CN106882965A - A kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two - Google Patents
A kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two Download PDFInfo
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- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/404—Refractory metals
Abstract
The invention discloses a kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two, the method is comprised the following steps：1) TiC: Ti: Al=(0.6~1.2) in molar ratio: (0.9~1.5): (1~1.5) weighs raw material TiC powder, Ti powder, Al powder；2) the mixed powder machine of raw material is obtained into mixed powder；3) mixed powder is placed in sintering furnace, 1200~1600 DEG C is heated under atmosphere or vacuum protection, kept for 30~180 minutes afterwards, the aluminium toner body material of titanium two is obtained after cooling.The method raw material is easy to get, and proportioning is simple, device therefor and preparation process is simple, and the synthesis aluminium toner body time of titanium two is short, and purity is high, without the aluminium carbon (Ti of titanium three3AlC2) and the presence of TiC dephasigns, it is adapted to large-scale production and application.
Description
Technical field
The present invention relates to a kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two, belong to metallic-ceramic powder material
Material preparation field.
Background technology
In recent years, a kind of novel tertiary lamellar compound, (M represents transition metal to MAX phases；A represents major element；X
Represent carbon or nitrogen), receive the extensive concern of whole world scientific worker.It had both had metalloid excellent conduction, heat conduction
And processing characteristics, and with high-melting-point, high thermal stability, the good decay resistance and antioxygenic property of similar ceramics.Titanium
Two aluminium carbon (Ti2AlC) it is prototypical member in the phase of MAX families 211, is found in the eighties of last century sixties (W.Jeitschko
Deng .J.Less-Common Met., 1963,7 (2), 133-138).It has relatively low density (4.11g/cm3), relatively low is aobvious
Microhardness (4.5GPa), electrical conductivity (0.36 μ Ω m) higher, thermal conductivity (8.2 × 10 higher-6·K-1), poplar higher
Family name's modulus (277GPa) and modulus of shearing (144GPa) (.Int.Mater.Rev. such as Z.M.Sun, 2011,56 (3), 143-
166).These premium properties make MAX turn into a kind of very potential material, future can be widely applied for the energy, electronics and
The application fields such as machinery, thus prepare high-purity the aluminium carbon dust of titanium two tool be of great significance.
In recent decades, most research work is concentrated mainly on the preparation of the aluminium toner body of titanium two and block materials.
Be encapsulated in vitreosil pipe for TiC, Ti, Al and C powder by W.Jeitschko et al., after electric arc melting 1200 DEG C anneal 170~
500h prepares the aluminium toner body of titanium two (.Monatash such as W.Jeitschko Chem., 1963,94 (2), 672-677).
Be positioned in alumina crucible for TiC, Ti, Al and C powder by H.Nowotny et al., under nitrogen atmosphere protection, 1530 DEG C of temperature sintering
20h obtains the aluminium toner body of titanium two (the .J.Solid State such as H.Nowotny Chem., 1980,32,213-219).Both the above
Method complex process, it is time-consuming long, only synthesize on a small scale as laboratory research.Document report researcher utilizes hot pressing
Or high temperature insostatic pressing (HIP) (HIP) sintering technology prepares the aluminium carbon of titanium two (HP).With TiC, Ti, Al are raw material to B.C.Mei et al., using HP
It is sintered in 1400 DEG C and has obtained the aluminium carbon block of titanium two, but contains Ti in product3AlC2Dephasign (B.C.Mei etc.
.Mater.Sci.Tech-Lond., 2005,13 (4), 361-364).J.F.Zhu et al. by Ti, after Al, C raw material high-energy ball milling,
The aluminium carbon block of titanium two (.Mat.Sci.Eng.A, 2008,490 (1-2), 62-65 such as J.F.Zhu) is synthesized using HP sintering.
