CN103667846B - A kind of preparation method without phase boundary titanium carbide gradient material - Google Patents
A kind of preparation method without phase boundary titanium carbide gradient material Download PDFInfo
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- CN103667846B CN103667846B CN201310682147.9A CN201310682147A CN103667846B CN 103667846 B CN103667846 B CN 103667846B CN 201310682147 A CN201310682147 A CN 201310682147A CN 103667846 B CN103667846 B CN 103667846B
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- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000000748 compression moulding Methods 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 100
- 239000010936 titanium Substances 0.000 claims description 54
- 229910052719 titanium Inorganic materials 0.000 claims description 54
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 240000001624 Espostoa lanata Species 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 13
- 239000011229 interlayer Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000002596 correlated effect Effects 0.000 abstract 1
- 230000000875 corresponding effect Effects 0.000 abstract 1
- 238000013459 approach Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- CYKMNKXPYXUVPR-UHFFFAOYSA-N [C].[Ti] Chemical compound [C].[Ti] CYKMNKXPYXUVPR-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- -1 titanium carbides Chemical class 0.000 description 1
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Abstract
Without a preparation method for phase boundary titanium carbide gradient material, it is according to the relation of carbon content and its performance, and through getting the raw materials ready, raw material portioning, ball milling, compression moulding, the step preparation such as sintering is without phase boundary titanium carbide gradient material.Utilize the corresponding relation that the method can utilize the content of carbon in titanium carbide and exist between its physics, chemistry and mechanical property, changed the correlated performance of titanium carbide by adjustment carbon content, its performance can be designed within the specific limits needed for purposes.The titanium carbide material interlayer carbon content prepared in the process of the present invention is different, interlayer performance differs greatly, but lattice types still can be kept identical for each layer and lattice parameter is more or less the same, thus makes interlayer without obvious phase boundary, therefore overcome the drawback that common material lost efficacy in interface formation weak link.
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, have broad application prospects in fields such as aerospace, communications and transportation, mechanical workout, medicine equipments; Meanwhile, owing to having unique physics, chemical property, also Chang Zuowei electrode, field-electron emission body, catalyzer etc. are applied to optics, electronics and field of petrochemical industry for it.In long-term investigation 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 namely 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, thus makes the room occurring a large amount of carbon in titanium carbide.According to document (MaterialScienceandEngineeringA, 1988,105/106 (1): 1 – 10) report, in titanium carbide, carbon vacancy content can reach more than 50% at most, and the chemical formula that therefore titanium carbide is definite should be TiC
x(0.48≤x≤1).Although the change of carbon content can not change the lattice types of titanium carbide, can its performance of remarkably influenced (comprising physicals, chemical property).Such as, document (PhysicalReviewLetters, 2001,86 (15): 3348 – 3351) have studied carbon content in titanium carbide and, on the impact of its hardness, finds to there is mutually corresponding relation between them; Document (JournalofExperimentalandTheoreticalPhysicsLetters, 1999,4:294 – 300) reports titanium carbide resistivity also by the impact of its carbon content.Therefore, by controlling the content of carbon in titanium carbide, just can obtain there is different performance but the titanium carbide that is more or less the same of the still identical and lattice parameter of lattice types, these different titanium carbides are carried out rational composite, just can obtain performance and to change in gradient and without the titanium carbide gradient material of obvious phase boundary.This material is different with titanium carbide content, and different aspects can have different performances, but because interlayer is without obvious phase boundary, therefore overcomes common material and 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 the identical and lattice parameter of lattice types is more or less the same.
Alleged by the present invention, problem solves by the following technical programs:
Without a preparation method for phase boundary titanium carbide gradient material, special feature is: it is made up of following step:
A. raw material prepares: be ready to prepare the raw material carbonized titanium powder needed for titanium carbide gradient material and titanium valve, the titanium of carbonized titanium powder and the atomic ratio of carbon are 1:1;
B. raw material portioning mixture: by carbonized titanium powder and titanium valve by mass percentage difference be divided into several parts, the mass percent 53.57%-100.00% in each part raw material shared by carbonized titanium powder, surplus is titanium valve, is mixed by two of each part kinds of raw materials respectively;
C. ball milling: each part carbonized titanium powder and titanium valve mixed powder are placed in respectively the high energy ball mill ball milling 2-6 hour under argon shield;
D. compression moulding: by the difference of each part mixed powder according to contained titanium valve ratio, is successively routed to also compression moulding in compacting tool set;
E. sinter: the raw material block suppressed is placed in sintering oven, namely obtain required without phase boundary titanium carbide gradient material through sintering, insulation, cooling.
