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- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention belongs to field of smelting, and in particular to a kind of surface modifying method of titanium carbide granule.Titanium carbide granule is mixed with alkali metal chloride, Titanium, sodium fluoride and titanium chloride, graphite powder first, is placed in 1101 DEG C -1199 DEG C of alkali metal chloride fused salt.Return middle characteristic using the disproportionation-of titanium elements, modify the sintering character of the surface, the spherical coefficient of raising of titanium carbide granule to improve titanium carbide powder using Titanium and graphite powder as raw material.The modified-reaction of invention titanium carbide carries out in molten salt bath, and reactant ion diffusion conditions are good, improves the surface nature of titanium carbide, and product titanium carbide surface is smooth, and spherical coefficient is high.
Description
Technical field
The invention belongs to Material Fields, are related to a kind of surface modifying method of titanium carbide granule.
Technical background
Titanium carbide has many excellent properties such as high temperature resistant, high intensity, corrosion-resistant, high thermal conductivity, is widely used in metal
The numerous areas such as ceramics, cutter material, wearing-proof refractory material, heat-resisting alloy.The particle properties of titanium carbide are to influence its burning
An important factor for tying performance.Common titanium carbide production method includes: carbothermic method, direct carborization, chemical vapor deposition
Method, self-propagating high-temperature synthetic method.For titanium carbide granule, the diffusion conditions of these methods are bad, and product titanium carbide quality is not
Height, application performance are limited.
Chinese invention patent CN108754491A discloses a kind of titanium alloy surface method of modifying and its surface Modified Titanium closes
Gold.Related titanium alloy surface method of modifying is the following steps are included: 1) titanium alloy substrate is fusion covers surface preparation；2) cladding
Material is prepared.After titanium carbide spherical powder and the drying of titanium alloy spherical powder, according to mass ratio 30~40；60~70 mixing are equal
It is even, obtain mixed-powder；3) laser melting coating.Cladding material is prepared in (step 2) by powder feeder under inert gas atmosphere
Mixed-powder is transported to behind cladding region, waits for cladding surface, cooperative mechanical hand using laser transmitting laser irradiation titanium alloy
The path set starts cladding, and titanium alloy surface is completed by the way of layer-by-layer cladding and is modified, heat preservation carries out immediately after the completion
Stress processing.
Chinese invention patent CN108557822A discloses a kind of preparation method of surface organic modification titanium carbide nanometer sheet.
Titanium carbide is prepared first with the al atomic layer in the mixed solution of lithium fluoride and hydrochloric acid etching aluminium-titanium carbonate in the method
It precipitates, is then dispersed in water titanium carbide precipitating again, ultrasound, centrifugation remove sediment, take supernatant liquor to get carbon is arrived
Change titanium nanometer sheet suspension；It is eventually adding the aqueous solution of surfactant, reaction obtains surface organic modification titanium carbide nanometer sheet.
The invention prepares titanium carbide using the al atomic layer in the mixed solution of lithium fluoride and hydrochloric acid etching aluminium-titanium carbonate, carves with hydrofluoric acid
The method of erosion aluminium-titanium carbonate is compared, and corrosivity reduces, and operational safety improves.The surface organic modification titanium carbide of invention preparation
Nanometer sheet surface-active with higher and thermal stability, it is good with the compatibility of high molecular material, it can be uniformly dispersed in macromolecule
In material, to improve the mechanical property of high molecular material, flame retardant property and hot property.
Chinese invention patent CN106633050A discloses a kind of modified titanium carbide of rodlike Polyaniline-Supported and its low temperature system
Standby method.This method is first by two-dimensional layer nano material MXene-Ti3C2It is added in tartaric acid solution, is uniformly dispersed to obtain
Ti3C2Mixed liquor；To Ti3C2Aniline is added in mixed liquor, is uniformly dispersed to obtain mixed solution；At 0~5 DEG C, into mixed solution
Catalyst is added dropwise, stirring polymerization is gradually become uniform dark solution by clear solution up to mixed solution, washs and do
It is dry, obtain the modified titanium carbide of rodlike Polyaniline-Supported.The invention prepares PANI/Ti in a low temperature of 0~5 DEG C3C2Composite material,
Reduce Ti3C2Oxidation, and reacted in organic acid soln, modified Ti3C2The functional group on surface makes PANI and Ti3C2Knot
That closes is even closer, improves the chemical property of material.