M.W.Barsoum et al. is with Ti, C and Al4C3Powder is raw material, the hot pressing 30h at hot pressing 4h or 300 DEG C at 40MPa, 1600 DEG C,
Synthesized purity up to more than 96wt.% the aluminium carbon block of titanium two (.Pro.Solid.Sta.Chem. such as M.W.Barsoum, 2000,
28,201-206).Y.C.Zhou et al. is raw material with Ti, Al and C powder, and the hot pressing 1h at 30MPa, 1400 DEG C has synthesized titanium two
Aluminium carbon block (.Z.Metallkd. such as Y.C.Zhou, 2002,93 (1), 66-67).J.F.Zhu et al. first will with mechanical alloying
Ti, Al, the C sphere of powder wear into TiAl, TiC and containing a small amount of Ti, the mixed powder of Al, then titanium two is prepared in hot pressing in vacuum or atmosphere
Aluminium carbon block (the patents such as J.F.Zhu, 2006, CN1958514A).C.G.Bo et al. with TiAl, TiC as raw material, in Vacuum Heat
Pressure or isostatic pressed under the conditions of prepare high purity 99wt.% the aluminium carbon block of titanium two (the patents such as C.G.Bo, 2016,
CN106032323A).But need to grind to form fine powder, complex process, and hot pressing with the aluminium toner body of titanium two prepared by HP or HIP
Equipment cost is too high, limits its large-scale production and applies.Additionally, C.G.Bo et al. is TiH2, the raw material such as Al and TiC with have
Machine solvent prepares spherical raw material after ultrasonic drilling machine dispersion using spray drying process granulation, and finally sintering is obtained in a vacuum
The aluminium carbon block of titanium two, the aluminium carbon spherical powder of POROUS TITANIUM two is obtained by grinding and screening, but finds exist greatly in thing phase result
The Ti of amount3AlC2And Al2O3Dephasign, and preparation technology is excessively numerous and diverse, high cost, it is difficult to application (the patents such as C.G.Bo,
2016, CN201610218497.3).Also researcher prepares the aluminium carbon of titanium two using spark plasma sintering technology (SPS).
B.C.Mei et al. is raw material with Ti, Al, C powder, and being incubated 1h by SPS at 30MPa, 1100 DEG C obtains the purer aluminium carbon of titanium two
Block, relative density is up to 99.8% (.Mater.Lett. such as B.C.Mei, 2005,59 (1), 131-134).J.F.Zhang etc.
People sinters 10~15min and obtains principal phase for the aluminium carbon block of titanium two with Ti powder, Al powder and carbon dust as raw material, using SPS, after grinding
To the aluminium toner body of titanium two, but in last thing phase result find have dephasign presence (the patents such as J.F.Zhang, 2016,
CN201610060019.4).Using CVD technology, the growth in situ on TiAl powder goes out the mixed of TiAl-CNTs to R.Shrinivas et al.
Compound, finally using SPS technologies prepare the single-phase aluminium carbon block of titanium two (.J.Alloy.Compd. such as R.Shrinivas,
2010,490 (1-2), 155-159).F.Yang et al. ball milling Ti and Al powder obtains TiAl, then TiAl powder is mixed with graphite powder
1100 DEG C of SPS sintering obtain the aluminium carbon block of titanium two (the patents such as F.Yang, 2011, CN102139370A) afterwards.SPS prepares titanium two
Though aluminium carbon block heat has the advantages that speed is fast, sample consistency is high, finally block needs plenty of time grind into powder,
And high cost, complex process and it is difficult to industrialization.In recent years, combustion method is that self- propagating (SHS) technology is widely used in preparing
The aluminium carbon of titanium two.With Ti, Al, C powder are raw material to J.M.Guo et al., and burning is prepared for the aluminium toner body of titanium two, but containing few in product
The Ti of amount3AlC2With TiC dephasigns (.Acta.Metall.Sin. such as J.M.Guo, 2003,39 (3), 315-319).C.L.Yeh etc.
People adds TiC and Al in Ti, Al, C raw material4C3, SHS technologies are recycled successfully by the aluminium carbon purity of titanium in product two from 85wt.%
Bring up to 90wt.% (.J.Alloy.Compd., 2009,470 (1-2), 424-428 such as C.L.Yeh).B.C.Mei et al. with
Ti, TiC, Al and C powder are lighted as raw material in microwave agglomerating furnace, prepare the tiny aluminium toner body of titanium two of crystal grain
(the patents such as B.C.Mei, 2007, CN101037201A).With Ti, Al, C powder are raw material, Ti, and C powder conducts to J.M.Guo et al.
Detonator, reactant is lighted with resistance wire, obtains the aluminium toner body of titanium two (the patents such as J.M.Guo, 2009, CN101531531A).
