CN109400171A - A method of preparing MAX phase material - Google Patents
A method of preparing MAX phase material Download PDFInfo
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- CN109400171A CN109400171A CN201811538390.2A CN201811538390A CN109400171A CN 109400171 A CN109400171 A CN 109400171A CN 201811538390 A CN201811538390 A CN 201811538390A CN 109400171 A CN109400171 A CN 109400171A
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- max phase
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- 239000000463 material Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 239000011343 solid material Substances 0.000 claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 7
- 150000003624 transition metals Chemical class 0.000 claims abstract description 5
- 238000003763 carbonization Methods 0.000 claims abstract description 3
- 239000000919 ceramic Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 4
- 238000009825 accumulation Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000000571 coke Substances 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 206010037660 Pyrexia Diseases 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000012620 biological material Substances 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 238000010348 incorporation Methods 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229920000620 organic polymer Polymers 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011295 pitch Substances 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052716 thallium Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 239000002006 petroleum coke Substances 0.000 claims 1
- 230000000087 stabilizing effect Effects 0.000 abstract description 2
- 238000010792 warming Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000001902 propagating effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910009817 Ti3SiC2 Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
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- 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
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Abstract
The present invention provides a kind of methods for preparing laminate ceramic MAX phase material, it is that transition metal source, major element source, carbon source and/or nitrogen source are mixed to form solid material, then directly solid material itself energization is made it generate heat and is gradually warming up to 900 DEG C or more in reacting furnace, carbonization and/or nitridation generate MAX phase material.It is an advantage of the invention that the thermal efficiency is high, power consumption is low, good product consistency, process stabilizing, and can be mass-produced MAX phase material.
Description
Technical field
The invention belongs to ceramic material fields, are related to the preparation method of MAX phase material.
Background technique
MAX phase material have density is low, modulus is high, good conductivity, thermal conductivity are good, thermal shock resistance is good, damage tolerance is high,
The advantages that high temperature oxidation resistance is good.Since MAX phase material has layer structure, and wherein elements A activity is relatively high, therefore
Elements A can also be removed by chemical attack and form two-dimensional layer material, may be used as electrode material, sensor component etc..?
Aerospace, nuclear industry, energy industry etc. have broad application prospects.
The preparation of MAX phase material has chemical vapour deposition technique (CVD), hot pressing sintering method, self- propagating sintering process, pulse electricity
The methods of heating, vacuum sputtering.Be easy to obscure with the present invention is pulse electrical heating method, and its essence is raw material is packed into one
In a graphite crucible, Current Heating graphite crucible is passed through to graphite crucible, then raw material is transferred heat to by graphite crucible
To complete the heating to raw material.Approach described above, batch is small, and generally laboratory prepares on a small scale.According to the inventors knowledge, mesh
Before until, have not seen process stabilizing and be suitble to the method for large scale preparation MAX phase material.
Summary of the invention
A method of preparing laminate ceramic MAX phase material, be by transition metal source, major element source, carbon source and/
Or nitrogen source is mixed to form solid material, then in reacting furnace, under protective atmosphere, solid material pass through a heating process, institute
The solid material carbonization and/or nitridation stated generate MAX phase material, it is characterised in that: the MAX phase material has Mn+1AXnIt is logical
Formula or chemical formula, M therein represents transition metal element, A represents major element, and X represents carbon and/or nitrogen, and n is positive number；
The heating process are as follows: in reacting furnace by by the current fed solid material and/or its described plus
Change resulting material (hereinafter referred to as material) in thermal process to be directly powered to material, passes through the resistance or material of material itself
Contact resistance fever and heated material between particle or block, and the maximum temperature that the material passes through is not less than 900
℃；
The reducing atmosphere pressure is lower than 2MPa.
Further, the reacting furnace is to the rotary kiln of the material direct-electrifying, the revolution kiln furnitures
There is bringing-up section, the material is accumulated in the bringing-up section of the rotary kiln forms current path；
Alternatively, the reacting furnace is to the vertical kiln of the material direct-electrifying, the vertical furnace stove has heating
Section, is provided with the positive and negative electrode of heating power supply at the both ends of the bringing-up section, which connects with the material electricity
Touching, the material are accumulated to form current path in the bringing-up section of vertical kiln.
Further, the protective atmosphere are as follows: methanol, CO, nitrogen, ammonia, hydrocarbon, other gaseous states are carbon containing
And/or one of organic matter of nitrogen perhaps their mixture or wherein incorporation be no more than 10% volume ratio oxygen；
The carbon source are as follows: carbon and the compound of element M and/or A, coal, graphite, carbon black, active carbon, coke, stone in Mn+1AXn
Oil coke, pitch, biological material, organic polymer, melamine, paraffin, sugar, in the carbonaceous material in the protective atmosphere
One or more than one kinds of mixtures；
The nitrogen source are as follows: nitrogen in the compound of element M in Mn+1AXn and/or A, the protective atmosphere nitrogen, contain
One of organic matter of nitrogen or more than one mixture；
The transition metal element are as follows: one of Sc, Ti, V, Cr, Zr, Nb, Mo, Ta, Hf or more than one；
The transition metal source is one of the simple substance containing the transition metal element, alloy or compound or one
Kind or more；
The major element are as follows: one of B, Al, Ga, In, Tl, Si, Ge, Sn, Pb, P, As, Sb, Bi, Zn, Cd or a kind of
More than；
The major element source be one of the simple substance containing the major element, alloy or compound or it is a kind of with
On.