The above-mentioned preparation method without phase boundary titanium carbide gradient material, first raw material block is heated to 1400-1600 DEG C by described sintering step, and insulation 2-4 hour, makes carbonized titanium powder and titanium valve react; Then continue raised temperature to 1900-2100 DEG C, insulation 2-4 hour, makes reacted titanium carbide local homogenization, 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, the mass percent difference in described adjacent layers raw material shared by 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 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.Described method is with carbonized titanium powder and titanium valve for raw material, and through getting the raw materials ready, raw material portioning, ball milling, compression moulding, the step such as sintering prepare titanium carbide gradient material.Utilize the method can utilize the corresponding relation that in titanium carbide, carbon content and its performance exist, changed the room quantity of carbon in titanium carbide by adjustment carbon content, thus the titanium carbide material performance of formation can be designed within the specific limits needed for purposes.The titanium carbide material interlayer carbon content prepared in the process of the present invention is different, interlayer performance differs greatly, but lattice types still can be kept identical for each layer and lattice parameter is more or less the same, thus make interlayer without obvious phase boundary, therefore overcome common material and easily form weak link in interface and the drawback lost efficacy.
Embodiment
The inventive method comprises five steps:
(1) raw material prepares: be ready to prepare the raw material carbonized titanium powder needed for titanium carbide gradient material 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 mixture: according to material require, by carbonized titanium powder and titanium valve by mass percentage difference be divided into several parts, the mass percent in each part raw material shared by carbonized titanium powder is 53.57%-100.00%, and surplus is titanium valve, is mixed by each part raw material.Wherein, the mass percent lower limit 53.57% shared by carbonized titanium powder is the minimum value ensureing that carbonized titanium powder and titanium valve fully react, otherwise there will be unnecessary titanium in material.For making the performance of each layer of material present notable difference, the mass percent difference in adjacent layers raw material shared by carbonized titanium powder should be not less than 3%.
(3) ball milling: each part carbonized titanium powder and titanium valve mixed powder are placed in respectively the high energy ball mill ball milling 2-6 hour under argon shield;
(4) compression moulding: by the difference of each part mixed powder according to contained titanium valve ratio, be 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 vacancy content at each layer edge and middle part is different, for ensureing that the performance of layers of material fully demonstrates, layers of material should have certain thickness, and therefore after each layer raw material compacting, thickness should be not less than 0.5 millimeter.
(5) sinter: the raw material suppressed is placed in sintering oven, adopt two-step approach to sinter it: first block to be heated to 1400-1600 DEG C, insulation 2-4 hour, makes carbonized titanium powder and titanium valve react; Then continue raised temperature to 1900-2100 DEG C, insulation 2-4 hour, makes reacted titanium carbide local homogenization; Namely material after above-mentioned sintering is cooled to the furnace room temperature obtains required without phase boundary titanium carbide gradient material.
Several specific embodiment is below provided:
Embodiment 1:
1. first get out raw material: granularity between 1 micron to 5 microns, the atomic ratio of titanium and carbon is the carbonized titanium powder of 1:1, the titanium valve of granularity between 1 micron to 10 microns.
2., by by quality such as different ratios are divided into four parts of ready carbonized titanium powder and titanium valve, in each part, the mass percent of carbonized titanium powder and titanium valve is respectively: the carbonized titanium powder of first part: 53.57% and the titanium valve of 46.63%; The carbonized titanium powder of second part: 65.20% and the titanium valve of 34.80%; 3rd part: the carbonized titanium powder of 83.33% and the titanium valve of 16.67%; 4th part: the carbonized titanium powder of 100.00% and the titanium valve of 0.00%.
3. the high energy ball mill be placed in by above-mentioned mixed powder under argon shield distinguishes ball milling 2 hours.
4. be set in compacting tool set by the powder after ball milling according to contained titanium valve ratio order place Min layers from less to more, then briquetting, after compacting, each layer thickness is 2 millimeters.
5. the block suppressed is placed in sintering oven, adopts two-step approach to sinter it: first block to be heated to 1600 DEG C, to be incubated 2 hours, carbonized titanium powder and titanium valve are reacted; Continue raised temperature to 2000 DEG C, be incubated 2 hours, make reacted titanium carbide local homogenization, then namely furnace cooling obtains required gradient material.