Although combustion synthesis method can directly prepare the aluminium toner body of titanium two, product purity is relatively low, often containing substantial amounts of
Ti3AlC2With the dephasign such as TiC, and complex process, its popularization and application in actual production is limited.Z.W.Liu et al. will mix
Uniform Ti, is put into stove after Al, C powder cold moudling and is heated to 700~800 DEG C or so, the use of power is 1~1.5kW ultrasounds
Auxiliary thermal explosion sintering obtains the aluminium carbon block of titanium two, but product thing phase result shows many TiC and Ti3AlC2Dephasign is remained
(the patents such as Z.W.Liu, 2015, CN201510743014.7).Y.Liu et al. similarly leads to Ti, Al and TiC powder as raw material
Cross thermal expousure and prepare the aluminium carbon block of titanium two, through the aluminium toner body of titanium two that overpickling acquisition is purer, but the method after grinding
Apparatus expensive, process are complicated, product still exist through overpickling a large amount of TiC dephasigns (the patents such as Y.Liu, 2015,
CN201510658890.X)。
Therefore, from the angle of industrialized production, it is impossible to use the high cost works such as HP, HIP, SPS, SHS and thermal explosion
The complicated agglomerating plant of skill, it should use normal pressure-sintered technology, the purity aluminium carbon of titanium two higher is produced in the short period of time
Powder, reduces production cost, improves efficiency.
The content of the invention
Technical problem：Mesh of the invention is to provide a kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two, the party
Method is with low cost, process is simple and easy industrialization, and the aluminium toner body purity of titanium two of preparation is high.The method changes traditional more multiple
Miscellaneous preparation technology, directly using TiC, the mode of Ti, Al powder mixing, with normal pressure-sintered technical substitution expensive vacuum, hot pressing, heat
The sintering technologies such as isostatic pressed, self- propagating, microwave and SPS, the aluminium of high purity titanium two of synthesis of high purity in the range of 1200~1600 DEG C
Toner body, solves that process present in existing technology of preparing is complicated, and preparation time is long, apparatus expensive and product purity is low asks
Topic.
Technical scheme：The invention provides a kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two, the method bag
Include following steps：
1) TiC: Ti: Al=(0.6~1.2) in molar ratio: (0.9~1.5): (1~1.5) weighs raw material TiC powder, Ti
Powder, Al powder；
2) by step 1) in the raw material that obtains mix 5~25 hours in mixed powder machine, well mixed obtains mixed powder；
3) by step 2) mixed powder that obtains is placed in sintering furnace, it is heated to 1200 under atmosphere or vacuum protection~
1600 DEG C, kept for 30~180 minutes afterwards, the aluminium toner body material of titanium two of high-purity is obtained after cooling.
Wherein：
Step 3) described in protective atmosphere be Ar gas.
Step 3) described in sintering furnace be ordinary sinter stove, the heating rate for being heated to 1200~1600 DEG C be 4
~12 DEG C/min.
Beneficial effect：The present invention compared with prior art, with advantages below：
1) TiC is directly used, Ti, Al powder are used as initial feed, and all raw materials are simple and easy to get.
2) process is simple, directly mixes initial feed, it is not necessary to be molded by high-energy mechanical ball milling and cold pressing etc.
Process, production efficiency is high, cost-effective.
3) at ambient pressure in ordinary sinter stove, under atmosphere or vacuum protection, in 1200~1600 DEG C of scope short time directly
The synthesis aluminium carbon of high purity titanium two, equipment is simple, with low cost, is adapted to large-scale production.
4) product purity is high, without obvious TiC and Ti in XRD spectrum3AlC2Exist etc. impurities phase.
5) the aluminium carbon dust of high purity titanium two that the technology is prepared has typical lamellar structure.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the normal pressure-sintered aluminium carbon of titanium two prepared of the present invention；
Fig. 2 is ESEM (SEM) picture of the normal pressure-sintered aluminium carbon of titanium two prepared of the present invention.
Specific embodiment
The present invention is described in detail with reference to example：
Embodiment 1：
According to TiC: Ti: Al=0.6: 0.9: 1 molar ratio ingredient, weigh 10.3 grams of TiC powder, 12.3 grams of Ti powder, Al powder
7.7 grams, it is put into plastic bottle, with ZrO2Ball is medium, and 5h is mixed on mixed powder machine, and mixed powder is put into common tubular type
In stove, Ar atmosphere or vacuum protection are warming up to 1200 DEG C with the heating rate of 4 DEG C/min, are incubated 30min, can system after cooling
The aluminium toner body of high-purity titanium two.