Chinese invention patent CN105861905A disclose a kind of modified by nano particles titanium carbide base hard alloy and its
Preparation method.Titanium carbide base hard alloy therein is made of the raw material of following mass percent: nano titanium carbide (TiC) 2-
8%, titanium carbide (TiC) 45-55%, tungsten carbide (WC) 15-20%, nickel (Ni) 15-20%, molybdenum (Mo) 6-10%, tungsten (W) 1-
2%, chromium carbide (Cr3C2) 1-2%, carbon dust (C) 0.5-1.5%；Preparation method are as follows: (1) preparation of mixture；(2) ball milling,
Glue, granulation are mixed in filtering, drying, obtain the mixture particle of even particle size；(3) compression moulding, vacuum-sintering, are cooled to
Room temperature is got product, and the cemented carbide material hardness of invention preparation is high, wearability, good corrosion resistance, and porosity is low and sexual valence
Than high, it can be used for the finishing of mild steel continuous cutting.
Chinese invention patent CN108103460A discloses a kind of titanium carbide target and preparation method thereof.First by pure carbonization
Titanium material powder carries out screening process, obtains even-grained powder, carries out handling with carbon later, obtains ingredient and suitably mix original
Material；Then it is uniformly filled into mold, carries out hot pressed sintering processing under vacuum conditions, after cooling, demoulding obtains sintered blank；
Finally sintered blank is machined out to obtain the titanium carbide target for meeting size and surface quality requirements.This method technique letter
List, forming effect are preferable, are conducive to industrialization large-scale production；Target is without any bonding phase constituent, and crystal grain is uniformly tiny, consistency
It can reach 99% or more, purity is 99.9% or more；The target improves in sputtering process and beats arc discharge phenomenon, the film of preparation
Layer surface defect is less, and coating is more fine and close, can be used as and prepares titanium carbide coating, improves coating mechanical property and tribology
Can, especially suitable for processing the flexible metal materials such as aluminium and aluminium alloy.
As it can be seen that existing invention is not directed to using alkali metal chloride molten salt bath progress titanium carbide granule surface modification, again
The method of structure particle surface composition and pattern, the present invention have originality.
Summary of the invention
The present invention provides a kind of surface modifying methods of titanium carbide granule, and titanium carbide is placed in alkali metal chloride fused salt
In bath, it is therefore an objective to improve the surface nature of titanium carbide, rather than prepare titanium carbide or increase on titanium carbide granule surface additional
Group.Improve particle surface pattern using the titanium ion exchange equilibrium between titanium carbide and fused salt.
A kind of surface modifying method of titanium carbide granule, it is characterised in that: with Titanium, titanium chloride, solid carbon particles
For raw material, the strong diffusion conditions and titanium elements provided in 1101 DEG C -1199 DEG C of molten salt bath by molten salt bath return in-disproportionation is special
Property, promote the titanium of Titanium and charcoal particle surface and carbon atom to deposit to titanium carbide granule surface, to reconstruct titanium carbide granule
The composition and pattern on surface.
Further, specific technical solution of the present invention is as follows:
(1) titanium carbide granule is added in the crucible for filling alkali metal chloride fused salt, titanium carbide and alkali metal chlorination
The mass ratio of object is 1:2.4~3.1.
(2) 0.02%~0.09% sodium fluoride of mass fraction, 0.08%~3.9% are added into alkali metal chloride fused salt
Titanium chloride, 0.5%~3.9% solid carbon, 0.6%~8.9% Titanium.Wherein, 0.02%, 0.09%, 0.08%,
0.5%, 0.6%, 3.9%, 8.9% the sum of all kinds of material qualities in reaction crucible are accounted for for sodium fluoride (or titanium chloride) quality
Percentage.
(3) it is warming up to mixture on the fusion temperature of alkali molten salt, keeps the temperature 30min~300min.
(4) reactants and products grain density is big, is easy to be sunken to reactor bottom.By the air pressure adjustment machine of reactor
Structure extrudes lower layer's fused salt containing reactant, separates solid product grain and liquid fused salt using porous plate later.It is cooling
Isolate titanium carbide granule from residue in a manner of eddy current separation again afterwards.
Further, the group of fused salt becomes sodium chloride or calcium chloride；Wherein, (mTi+mTiC+mTC+mc): ms=1:2.4~
3.1, mTi、mTiC、mTC、mc、msTitanium (m respectively in fused saltTi), titanium carbide (mTiC), titanium chloride (mTC), solid carbon (mc)
With fused salt (ms) quality.
