CN105621378A - Preparation method for TiN (1-x) Cx daltonide powder - Google Patents
Preparation method for TiN (1-x) Cx daltonide powder Download PDFInfo
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- CN105621378A CN105621378A CN201510999626.2A CN201510999626A CN105621378A CN 105621378 A CN105621378 A CN 105621378A CN 201510999626 A CN201510999626 A CN 201510999626A CN 105621378 A CN105621378 A CN 105621378A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/58007—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
- C04B35/58014—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on titanium nitrides, e.g. TiAlON
- C04B35/58021—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on titanium nitrides, e.g. TiAlON based on titanium carbonitrides
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/0828—Carbonitrides or oxycarbonitrides of metals, boron or silicon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
The invention discloses a preparation method for TiN (1-x) Cx daltonide powder and belongs to the field of inorganic functional ceramic powder metallurgy. According to the preparation method, titanium oxide and carbon are adopted as raw materials, and by means of process control through a solid-gas reaction two-stage method, at the nitridation stage: in a nitrogen atmosphere at the temperature of 1,000-1,600 DEG C, the temperature is maintained for 1-6 hours for nitridation to obtain a precursor TiN; at the carbonization stage, the temperature is raised to 1,600-2,200 DEG C in an argon atmosphere and maintained for 1-5 hours to obtain quantitative carbon-doped TiN (1-x) Cx daltonide powder; the carbon doping amount of final TiN (1-x) Cx is controlled by controlling the mixing amount of carbon, and the TiN (1-x) Cx daltonide with the precursorTiN and different carbon doping amounts is prepared. Through the method, the requirement on equipment is low, operation is easy, finally prepared TiN (1-x) Cx is low in oxygen content, and the carbon doping amount is precise and controllable.
Description
Technical field
The invention belongs to inorganic functional ceramic powder body field of metallurgy, it is specifically related to a kind of accurate quantification carbon doping and prepares the fixed preparation technology than compound powder of TiN (1-x) Cx.
Background technology
TiN(1-x)Cx(0 < x < 1) is continuous " zero dimension " ternary solid solution of TiN and TiC, for FCC type NaCl structure, inherit the excellent properties feature of TiN and TiC, the advantage such as there is high-melting-point, high strength, height is anti-corrosion, electric-conductivity heat-conductivity high, stability are strong. It is widely used in cutting members, coating and ceramic article.
TiN(1-x)CxThe preparation of powder body, because the C/N comparison final performance of powder body has important impact, so accurately control C/N ratio is preparation TiN(1-x)CxKey be also difficult point place. TiN(1-x)CxRaw powder's production technology has a lot. High-temperature synthesis, high-energy ball milling method etc. adopt the direct high temperature of TiN and TiC mixed powder or high-energy ball milling solid solution, this type of method energy consumption height, and final sosoloid uneven components. High-temperature ammonolysis method, carbothermic method etc. adopt different titanium sources and carbon source to carry out the obtained TiN of reduction reaction in a nitrogen atmosphere(1-x)Cx, this type of method reaction atmosphere is always nitrogen, does not consider nitrogen displacement carbon source and causes C/N than reducing, causes product cannot accurately determine C/N ratio. Therefore, for TiN(1-x)CxThere is not a good processing method in quantitatively mixing of middle carbon.
Summary of the invention
The present invention is intended on the basis of solid and gas carbothermic reduction reaction method, by two-stage method technology controlling and process, designs one and quantitatively mixes carbon and prepare TiN(1-x)CxProcessing method. This method is easy and simple to handle, cost is low, product purity height, carbon content can accuracy controlling.
Above-mentioned TiN(1-x)CxDetermine to be obtained by following step than compound powder:
A kind of TiN(1-x)CxThe fixed preparation method than compound powder, wherein 0 < x < 1, it is characterized in that: taking titanium oxide and carbon as raw material, by two-part solid slope technology nitrogenize section: be incubated 1��6h nitrogenize under 1000��1600 DEG C of nitrogen atmospheres and obtain presoma TiN; Carbonization section: be incubated the TiN that 1��5h obtains quantitative carbon doping under being warming up to 1600��2200 DEG C of argon gas atmosphere(1-x)CxDetermine compare compound powder; Final TiN is controlled by controlling the mixed volume of carbon(1-x)CxCarbon doping amount, x is adjustable from 0 to 1.
