CN103667846A - Preparation method of phase-boundary-free titanium carbide gradient material - Google Patents
Preparation method of phase-boundary-free titanium carbide gradient material Download PDFInfo
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- CN103667846A CN103667846A CN201310682147.9A CN201310682147A CN103667846A CN 103667846 A CN103667846 A CN 103667846A CN 201310682147 A CN201310682147 A CN 201310682147A CN 103667846 A CN103667846 A CN 103667846A
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Abstract
The invention discloses a preparation method of a phase-boundary-free titanium carbide gradient material. The phase-boundary-free titanium carbide gradient material is prepared by the steps of preparing raw materials, mixing the raw materials, performing ball-milling, performing compression molding, sintering and the like according to a relationship between the carbon content and the performance of titanium carbide. According to the method, the related performance of titanium carbide can be changed by adjusting the carbon content according to the congruent relationship between the carbon content and the physical, chemical and mechanical performance of titanium carbide, so that the performance of the titanium carbide material can be designed in a certain range according to the application need. According to the titanium carbide material prepared by the method, the interlayer carbon contents are different and the interlayer performance difference is larger but all layers still can keep the same crystal lattice types and the crystal lattice constant difference is not large, so that no obvious phase boundary exists between the layers and the disadvantage of failure of a general material caused by formation of weak links at the boundary is overcome.
Description
Technical field
The present invention relates to a kind of alloy material preparation method, particularly, without the preparation method of phase boundary titanium carbide gradient material, belong to technical field of alloy material.
Background technology
Titanium carbide has the features such as high-melting-point, high rigidity, high elastic coefficient, good high-temperature oxidation resistance and biocompatibility, be widely used in preparing ceramic base and metal-base composites, in fields such as aerospace, communications and transportation, mechanical workout, medicine equipments, have broad application prospects; Meanwhile, owing to having unique physics, chemical property, also Chang Zuowei electrode, an electron emitter, catalyzer etc. are applied to optics, electronics and field of petrochemical industry for it.In long-term research and application process, it is found that, titanium carbide has unique feature on crystalline structure.Titanium carbide has NaCl type crystal structure, and titanium is positioned at the position of cubical summit and the center of area, and carbon potential is in octahedral interstice position, and its desirable titanium carbon atomic ratio is 1:1, and the desirable chemical formula of titanium carbide is TiC.But in the titanium carbide of actual preparation, the content of carbon often can not reach perfect condition, thereby makes to occur in titanium carbide the room of a large amount of carbon.According to document (Material Science and Engineering A, 1988,105/106 (1): 1 – 10) report, in titanium carbide, carbon room content can reach more than 50% at most, so the definite chemical formula of titanium carbide should be TiC
x(0.48≤x≤1).Although the variation of carbon content can not change the lattice types of titanium carbide, can its performance of remarkably influenced (comprising physicals, chemical property).For example, document (Physical Review Letters, 2001,86 (15): 3348 – 3351) has been studied the impact of carbon content on its hardness in titanium carbide, finds to exist between them the relation of mutual correspondence; Document (Journal of Experimental and Theoretical Physics Letters, 1999,4:294 – 300) has reported that titanium carbide resistivity is also subject to the impact of its carbon content.Therefore, by controlling the content of carbon in titanium carbide, just can obtain thering is different performance but the lattice types titanium carbide that still identical and lattice parameter is more or less the same, these different titanium carbides are carried out to rational composite, just can obtain that performance changes in gradient and without the obvious titanium carbide gradient material of phase boundary.This material is different with titanium carbide content, in different aspects, can have different performances, but because interlayer is without obvious phase boundary, has therefore overcome that common material easily forms weak link in interface and the drawback that lost efficacy.
Summary of the invention
The object of the invention is to utilize the feature that in titanium carbide, carbon content can change in a big way, provide that a kind of interlayer carbon content is different, performance is different, but the preparation method without phase boundary titanium carbide gradient material that lattice types is identical and lattice parameter is more or less the same.