Embodiment 2
1. first get out raw material: granularity between 1 micron to 5 microns, the atomic ratio of titanium and carbon is the carbonized titanium powder of 1:1, the titanium valve of granularity between 1 micron to 10 microns.
2., by by quality such as different ratios are divided into three parts of ready carbonized titanium powder and titanium valve, in each part, the mass percent of carbonized titanium powder and titanium valve is respectively: the carbonized titanium powder of first part: 65.20% and the titanium valve of 34.80%; The carbonized titanium powder of second part: 83.33% and the titanium valve of 16.67%; 3rd part: carbonized titanium powder is identical with second part with the ratio of titanium valve;
3. the high energy ball mill be placed in by above-mentioned mixed powder under argon shield distinguishes ball milling 4 hours.
4. the powder after ball milling is routed in development mould according to the order of second part, first part and the 3rd part, then compression moulding.After compacting, each layer thickness is 3 millimeters.
5. the raw material suppressed is placed in sintering oven, two-step approach is adopted to sinter it: first block to be heated to 1500 DEG C, be incubated 4 hours, carbonized titanium powder and titanium valve are reacted, then raised temperature to 1900 DEG C is continued, be incubated 4 hours, make reacted titanium carbide local homogenization, then namely furnace cooling obtains required gradient material.
Embodiment 3
1. first get out raw material: granularity between 1 micron to 5 microns, the atomic ratio of titanium and carbon is the carbonized titanium powder of 1:1, 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: the carbonized titanium powder of first part: 64.10%% and the titanium valve of 35.90%; The carbonized titanium powder of second part: 91.91% and the titanium valve of 8.19%; 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 the high energy ball mill ball milling under argon shield, wherein first part of raw material ball milling 3 hours, second part of ball milling 5 hours.
4. the powder order after ball milling is routed in development mould, then compression moulding.Thickness wherein after first part of raw material compacting is 1 millimeter, and second part is 4 millimeters.
5. the raw material suppressed is placed in sintering oven, two-step approach is adopted to sinter it: first block to be heated to 1600 DEG C, be incubated 3 hours, carbonized titanium powder and titanium valve are reacted, then raised temperature to 1900 DEG C is continued, be incubated 3 hours, make reacted titanium carbide local homogenization, then namely furnace cooling obtains required gradient material.
Claims (1)
1. without a preparation method for phase boundary titanium carbide gradient material, it is characterized in that: it is made up of following step:
A. raw material prepares: be ready to prepare the raw material carbonized titanium powder needed for titanium carbide gradient material and titanium valve, the titanium of carbonized titanium powder and the atomic ratio of carbon are 1:1;
B. raw material portioning mixture: by carbonized titanium powder and titanium valve by mass percentage difference be divided into several parts, the mass percent 53.57%-100.00% in each part raw material shared by carbonized titanium powder, surplus is titanium valve, is mixed by two of each part kinds of raw materials respectively;
C. ball milling: each part carbonized titanium powder and titanium valve mixed powder are placed in respectively the high energy ball mill ball milling 2-6 hour under argon shield;
D. compression moulding: by the difference of each part mixed powder according to contained titanium valve ratio, be successively routed to also compression moulding in compacting tool set, the mass percent difference in adjacent layers raw material shared by carbonized titanium powder is not less than 3%;
E. sinter: the raw material block suppressed is placed in sintering oven, namely obtain required without phase boundary titanium carbide gradient material through sintering, insulation, cooling;
First raw material block is heated to 1400-1600 DEG C by described sintering step, and insulation 2-4 hour, makes carbonized titanium powder and titanium valve react; Then continue raised temperature to 1900-2100 DEG C, insulation 2-4 hour, makes reacted titanium carbide local homogenization, cools to the block after above-mentioned sintering with the furnace room temperature;
Thickness in described compression moulding step after each part mixed powder compacting is not less than 0.5 millimeter;
Described 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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| PL422609A1 (en) * | 2017-08-22 | 2019-02-25 | Zakład Mechaniki Maszyn Bukpol Łagodziński Spółka Jawna | Burnishing element of the hydraulic burnishing tool |
| 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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| 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 |
| 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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| JPS59146918A (en) * | 1983-02-10 | 1984-08-23 | Toyo Soda Mfg Co Ltd | Production of double carbide |
| JP4593686B1 (en) * | 2010-02-26 | 2010-12-08 | 昭和電工株式会社 | Die for forging process, manufacturing method thereof, and forging method |
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| 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 |
| 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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