Further, molten salt bath is handled using interim heating and keeping temperature rule；Wherein, liter when room temperature is to 575 DEG C
Warm rate is between 2.81 DEG C/min and 8.53 DEG C/min, and the heating rate between 575 DEG C -998 DEG C is between 1.91 DEG C/min
Between 6.25 DEG C/min, the heating rate between 999 DEG C -1198 DEG C is between 0.81 DEG C/min and 6.13 DEG C/min；It rises
Temperature needs to keep the temperature after reaching predetermined temperature, and holding temperature section is 1-2 in following sections, 1101 DEG C -1148 DEG C (heat preservations
21min~89min) and 1151 DEG C -1198 DEG C (heat preservation 30min~300min).
Further, using the molten salt bath with reproducibility as reaction media, and the reproducibility of molten salt bath is not by dissolving in
The solid carbon particles of fused salt provide；Solid carbon is (m with dosage ratioTi+mTiC+mTC+ms): mc=1:0.05~0.2；Wherein,
mTi、mTiC、mTC、ms、mcThe quality of titanium, titanium carbide, titanium chloride, fused salt and solid carbon respectively in molten salt bath.
Further, solid carbon is graphite powder or petroleum coke, and the ingredient of the selection of fused salt, holding temperature and solid carbon
It is related；The volatile matter of solid carbon between 0.001~0.01%, ash content between 0.01~0.1%, sulphur content 0.001~
0.01%, 949 DEG C -998 DEG C of holding temperature.
Further, most of liquid fused salt is filtered out from solid product using porous plate at high temperature；Fused salt is cooling
Afterwards, solid product is removed to and added water, pulp density is adjusted to 45%~65%, is melted with eddy current separation technology from after cooling
Nonconducting solid carbon and solid salt are isolated in salt；Wherein, remaining reguline metal titanium granularity is larger, is enriched on sieve plate
Layer, titanium carbide fine size leak under sieve plate, to realize the separation for participating in titanium and titanium carbide granule.
The present invention with sodium fluoride, titanium chloride, high purity graphite powder, Titanium alkali metal chloride molten salt bath in repair
Titanium carbide surface is adornd, can realize that the surface of titanium carbide granule is modified under≤1198 DEG C of medium temperature.With the difference master of the prior art
It is embodied in:
(1) raw material.Reaction environment, sodium fluoride, titanium chloride, high purity graphite powder, gold are constructed with sodium chloride (or calcium chloride)
Belonging to titanium is that raw material modifies titanium carbide surface.The spontaneous progress of entire modification, can be by state modulator critical processes.
(2) reaction environment.The modified-reaction of titanium carbide carries out in molten salt bath, and reactant ion diffusion conditions are good, product
Titanium carbide surface is smooth, and spherical coefficient is high.
Detailed description of the invention
Fig. 1 particle titanium carbide is modified process.
Specific embodiment
Following instance is not limited to application method of the invention and applicable model for illustrating implementation process of the invention
It encloses.
Example 1:
The spherical coefficient of certain commodity titanium carbide granule is about 67%.Using sodium chloride as fused salt, (mTi+mTiC+mTC+mc): ms=
1:2.4.Wherein, mTi、mTiC、mTC、mc、msTitanium respectively in fused salt, titanium carbide, titanium chloride, solid carbon and fused salt matter
Amount.Liter of the heating rate between 5.51 DEG C/min and 5.56 DEG C/min, between 575 DEG C -998 DEG C when room temperature is to 575 DEG C
Warm rate is between 3.96 DEG C/min and 3.99 DEG C/min, and the heating rate between 999 DEG C -1198 DEG C is between 2.88 DEG C/min
Between 2.91 DEG C/min；It heats up after reaching predetermined temperature in 1191 DEG C of -1198 DEG C of heat preservation 3h.Utilize porous plate will at high temperature
Most of liquid fused salt is filtered out from solid product；After fused salt is cooling, solid product is removed to and added water, pulp density is adjusted to
51%~52%, nonconducting solid carbon and solid salt are isolated from fused salt after cooling with eddy current separation technology.Wherein,
Remaining reguline metal titanium granularity is larger, is enriched on 3.5mm sieve plate, and titanium carbide is realized because fine size is sieved under sieve plate thoroughly
The separation of residual metallic titanium and titanium carbide granule.Modified titanium carbide granule spherical shape coefficient raising reaches 89.7%, significantly improves
Application performance.