The alleged problem of the present invention solves by the following technical programs:
Without a preparation method for phase boundary titanium carbide gradient material, special feature is: it is comprised of following step:
A. raw material is prepared: be ready to prepare titanium carbide gradient material required raw material carbonized titanium powder and titanium valve, the titanium of carbonized titanium powder and the atomic ratio of carbon are 1:1;
B. raw material portioning is mixed: by carbonized titanium powder and titanium valve by mass percentage difference be divided into several parts, the shared mass percent 53.57%-100.00% of carbonized titanium powder in each part of raw material, surplus is titanium valve, respectively two kinds of raw materials of each part is mixed;
C. ball milling: each part of carbonized titanium powder and titanium valve mixed powder are placed in respectively to the high energy ball mill ball milling 2-6 hour under argon shield;
D. compression moulding: each part of mixed powder, according to the difference of contained titanium valve ratio, is successively routed in compacting tool set and compression moulding;
E. sintering: the raw material block suppressing is placed in to sintering oven, through sintering, insulation, cooling obtain required without phase boundary titanium carbide gradient material.
The above-mentioned preparation method without phase boundary titanium carbide gradient material, first described sintering step is heated to 1400-1600 ℃ by raw material block, and insulation 2-4 hour, makes carbonized titanium powder react with titanium valve; Then continue rising temperature to 1900-2100 ℃, insulation 2-4 hour, makes reacted titanium carbide local uniform, cools to the block after above-mentioned sintering with the furnace room temperature.
The above-mentioned preparation method without phase boundary titanium carbide gradient material, in described adjacent layers raw material, the shared mass percent difference of carbonized titanium powder is not less than 3%.
The above-mentioned preparation method without phase boundary titanium carbide gradient material, the thickness in described compression moulding step after each part of mixed powder compacting is not less than 0.5 millimeter.
The above-mentioned preparation method without phase boundary titanium carbide gradient material, described raw material carbonized titanium powder granularity is between 1 micron to 5 microns, and raw material titanium valve granularity is between 1 micron to 10 microns.
The present invention utilizes the feature that in titanium carbide, carbon content can change in a big way, according to the relation of carbon content and its performance, provides a kind of preparation method without phase boundary titanium carbide gradient material.It is raw material that described method be take carbonized titanium powder and titanium valve, through getting the raw materials ready, the step such as raw material portioning, ball milling, compression moulding, sintering prepares titanium carbide gradient material.Utilize the method can utilize the corresponding relation that in titanium carbide, carbon content and its performance exist, by adjusting carbon content, change the room quantity of carbon in titanium carbide, thereby make the titanium carbide material property forming can be according to the required design within the specific limits of purposes.Between the titanium carbide material layer of preparing with the inventive method, carbon content is different, interlayer performance differs greatly, but each layer still can keep the identical and lattice parameter of lattice types to be more or less the same, therefore thereby make interlayer without obvious phase boundary, overcome that common material easily forms weak link in interface and the drawback that lost efficacy.
Embodiment
The inventive method comprises five steps:
(1) raw material is prepared: be ready to prepare titanium carbide gradient material required raw material carbonized titanium powder and titanium valve, wherein raw material carbonized titanium powder granularity between 1 micron to 5 microns, the atomic ratio of titanium and carbon is 1:1, raw material titanium valve granularity is between 1 micron to 10 microns.
(2) raw material portioning is mixed: according to material require, by carbonized titanium powder and titanium valve by mass percentage difference be divided into several parts, in each part of raw material, the shared mass percent of carbonized titanium powder is 53.57%-100.00%, surplus is titanium valve, and each part of raw material mixed.Wherein, the shared mass percent lower limit 53.57% of carbonized titanium powder is the minimum value that guarantees that carbonized titanium powder fully reacts with titanium valve, otherwise in material, there will be unnecessary titanium.For making the performance of each layer of material present notable difference, in adjacent layers raw material, the shared mass percent difference of carbonized titanium powder should be not less than 3%.
(3) ball milling: each part of carbonized titanium powder and titanium valve mixed powder are placed in respectively to the high energy ball mill ball milling 2-6 hour under argon shield;
(4) compression moulding: each part of mixed powder, according to the difference of contained titanium valve ratio, is successively routed to compression moulding in mould.Consider in high-temperature sintering process, material adjacent layers intersection can produce a small amount of atomic diffusion, the carbon room content at each layer of edge and middle part is different, for guaranteeing that the performance of layers of material fully demonstrates, layers of material should have certain thickness, so after each layer of raw material compacting, thickness should be not less than 0.5 millimeter.
(5) sintering: the raw material suppressing is placed in to sintering oven, adopts two-step approach to carry out sintering to it: first block is heated to 1400-1600 ℃, insulation 2-4 hour, makes carbonized titanium powder react with titanium valve; Then continue rising temperature to 1900-2100 ℃, insulation 2-4 hour, makes reacted titanium carbide local uniform; Cooling to the material after above-mentioned sintering with the furnace room temperature obtains required without phase boundary titanium carbide gradient material.