Embodiment 2：
According to TiC: Ti: Al=0.6: 0.9: 1.5 molar ratio ingredient, weigh 10.3 grams of TiC powder, 12.3 grams of Ti powder, Al
11.6 grams of powder, is put into plastic bottle, with ZrO2Ball is medium, and 6h is mixed on mixed powder machine, and mixed powder is put into commonly
In tube furnace, Ar atmosphere or vacuum protection are warming up to 1250 DEG C with the heating rate of 5 DEG C/min, are incubated 40min, after cooling i.e.
The aluminium toner body of high-purity titanium two that can be made.
Embodiment 3：
According to TiC: Ti: Al=0.6: 1.5: 1 molar ratio ingredient, weigh 10.3 grams of TiC powder, 20.5 grams of Ti powder, Al powder
7.7 grams, it is put into plastic bottle, with ZrO2Ball is medium, and 7h is mixed on mixed powder machine, and mixed powder is put into common tubular type
In stove, Ar atmosphere or vacuum protection are warming up to 1300 DEG C with the heating rate of 6 DEG C/min, are incubated 50min, can system after cooling
The aluminium toner body of high-purity titanium two.
Embodiment 4：
According to TiC: Ti: Al=0.6: 1.5: 1.5 molar ratio ingredient, weigh 10.3 grams of TiC powder, 20.5 grams of Ti powder, Al
11.6 grams of powder, is put into plastic bottle, with ZrO2Ball is medium, and 8h is mixed on mixed powder machine, and mixed powder is put into commonly
In tube furnace, Ar atmosphere or vacuum protection are warming up to 1320 DEG C with the heating rate of 7 DEG C/min, are incubated 55min, after cooling i.e.
The aluminium toner body of high-purity titanium two that can be made.
Embodiment 5：
According to TiC: Ti: Al=0.8: 1.1: 1.1 molar ratio ingredient, weigh 13.6 grams of TiC powder, 15.1 grams of Ti powder, Al
8.5 grams of powder, is put into plastic bottle, with ZrO2Ball is medium, and 12h is mixed on mixed powder machine, and mixed powder is put into commonly
In tube furnace, Ar atmosphere or vacuum protection are warming up to 1350 DEG C with the heating rate of 8 DEG C/min, are incubated 60min, after cooling i.e.
The aluminium toner body of high-purity titanium two that can be made.
Embodiment 6：
According to TiC: Ti: Al=1.0: 1.3: 1.3 molar ratio ingredient, weigh 17.1 grams of TiC powder, 17.8 grams of Ti powder, Al
10.0 grams of powder, is put into plastic bottle, with ZrO2Ball is medium, and 18h is mixed on mixed powder machine, and mixed powder is put into commonly
In tube furnace, Ar atmosphere or vacuum protection are warming up to 1450 DEG C with the heating rate of 10 DEG C/min, 120min are incubated, after cooling
The aluminium toner body of high-purity titanium two that can be made.
Embodiment 7：
According to TiC: Ti: Al=1.2: 1.5: 1.5 molar ratio ingredient, weigh 20.5 grams of TiC powder, 20.5 grams of Ti powder, Al
11.6 grams of powder, is put into plastic bottle, with ZrO2Ball is medium, and 25h is mixed on mixed powder machine, and mixed powder is put into commonly
In tube furnace, Ar atmosphere or vacuum protection are warming up to 1600 DEG C with the heating rate of 12 DEG C/min, 180min are incubated, after cooling
The aluminium toner body of high-purity titanium two that can be made.
Embodiment 8：
According to TiC: Ti: Al=1.2: 1.5: 1 molar ratio ingredient, weigh 20.5 grams of TiC powder, 20.5 grams of Ti powder, Al powder
7.7 grams, it is put into plastic bottle, with ZrO2Ball is medium, and 20h is mixed on mixed powder machine, and mixed powder is put into common tube
In formula stove, Ar atmosphere or vacuum protection are warming up to 1550 DEG C with the heating rate of 11 DEG C/min, are incubated 160min, after cooling i.e.
The aluminium toner body of high-purity titanium two that can be made.
Embodiment 9：
According to TiC: Ti: Al=1.2: 0.9: 1.5 molar ratio ingredient, weigh 20.5 grams of TiC powder, 12.3 grams of Ti powder, Al
11.6 grams of powder, is put into plastic bottle, with ZrO2Ball is medium, and 16h is mixed on mixed powder machine, and mixed powder is put into commonly
In tube furnace, Ar atmosphere or vacuum protection are warming up to 1500 DEG C with the heating rate of 11 DEG C/min, 140min are incubated, after cooling
The aluminium toner body of high-purity titanium two that can be made.