Further, concrete steps are as follows:
(1) nitrogenize section: furnace chamber is carried out pre-treatment, ensures that in stove, oxygen partial pressure is less than 10-2Pa, by carbon and TiO2Mixed powder is placed in plumbago crucible; Leading to into flowing nitrogen, be warming up to 1000��1600 DEG C with the heat-up rate of 10��20 DEG C/min, insulation 1��6h carries out nitriding treatment;
(2) carbonization section: stop nitrogen gas supply, lead to into flowing argon gas, be warming up to 1600��2200 DEG C with 5��15 DEG C/min heat-up rate, insulation 1��5h carries out carbonizing treatment.
Further, step (1) mixed powder carbon used is graphite or carbon black.
Further, increasing with carbon amounts in step (2), holding temperature increases.
More specifically:
(1) TiO of certain mass ratio is taken2And toner body, it being placed in alloy ball grinding jar, add alcohol and sintered carbide ball, ball milling 1��2h carries out mixed powder. By ball milling disposed slurry drying and screening.
(2) the powder body handled well in (1) is placed in plumbago crucible, puts into reaction atmosphere stove. Being vacuumized by reaction atmosphere stove, vacuum tightness is less than 10-1Lead to into nitrogen after Pa, again vacuumize after normal pressure to lead to and carry out washing gas disposal into nitrogen, ensure that in furnace chamber, oxygen partial pressure is less than 10-2Pa��
(3) leading to into flowing nitrogen, be warming up to 1000��1600 DEG C with the heat-up rate of 10��20 DEG C/min, insulation 1��6h carries out nitriding treatment.
(4) stopping nitrogen gas supply, lead to into flowing argon gas, be warming up to 1600��2200 DEG C with 5��15 DEG C/min heat-up rate, insulation 1��5h carries out carbonizing treatment.
(5) adjust temperature control program, make furnace chamber furnace cooling, take out sample after being down to room temperature, do subsequent disposal.
TiN can be accurately controlled by solid slope technology two-stage method(1-x)CxMiddle C/N ratio, can be used for TiN(1-x)CxThe comprehensive adjustment of stupalith strength and toughness, prepares the functional structure pottery of high-toughness high-strength.
With conventional Ti N(1-x)CxPreparation method compares, and this method adopts two-stage method control: low temperature nitrogenize section carbon participates in reduction and obtains cryostatic stabilization phase TiN; High temperature mix carbon section carbon serve as doped source mix TiN lattice formed continuous solid solution.
With conventional Ti N(1-x)CxPreparation method compares, and this method adopts two-stage method control: low-temperature zone nitrogen participates in nitrogenizing reaction as nitrogenous source and forms pure phase TiN, and high temperature section switches to argon gas shielded and effectively prevents high temperature section N/C phase double replacement and temperature descending section from stablizing the generation of phase TiN.
With conventional Ti N(1-x)CxPreparation method compares, this method by two-stage method control, by TiN(1-x)CxThe preparation of TiN and the quantitative carbon doping of TiN are resolved in preparation. Avoid nitrogenous source non-quantitation problem, eliminate nitrogenous source to the impact of product C/N ratio. TiN(1-x)CxMiddle C/N can pass through raw material TiO than preparation surely2Carry out accuracy controlling with the mass ratio of carbon, obtain the TiN of different C/N ratio according to demand(1-x)Cx��
Accompanying drawing explanation
Fig. 1 prepares TiN for quantitatively mixing carbon(1-x)CxProcess diagram
Fig. 2 is the Gibbs free energy of TiN and TiC at low temperature high temperature
Fig. 3 is that TiN mixes carbon reaction Gibbs free energy
Fig. 4 is for preparing TiN(1-x)CxThe XRD of powder body
Fig. 5 is for preparing TiN(1-x)CxRelation between the lattice parameter of powder body and carbon content
Fig. 6 is for preparing TiN(1-x)CxThe SEM of powder body, wherein (a) TiN0.9C0.1; (b) TiN0.6C0.4; (c) TiN0.4C0.6; (d) TiN0.1C0.9
Fig. 7 is for preparing TiN(1-x)CxThe size distribution of powder body, wherein (a) TiN0.9C0.1; (b) TiN0.1C0.9
Embodiment
Below in conjunction with example, summary of the invention is made detail:
Example 1 (TiN0.9C0.1Preparation):
(1) 6gTiO is taken2With 1.89g carbon black powder, powder body being placed in alloy ball grinding jar, add alcohol and sintered carbide ball, ball milling 1h carries out mixed powder. By ball milling disposed slurry drying and screening.