Several specific embodiments are below provided:
Embodiment 1:
1. be first ready to raw material: granularity between 1 micron to 5 microns, the atomic ratio of titanium and carbon be 1:1 carbonized titanium powder, the titanium valve of granularity between 1 micron to 10 microns.
By ready carbonized titanium powder and titanium valve by four parts of the quality such as different ratios is divided into, in each part, the mass percent of carbonized titanium powder and titanium valve is respectively: first part: 53.57% carbonized titanium powder and 46.63% titanium valve; Second part: 65.20% carbonized titanium powder and 34.80% titanium valve; The 3rd part: 83.33% carbonized titanium powder and 16.67% titanium valve; The 4th part: 100.00% carbonized titanium powder and 0.00% titanium valve.
3. the high energy ball mill above-mentioned mixed powder being placed under argon shield is distinguished ball milling 2 hours.
4. the powder after ball milling is set in compacting tool set according to contained titanium valve ratio order place Min layers from less to more, then briquetting, suppresses rear each layer thickness and is 2 millimeters.
5. the block suppressing is placed in to sintering oven, adopts two-step approach to carry out sintering to it: first block to be heated to 1600 ℃, to be incubated 2 hours, carbonized titanium powder is reacted with titanium valve; Continue rising temperature to 2000 ℃, be incubated 2 hours, make reacted titanium carbide local uniform, then furnace cooling obtains required gradient material.
Embodiment 2
1. be first ready to raw material: granularity between 1 micron to 5 microns, the atomic ratio of titanium and carbon be 1:1 carbonized titanium powder, the titanium valve of granularity between 1 micron to 10 microns.
By ready carbonized titanium powder and titanium valve by three parts of the quality such as different ratios is divided into, in each part, the mass percent of carbonized titanium powder and titanium valve is respectively: first part: 65.20% carbonized titanium powder and 34.80% titanium valve; Second part: 83.33% carbonized titanium powder and 16.67% titanium valve; The 3rd part: the ratio of carbonized titanium powder and titanium valve and second part identical;
3. the high energy ball mill above-mentioned mixed powder being placed under argon shield is distinguished ball milling 4 hours.
4. the powder after ball milling is routed in development mould to then compression moulding according to the order of second part, first part and the 3rd part.After compacting, each layer thickness is 3 millimeters.
5. the raw material suppressing is placed in to sintering oven, adopt two-step approach to carry out sintering to it: first block to be heated to 1500 ℃, be incubated 4 hours, carbonized titanium powder is reacted with titanium valve, then continue rising temperature to 1900 ℃, be incubated 4 hours, make reacted titanium carbide local uniform, then furnace cooling obtains required gradient material.
Embodiment 3
1. be first ready to raw material: granularity between 1 micron to 5 microns, the atomic ratio of titanium and carbon be 1:1 carbonized titanium powder, the titanium valve of granularity between 1 micron to 10 microns.
2. ready carbonized titanium powder and titanium valve are divided into two parts by different ratios, in each part, the mass percent of carbonized titanium powder and titanium valve is respectively: first part: 64.10%% carbonized titanium powder and 35.90% titanium valve; Second part: 91.91% carbonized titanium powder and 8.19% titanium valve; Wherein the quality of second part of raw material is 4 times of first part of raw material.
3. above-mentioned mixed powder is placed in to the high energy ball mill ball milling under argon shield, wherein first part of raw material ball milling is 3 hours, second part of ball milling 5 hours.
4. the powder after ball milling is sequentially routed in development mould to then compression moulding.Wherein the thickness after first part of raw material compacting is 1 millimeter, and second part is 4 millimeters.
5. the raw material suppressing is placed in to sintering oven, adopt two-step approach to carry out sintering to it: first block to be heated to 1600 ℃, be incubated 3 hours, carbonized titanium powder is reacted with titanium valve, then continue rising temperature to 1900 ℃, be incubated 3 hours, make reacted titanium carbide local uniform, then furnace cooling obtains required gradient material.