Further, the n in the formula M n+1AXn is more than or equal to the 1, positive integer less than or equal to 20.
Further, being 10~10000 volts to the voltage of the material direct-electrifying, electric current is 10~100000
Ampere.
Further, carrying out ball milling before the solid material enters reacting furnace, rolling, mix and/or form.
Compared with the prior art, the present invention has a characteristic that
1) apply direct current or alternating voltage directly into solid material with electrode and be passed through electric current, solid material heap puts away this
Body with certain resistance (or nonconducting solid material generated after the pre- thermal response of preheating section of reacting furnace have it is certain
Electric conductivity material), which generates heat under the function of current, eliminate diabatic process of the heat from heater element to material,
It avoids to fire resisting material of furnace body and the nondistinctive heating of material, heat utilization ratio is high, and power consumption is low.And it avoids because of heat transfer
It is required that and cause the limitation of material accumulation thinner thickness, furnace cavity utilization rate improves, and the thermal efficiency improves, but also reacting furnace fills
Set can do it is smaller.
2) it due to carrying out heating reaction by the way of to the heating of raw material direct-electrifying, avoids having used Elema, silicon molybdenum
The heater elements such as stick or molybdenum filament and nickel boat or crucible.But also material is easier to be heated to reaction temperature, so that reaction
Rate is very fast, and the reaction time shortens, and product oxygen content is low, the product that product free carbon is low, available quality is high.
3) reacting furnace can be rotary kiln, further improve the heat and mass transfer process in reaction process, so that when reaction
Between it is short, the thermal efficiency is high, and uniform in quality is stablized, and material is movable continuously travelings inside reacting furnace, convenient for large-scale industry
Metaplasia produces, good product consistency.
4) it avoids chemical vapor deposition method and needs high valuable stuff, the small problem of production scale.
5) avoiding hot pressure reaction method, the device is complicated, the problem that intermittence produces and production scale is small.
6) the problem of avoiding the production of Self- propagating Sintering Synthetic method intermittence.
Specific embodiment
Illustrate specific technical solution of the invention now in conjunction with embodiment.Following embodiment only illustrates skill of the invention
Art scheme reliable and effective can be realized, but technical solution of the invention is not limited in following embodiment.
Embodiment 1
1000kg is contained into TiO2, metallic silicon, carbon black+pitch (Ti:Si:C=3:1.2:2 molar ratio) raw material mixing, add
Enter a small amount of water heating and rolling, to roll-in ball machine pressure ball molding, is fed in directly-heated type rotary kiln with the speed of 100kg per hour
(the electric heating rotary kiln disclosed using Chinese patent CN103335513A).Solid original is piled between directly-heated type rotary kiln positive and negative anodes
Material passes through the direct current or alternating current of 3500A between positive and negative anodes.Material successively passes through warming-up section (namely preheating section), returns
High temperature section (namely bringing-up section) between rotary kiln positive and negative electrode, temperature descending section discharging.Rotary kiln discharge end is passed through argon gas as protection
Atmosphere, argon flow 80Nm3/ h, reaction end gas are withdrawn from from rotary kiln feed end.Sky of the material in directly-heated type rotary kiln bringing-up section
Speed is 6h-1, 1100 ~ 1450 DEG C of bringing-up section temperature.Products obtained therefrom is through X-ray diffraction analysis, main ingredient Ti3SiC2, have no
The diffraction maximum of other compositions.
Embodiment 2
1000kg is contained into Cr3C2、γ-Al2O3, carbon black+pitch (Cr:Al:C=3:1:2 molar ratio) raw material mixing, add
Enter a small amount of water heating and rolling, to roll-in ball machine pressure ball molding, is fed in electric heating shaft kiln with the speed of 100kg per hour.Institute
The hot shaft kiln of the click stated has bringing-up section, the both ends of the bringing-up section is provided with the positive and negative electrode of heating power supply, this is just
Negative electrode and the material are in electrical contact, and the material is accumulated to form current path in the bringing-up section of vertical kiln.Positive and negative
Pass through the direct current or alternating current of 5000A between pole.Material successively passes through warming-up section (namely preheating section), shaft kiln positive and negative electrode
Between high temperature section (namely bringing-up section), temperature descending section discharging.Shaft kiln discharge end is passed through nitrogen as protective atmosphere, nitrogen flow
80Nm3/ h, reaction end gas are withdrawn from from rotary kiln feed end.Material is 8h in the air speed of shaft kiln bringing-up section-1, bringing-up section temperature is
1250~1450℃.Products obtained therefrom is through X-ray diffraction analysis, main ingredient Cr3AlCN has no the diffraction maximum of other compositions.