(2) the powder body handled well in (1) is placed in plumbago crucible, puts into reaction atmosphere stove. Being vacuumized by reaction atmosphere stove, vacuum tightness is less than 10-1Lead to into nitrogen after Pa, again vacuumize after normal pressure to lead to and carry out washing gas disposal into nitrogen so that furnace chamber oxygen partial pressure is 0.2 �� 10-2Pa��
(3) leading to the nitrogen into flowing, be warming up to 1000 DEG C with the heat-up rate of 10 DEG C/min, insulation 6h carries out nitriding treatment.
(4) stopping nitrogen gas supply, lead to into flowing argon gas, be warming up to 1600 DEG C with 5 DEG C/min heat-up rate, insulation 5h carries out carbonizing treatment.
(5), after furnace cooling is cooled to room temperature, powder ball milling drying and screening will be produced, carry out XRD, SEM and particle size analysis. The TiN prepared can be found out0.9C0.1Thing be pure phase mutually, TiO2It is changed into TiN completely, and C mixes in TiN lattice completely. Product TiN0.9C0.1Peak position relatively TiN occur moving to left, lattice parameter increase. Final SEM and particle size analysis display product powder granule are at about 1 ��m.
Example 2 (TiN0.6C0.4Preparation):
(1) 6gTiO is taken2With 2.16g carbon black powder, powder body being placed in alloy ball grinding jar, add alcohol and sintered carbide ball, ball milling 1h carries out mixed powder. By ball milling disposed slurry drying and screening.
(2) the powder body handled well in (1) is placed in earthenware pot, puts into reaction atmosphere stove. Being vacuumized by reaction atmosphere stove, vacuum tightness is less than 10-1Lead to into nitrogen after Pa, again vacuumize after normal pressure to lead to and carry out washing gas disposal into nitrogen so that furnace chamber oxygen partial pressure is 0.2 �� 10-2Pa��
(3) leading to the nitrogen into flowing, be warming up to 1200 DEG C with the heat-up rate of 15 DEG C/min, insulation 4h carries out nitriding treatment.
(4) stopping nitrogen gas supply, lead to into flowing argon gas, continue subsequently to be warming up to 1800 DEG C with 10 DEG C/min heat-up rate, insulation 4h carries out carbonizing treatment.
(5), after furnace cooling is cooled to room temperature, powder ball milling drying and screening will be produced, carry out XRD, SEM and particle size analysis. The TiN prepared can be found out0.6C0.4Thing be pure phase mutually, TiO2It is changed into TiN completely, and C mixes in TiN lattice completely. Product TiN0.6C0.4Peak position is TiN relatively0.9C0.1Appearance moves to left, and lattice parameter increases thereupon. Final SEM and particle size analysis display product powder granule are at about 1 ��m.
Example 3 (TiN0.4C0.6Preparation):
(1) 6gTiO is taken2With 2.34g carbon black powder, powder body being placed in alloy ball grinding jar, add alcohol and sintered carbide ball, ball milling 1h carries out mixed powder. By ball milling disposed slurry drying and screening.
(2) the powder body handled well in (1) is placed in plumbago crucible, puts into reaction atmosphere stove. Being vacuumized by reaction atmosphere stove, vacuum tightness is less than 10-1Lead to into nitrogen after Pa, again vacuumize after normal pressure to lead to and carry out washing gas disposal into nitrogen so that furnace chamber oxygen partial pressure is 0.2 �� 10-2Pa��
(3) leading to the nitrogen into flowing, be warming up to 1400 DEG C with the heat-up rate of 15 DEG C/min, insulation 2h carries out nitriding treatment.
(4) stopping nitrogen gas supply, lead to into flowing argon gas, be warming up to 1900 DEG C with 10 DEG C/min heat-up rate subsequently, insulation 3h carries out carbonizing treatment.