Claims (5)
1. without a preparation method for phase boundary titanium carbide gradient material, it is characterized in that: it is comprised of following step:
A. raw material is prepared: be ready to prepare titanium carbide gradient material required raw material carbonized titanium powder and titanium valve, the titanium of carbonized titanium powder and the atomic ratio of carbon are 1:1;
B. raw material portioning is mixed: by carbonized titanium powder and titanium valve by mass percentage difference be divided into several parts, the shared mass percent 53.57%-100.00% of carbonized titanium powder in each part of raw material, surplus is titanium valve, respectively two kinds of raw materials of each part is mixed;
C. ball milling: each part of carbonized titanium powder and titanium valve mixed powder are placed in respectively to the high energy ball mill ball milling 2-6 hour under argon shield;
D. compression moulding: each part of mixed powder, according to the difference of contained titanium valve ratio, is successively routed in compacting tool set and compression moulding;
E. sintering: the raw material block suppressing is placed in to sintering oven, through sintering, insulation, cooling obtain required without phase boundary titanium carbide gradient material.
2. the preparation method without phase boundary titanium carbide gradient material according to claim 1, is characterized in that: first described sintering step is heated to 1400-1600 ℃ by raw material block, and insulation 2-4 hour, makes carbonized titanium powder react with titanium valve; Then continue rising temperature to 1900-2100 ℃, insulation 2-4 hour, makes reacted titanium carbide local uniform, cools to the block after above-mentioned sintering with the furnace room temperature.
3. the preparation method without phase boundary titanium carbide gradient material according to claim 2, is characterized in that: in described adjacent layers raw material, the shared mass percent difference of carbonized titanium powder is not less than 3%.
4. the preparation method without phase boundary titanium carbide gradient material according to claim 3, is characterized in that: the thickness in described compression moulding step after each part of mixed powder compacting is not less than 0.5 millimeter.
5. the preparation method without phase boundary titanium carbide gradient material according to claim 4, is characterized in that: described raw material carbonized titanium powder granularity is between 1 micron to 5 microns, and raw material titanium valve granularity is between 1 micron to 10 microns.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242571A (en) * | 2016-08-29 | 2016-12-21 | 华北电力大学（保定） | A kind of preparation method of titanium carbide hydrogen storage material |
| PL422609A1 (en) * | 2017-08-22 | 2019-02-25 | Zakład Mechaniki Maszyn Bukpol Łagodziński Spółka Jawna | Burnishing element of the hydraulic burnishing tool |
| CN111875383A (en) * | 2020-08-13 | 2020-11-03 | 华北电力大学（保定） | Non-stoichiometric titanium carbide hydrogen storage material and preparation method thereof |
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| JPS59146918A (en) * | 1983-02-10 | 1984-08-23 | Toyo Soda Mfg Co Ltd | Production of double carbide |
| CN101565790A (en) * | 2009-06-03 | 2009-10-28 | 南京航空航天大学 | Gradient structure carbon nano-tube enhanced Ti(C, N)-based metal ceramic and preparation method thereof |
| JP2011177716A (en) * | 2010-02-26 | 2011-09-15 | Showa Denko Kk | Forging die, method for manufacturing the same, and forging method |
| CN102796933A (en) * | 2012-09-04 | 2012-11-28 | 四川大学 | High-entropy alloy binder phase-based nitrogen-containing hard alloy and preparation method thereof |
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2013
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59146918A (en) * | 1983-02-10 | 1984-08-23 | Toyo Soda Mfg Co Ltd | Production of double carbide |
| CN101565790A (en) * | 2009-06-03 | 2009-10-28 | 南京航空航天大学 | Gradient structure carbon nano-tube enhanced Ti(C, N)-based metal ceramic and preparation method thereof |
| JP2011177716A (en) * | 2010-02-26 | 2011-09-15 | Showa Denko Kk | Forging die, method for manufacturing the same, and forging method |
| CN102796933A (en) * | 2012-09-04 | 2012-11-28 | 四川大学 | High-entropy alloy binder phase-based nitrogen-containing hard alloy and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242571A (en) * | 2016-08-29 | 2016-12-21 | 华北电力大学（保定） | A kind of preparation method of titanium carbide hydrogen storage material |
| PL422609A1 (en) * | 2017-08-22 | 2019-02-25 | Zakład Mechaniki Maszyn Bukpol Łagodziński Spółka Jawna | Burnishing element of the hydraulic burnishing tool |
| CN111875383A (en) * | 2020-08-13 | 2020-11-03 | 华北电力大学（保定） | Non-stoichiometric titanium carbide hydrogen storage material and preparation method thereof |
| CN111875383B (en) * | 2020-08-13 | 2022-04-15 | 华北电力大学（保定） | Non-stoichiometric titanium carbide hydrogen storage material and preparation method thereof |
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