Claims (7)
1. a kind of method for preparing laminate ceramic MAX phase material, be by transition metal source, major element source, carbon source and/or
Nitrogen source is mixed to form solid material, then in reacting furnace, under protective atmosphere, solid material pass through a heating process, it is described
Solid material carbonization and/or nitridation generate MAX phase material, it is characterised in that:
The MAX phase material has Mn+1AXnGeneral formula or chemical formula, M therein represents transition metal element, A represents main group member
Element, X represent carbon and/or nitrogen, and n is positive number；
The heating process are as follows: in reacting furnace by by the current fed solid material and/or its described plus
Change resulting material (hereinafter referred to as material) in thermal process to be directly powered to material, passes through the resistance or material of material itself
Contact resistance fever and heated material between particle or block, and the maximum temperature that the material passes through is not less than 900
℃；
The reducing atmosphere pressure is lower than 2MPa.
2. the method according to claim 1 for preparing MAX phase material, it is characterised in that: the reacting furnace is to described
Material direct-electrifying rotary kiln, the rotary kiln have bringing-up section, heating of the material in the rotary kiln
Accumulation forms current path in section.
3. the method according to claim 1 for preparing MAX phase material, it is characterised in that: the reacting furnace is to described
Material direct-electrifying vertical kiln, the vertical furnace stove has bringing-up section, is arranged at the both ends of the bringing-up section
There is the positive and negative electrode of heating power supply, the positive and negative electrode and the material are in electrical contact, heating of the material in vertical kiln
Section accumulation forms current path.
4. the method as claimed in any of claims 1 to 3 for preparing MAX phase material, it is characterised in that: described
Protective atmosphere are as follows: methanol, CO, nitrogen, ammonia, hydrocarbon, other gaseous states be carbon containing and/or one of the organic matter of nitrogen or
Their mixture of person, or it is no more than the oxygen of 10% volume ratio in wherein incorporation；
The carbon source are as follows: carbon and Mn+1AXnThe compound of middle element M and/or A, coal, graphite, carbon black, active carbon, coke, petroleum
Coke, pitch, biological material, organic polymer, melamine, paraffin, sugar, in the carbonaceous material in the protective atmosphere
One or more than one kinds of mixtures；
The nitrogen source are as follows: nitrogen and Mn+1AXnIt is the compound of middle element M and/or A, the nitrogen in the protective atmosphere, nitrogenous
One of organic matter or more than one mixture；
The transition metal element are as follows: one of Sc, Ti, V, Cr, Zr, Nb, Mo, Ta, Hf or more than one；
The transition metal source is one of the simple substance containing the transition metal element, alloy or compound or one
Kind or more；
The major element are as follows: one of B, Al, Ga, In, Tl, Si, Ge, Sn, Pb, P, As, Sb, Bi, Zn, Cd or a kind of
More than；
The major element source be one of the simple substance containing the major element, alloy or compound or it is a kind of with
On.
5. the method as claimed in any of claims 1 to 4 for preparing MAX phase material, it is characterised in that: described is logical
N in formula Mn+1AXn is more than or equal to the 1, positive integer less than or equal to 20.
6. the method as claimed in any of claims 1 to 5 for preparing MAX phase material, it is characterised in that: to described
The voltage of material direct-electrifying is 10~10000 volts, and electric current is 10~100000 amperes.
7. the method as claimed in any of claims 1 to 6 for preparing MAX phase material, it is characterised in that: described
Solid material carries out ball milling, rolls, mixes and/or form before entering reacting furnace.
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| CN110394449A (en) * | 2019-08-27 | 2019-11-01 | 西安交通大学 | A kind of quaternary MAX phase enhances nickel-base high-temperature Oxidation Resistance Composites and its synthetic method |
| CN111725380A (en) * | 2020-06-12 | 2020-09-29 | 清华大学 | Layered high-entropy MAX-phase ceramic thermoelectric material and preparation method thereof |
| CN113564546A (en) * | 2020-04-28 | 2021-10-29 | 安泰科技股份有限公司 | Preparation method and system of precoating metal strip for metal bipolar plate |
| CN117286359A (en) * | 2023-09-27 | 2023-12-26 | 江苏美特林科特殊合金股份有限公司 | Nitride reinforced high-temperature alloy and preparation method thereof |
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| CN117286359A (en) * | 2023-09-27 | 2023-12-26 | 江苏美特林科特殊合金股份有限公司 | Nitride reinforced high-temperature alloy and preparation method thereof |
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Application publication date: 20190301 |