(5), after furnace cooling is cooled to room temperature, powder ball milling drying and screening will be produced, carry out XRD, SEM and particle size analysis. The TiN prepared can be found out0.4C0.6Thing be pure phase mutually, TiO2It is changed into TiN completely, and C mixes in TiN lattice completely. Product TiN0.4C0.6Peak position is TiN relatively0.6C0.4Appearance moves to left, and lattice parameter increases further. Final SEM and particle size analysis display product powder granule are at about 1 ��m.
Example 4 (TiN0.1C0.9Preparation):
(1) 6gTiO is taken2With 2.61g carbon black powder, powder body being placed in alloy ball grinding jar, add alcohol and sintered carbide ball, ball milling 1h carries out mixed powder. By ball milling disposed slurry drying and screening.
(2) the powder body handled well in (1) is placed in earthenware pot, puts into reaction atmosphere stove. Being vacuumized by reaction atmosphere stove, vacuum tightness is less than 10-1Lead to into nitrogen after Pa, again vacuumize after normal pressure to lead to and carry out washing gas disposal into nitrogen so that furnace chamber oxygen partial pressure is 0.2 �� 10-2Pa��
(3) leading to the nitrogen into flowing, be warming up to 1600 DEG C with the heat-up rate of 20 DEG C/min, insulation 1h carries out nitriding treatment.
(4) stopping nitrogen gas supply, lead to into flowing argon gas, continue subsequently to be warming up to 2200 DEG C with 15 DEG C/min heat-up rate, insulation 1h carries out carbonizing treatment.
(5), after furnace cooling is cooled to room temperature, powder ball milling drying and screening will be produced, carry out XRD, SEM and particle size analysis. The TiN prepared can be found out0.1C0.9Thing be pure phase mutually, TiO2It is changed into TiN completely, and C mixes in TiN lattice completely. Product TiN0.1C0.9Peak position is TiN relatively0.4C0.6Appearance moves to left, and lattice parameter increases. Final SEM and particle size analysis display product powder granule are at about 1 ��m.
Claims (4)
1. a TiN(1-x)CxThe fixed preparation method than compound powder, wherein 0 < x < 1, it is characterized in that: taking titanium oxide and carbon as raw material, by two-part solid slope technology nitrogenize section: be incubated 1��6h nitrogenize under 1000��1600 DEG C of nitrogen atmospheres and obtain presoma TiN; Carbonization section: be incubated the TiN that 1��5h obtains quantitative carbon doping under being warming up to 1600��2200 DEG C of argon gas atmosphere(1-x)CxDetermine compare compound powder; Final TiN is controlled by controlling the mixed volume of carbon(1-x)CxCarbon doping amount, x is adjustable from 0 to 1.
2. TiN according to claim 1(1-x)CxThe fixed preparation method than compound powder, it is characterised in that concrete steps are as follows:
(1) nitrogenize section: furnace chamber is carried out pre-treatment, ensures that in stove, oxygen partial pressure is less than 10-2Pa, by carbon and TiO2Mixed powder is placed in plumbago crucible; Leading to into flowing nitrogen, be warming up to 1000��1600 DEG C with the heat-up rate of 10��20 DEG C/min, insulation 1��6h carries out nitriding treatment;
(2) carbonization section: stop nitrogen gas supply, lead to into flowing argon gas, be warming up to 1600��2200 DEG C with 5��15 DEG C/min heat-up rate, insulation 1��5h carries out carbonizing treatment.
3. according to the method described in claim 2, it is characterised in that: step (1) mixed powder carbon used is graphite or carbon black.
4. according to the method described in claim 2, it is characterised in that: increasing with carbon amounts in step (2), holding temperature increases.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107034433A (en) * | 2017-05-05 | 2017-08-11 | 四川理工学院 | A kind of preparation method of TiCN gradient coatings |
| CN112357896A (en) * | 2020-11-23 | 2021-02-12 | 株洲昊坤硬质材料有限公司 | Preparation method and device of superfine titanium carbonitride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107034433A (en) * | 2017-05-05 | 2017-08-11 | 四川理工学院 | A kind of preparation method of TiCN gradient coatings |
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| CN112357896A (en) * | 2020-11-23 | 2021-02-12 | 株洲昊坤硬质材料有限公司 | Preparation method and device of superfine titanium carbonitride |
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