Example 2:
The spherical coefficient of certain commodity titanium carbide granule is about 71%, and granularity is uneven.Using calcium chloride as fused salt, (mTi+mTiC+
mTC+mc): ms=1:2.9.Wherein, mTi、mTiC、mTC、mc、msTitanium, titanium carbide, titanium chloride, solid respectively in fused salt
The quality of charcoal and fused salt.Heating rate when room temperature is to 575 DEG C between 5.51 DEG C/min and 5.56 DEG C/min, 575 DEG C-
Heating rate of the heating rate between 3.96 DEG C/min and 3.99 DEG C/min, between 999 DEG C -1198 DEG C between 998 DEG C
Between 2.88 DEG C/min and 2.91 DEG C/min, reach after predetermined temperature in 1161 DEG C of -1168 DEG C of heat preservation 5h.It is sharp at high temperature
Most of liquid fused salt is filtered out from solid product with porous plate；After fused salt is cooling, solid product is removed to and added water, will be expected
Slurry concentration is adjusted to 51%~52%, isolates nonconducting solid carbon from fused salt after cooling with eddy current separation technology and consolidates
Body salt.Wherein, remaining reguline metal titanium granularity is larger, is enriched on 3mm sieve plate, titanium carbide is sieved to sieve plate because of fine size thoroughly
Under, realize the separation of residual metallic titanium and titanium carbide granule.Modified titanium carbide granule spherical shape coefficient raising reaches 90.11%,
Significantly improve application performance.
Example 3:
The spherical coefficient of certain commodity titanium carbide granule is about 82%, and granularity is uneven.Using calcium chloride as fused salt, (mTi+mTiC+
mTC+mc): ms=1:3.5.Wherein, mTi、mTiC、mTC、mc、msTitanium, titanium carbide, titanium chloride, solid respectively in fused salt
The quality of charcoal and fused salt.Heating rate when room temperature is to 575 DEG C between 5.22 DEG C/min and 5.23 DEG C/min, 575 DEG C-
Heating rate of the heating rate between 3.83 DEG C/min and 3.84 DEG C/min, between 999 DEG C -1198 DEG C between 998 DEG C
Between 2.66 DEG C/min and 2.68 DEG C/min, reach after predetermined temperature in 1196 DEG C of -1197 DEG C of heat preservation 4h.It is sharp at high temperature
Most of liquid fused salt is filtered out from solid product with porous plate；After fused salt is cooling, solid product is removed to and added water, will be expected
Slurry concentration is adjusted to 55%~56%, isolates nonconducting solid carbon from fused salt after cooling with eddy current separation technology and consolidates
Body salt.Wherein, remaining reguline metal titanium granularity is larger, is enriched on 3.2mm sieve plate, and titanium carbide is sieved to thoroughly because of fine size
Under plate, the separation of residual metallic titanium and titanium carbide granule is realized.Modified titanium carbide granule spherical shape coefficient raising reaches
90.11%, significantly improve application performance.
Claims (7)
1. a kind of surface modifying method of titanium carbide granule, it is characterised in that: with Titanium, unmodified titanium carbide, dichloride
Titanium, solid carbon particles are raw material, and mixture is warming up to predetermined temperature from room temperature using step-up temperature, keeping temperature rule, by molten
In the strong diffusion conditions and the returning of titanium elements that salt bath provides-disproportionation characteristic, expand the titanium on titanium carbide granule surface with ionic forms
It is scattered to fused salt, recycles ionic reaction that titanium atom, carbon atom is made to deposit to titanium carbide granule surface, reconstructs the table of titanium carbide granule
Face pattern realizes modification.
2. a kind of surface modifying method of titanium carbide granule according to claim 1, it is characterised in that: specific steps are such as
Under:
(1) titanium carbide granule is added in the crucible for filling alkali metal chloride fused salt, titanium carbide and alkali metal chloride
Mass ratio is 1:2.4~3.1；
(2) into alkali metal chloride fused salt be added 0.02%~0.09% sodium fluoride, 0.08%~3.9% titanium chloride,
0.5%~3.9% high purity graphite powder, 0.6%~8.9% Titanium；Wherein, 0.02%, 0.09%, 0.08%, 0.5%,
0.6%, 3.9%, 8.9% is sodium fluoride or titanium chloride, and quality accounts for the percentage of the sum of all kinds of material qualities in reaction crucible；
(3) it is warming up to mixture on the fusion temperature of alkali molten salt, heating needs to keep the temperature after reaching predetermined temperature, keeps the temperature
Temperature range is 1-2 in following sections, and 1101 DEG C -1148 DEG C (heat preservation 21min~89min) and 1151 DEG C -1198 DEG C (are protected
Warm 30min~300min)；
(4) reactants and products grain density is big, is easy to be sunken to reactor bottom.It, will by the Pneumatic adjusting mechanism of reactor
Lower layer's fused salt containing reactant extrudes, and separates solid product grain and liquid fused salt using porous plate later；After cooling again
Titanium carbide granule is isolated from residue in a manner of eddy current separation.