The XRD spectrum of the prepared aluminium toner body of titanium two is as shown in Figure 1.As seen from the figure, product purity is high, in XRD results
It is middle without obvious Ti3AlC2Exist with TiC dephasigns.The pattern of the aluminium toner body of titanium two as shown in Fig. 2 as seen from the figure, the aluminium carbon particle of titanium two
Typical lamellar structure is presented, particle size is in 10 μ ms.
Claims (3)
1. a kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two, it is characterised in that：The method is comprised the following steps：
1) TiC: Ti: A1=(0.6~1.2) in molar ratio: (0.9~1.5): (1~1.5) weighs raw material TiC powder, Ti powder, Al
Powder；
2) by step 1) in the raw material that weighs mix 5~25 hours in mixed powder machine, obtain well mixed mixed powder；
3) by step 2) mixed powder that obtains is placed in sintering furnace, and 1200~1600 are heated under atmosphere or vacuum protection
DEG C, kept for 30~180 minutes afterwards, the aluminium toner body material of high purity titanium two is obtained after cooling.
2. a kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two according to claim 1, it is characterised in that：Step
3) protective atmosphere described in is Ar gas.
3. a kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two according to claim 1, it is characterised in that：Step
3) sintering furnace described in is ordinary sinter stove, and the heating rate for being heated to 1200~1600 DEG C is 4~12 DEG C/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957175A (en) * | 2017-03-17 | 2017-07-18 | 东南大学 | A kind of method that normal pressure prepares the aluminium toner body material of high purity titanium two |
| CN108059461A (en) * | 2017-12-06 | 2018-05-22 | 东南大学 | A kind of method that pressureless sintering prepares high-compactness Ti3AlC2 blocks |
| CN109231988A (en) * | 2018-11-01 | 2019-01-18 | 燕山大学 | A kind of non-metering specific activity Ti in big vacancy3AlC2The preparation method of ceramic material |
| CN110872121A (en) * | 2018-08-29 | 2020-03-10 | 中国科学院上海硅酸盐研究所 | Nb-shaped alloy4AlC3Method for preparing ceramic powder |
| CN111116211A (en) * | 2019-12-27 | 2020-05-08 | 中铭瓷(苏州)纳米粉体技术有限公司 | Preparation method of ternary nano lamellar MAX phase powder and product thereof |
| CN113044842A (en) * | 2021-01-12 | 2021-06-29 | 辽宁中色新材科技有限公司 | Production process of high-purity aluminum titanium carbide |
| CN115650729A (en) * | 2022-11-04 | 2023-01-31 | 烟台大学 | Di-titanium-vanadium-aluminum-carbon ceramic powder material and preparation method and application thereof |
| CN116768629A (en) * | 2023-07-03 | 2023-09-19 | 辽宁中色新材科技有限公司 | Process for producing high-purity aluminum titanium carbide by low-cost one-step method |
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| CN108059461A (en) * | 2017-12-06 | 2018-05-22 | 东南大学 | A kind of method that pressureless sintering prepares high-compactness Ti3AlC2 blocks |
| CN110872121A (en) * | 2018-08-29 | 2020-03-10 | 中国科学院上海硅酸盐研究所 | Nb-shaped alloy4AlC3Method for preparing ceramic powder |
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| CN109231988B (en) * | 2018-11-01 | 2020-09-22 | 燕山大学 | Large-vacancy non-metered specific activity Ti3AlC2Method for preparing ceramic material |
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| CN113044842A (en) * | 2021-01-12 | 2021-06-29 | 辽宁中色新材科技有限公司 | Production process of high-purity aluminum titanium carbide |
| CN113044842B (en) * | 2021-01-12 | 2022-05-17 | 辽宁中色新材科技有限公司 | Production process of high-purity aluminum titanium carbide |
| CN115650729A (en) * | 2022-11-04 | 2023-01-31 | 烟台大学 | Di-titanium-vanadium-aluminum-carbon ceramic powder material and preparation method and application thereof |
| CN115650729B (en) * | 2022-11-04 | 2023-05-12 | 烟台大学 | Dititanium vanadium aluminum carbon ceramic powder material and preparation method and application thereof |
| CN116768629A (en) * | 2023-07-03 | 2023-09-19 | 辽宁中色新材科技有限公司 | Process for producing high-purity aluminum titanium carbide by low-cost one-step method |
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