3. a kind of surface modifying method of titanium carbide granule according to claim 1, it is characterised in that (mTi+mTiC+mTC+
mc): ms=1:2.4~3.1, wherein mTi、mTiC、mTC、mc、msTitanium respectively in fused salt, titanium carbide, titanium chloride, solid carbon,
The group of the quality of fused salt, fused salt becomes sodium chloride or calcium chloride；.
4. a kind of surface modifying method of titanium carbide granule according to claim 1, it is characterised in that: using stage
Heating and keeping temperature rule handle molten salt bath；Wherein, heating rate when room temperature is to 575 DEG C between 2.81 DEG C/min and 8.53 DEG C/
Between min, the heating rate between 575 DEG C -998 DEG C is between 1.91 DEG C/min and 6.25 DEG C/min, and 999 DEG C -1198 DEG C
Between heating rate between 0.81 DEG C/min and 6.13 DEG C/min；Heating needs to keep the temperature after reaching predetermined temperature, keeps the temperature
Temperature range is 1-2 in following sections: 1101 DEG C of 21min~89min and 1151 DEG C -1198 DEG C of -1148 DEG C of heat preservations, heat preservation
30min~300min.
5. a kind of surface modifying method of titanium carbide granule according to claim 1, it is characterised in that: restored using having
Property molten salt bath as reaction media, and the reproducibility of molten salt bath is provided by the solid carbon particles insoluble in fused salt；Solid carbon
It is (m with dosage ratioTi+mTiC+mTC+mS): mc=1:0.05~0.2；Wherein, mTi、mTiC、mTC、mS、mcRespectively in fused salt
The quality of titanium, titanium carbide, titanium chloride, fused salt and solid carbon.
6. a kind of surface modifying method of titanium carbide granule according to claim 1, it is characterised in that: solid carbon is graphite
Powder or petroleum coke, and the selection of fused salt, holding temperature are related to the ingredient of solid carbon: the volatile matter of solid carbon 0.001~
Between 0.01%, sulphur content is 0.001~0.01%.1101 DEG C -1148 DEG C of holding temperature when ash content is between 0.01~0.1%；
1151 DEG C -1198 DEG C of holding temperature when ash content is between 0.001~0.01%.
7. a kind of surface modifying method of titanium carbide granule according to claim 1, it is characterised in that: utilize at high temperature
Porous plate filters out most of liquid fused salt from solid product；After fused salt is cooling, solid product is removed to and is added water, by slurry
Concentration is adjusted to 45%~65%, and nonconducting solid carbon and solid are isolated from fused salt after cooling with eddy current separation technology
Salt；Wherein, remaining reguline metal titanium granularity is larger, is enriched in sieve plate upper layer, and titanium carbide fine size leaks under sieve plate, from
And realize the separation for participating in titanium and titanium carbide granule.
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| CN1718539A (en) * | 2004-07-08 | 2006-01-11 | 武汉科技大学 | Method of preparing titanium carbide material using fused salt method |
| WO2015030388A1 (en) * | 2013-08-27 | 2015-03-05 | 주식회사 나노테크 | Method for preparing titanium carbide powder |
| CN105200458A (en) * | 2015-10-27 | 2015-12-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium carbide |
| CN105314635A (en) * | 2015-12-07 | 2016-02-10 | 武汉科技大学 | High-purity titanium carbide powder and preparation method thereof |
| US10081874B2 (en) * | 2013-09-16 | 2018-09-25 | Hongmin Zhu | Method for electrowinning titanium from titanium-containing soluble anode molten salt |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1718539A (en) * | 2004-07-08 | 2006-01-11 | 武汉科技大学 | Method of preparing titanium carbide material using fused salt method |
| WO2015030388A1 (en) * | 2013-08-27 | 2015-03-05 | 주식회사 나노테크 | Method for preparing titanium carbide powder |
| US10081874B2 (en) * | 2013-09-16 | 2018-09-25 | Hongmin Zhu | Method for electrowinning titanium from titanium-containing soluble anode molten salt |
| CN105200458A (en) * | 2015-10-27 | 2015-12-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium carbide |
| CN105314635A (en) * | 2015-12-07 | 2016-02-10 | 武汉科技大学 | High-purity titanium carbide powder and preparation method thereof |
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