CN101747042A - Method for preparing Nb2AlC ceramic powders - Google Patents
Method for preparing Nb2AlC ceramic powders Download PDFInfo
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- CN101747042A CN101747042A CN200910073099A CN200910073099A CN101747042A CN 101747042 A CN101747042 A CN 101747042A CN 200910073099 A CN200910073099 A CN 200910073099A CN 200910073099 A CN200910073099 A CN 200910073099A CN 101747042 A CN101747042 A CN 101747042A
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Abstract
The invention discloses a method for preparing Nb2AlC ceramic powders, relates to a method for preparing layered ternary compound single-phase ceramic powders, and solves the problems that the existing conventional preparation method for preparing the Nb2AlC ceramic powders has long reaction time, large energy consumption, complex process and high cost, and the structure of the obtained Nb2AlC ceramic powders is coarsened. The method of the invention comprises the following steps: (1) weighing niobium powders, aluminium powders and carbon powders, and then carrying out ball-milling to obtain mixed powders; and (2) putting the mixed powders into a graphite boat, then putting the graphite boat in a reactor, filling the reactor with inert gases, lighting the fire to make a self-propagation reaction occur, and carrying out cooling, grinding, sieving and drying on the product to obtain the Nb2AlC ceramic powders. The method of the invention has the advantages of rapid reaction speed, short synthesis time, small energy consumption, low cost and high production efficiency. The obtained Nb2AlC ceramic powders have high purity. The Nb2AlC ceramic powders obtained by the method can be used for industries of aviation, aerospace, electronic industry, nuclear industry and the like.
Description
Technical field
The present invention relates to a kind of preparation method of ternary layered compound single-phase ceramic powder.
Background technology
M
N+1AX
n(M is a magnesium-yttrium-transition metal, and A is a main group element, and X is C or N, n=1-3) has lamellated hexagonal structure.From (American Ceramic Society, J.Am.Ceram.Soc.79 (1996) 1953) such as M.W.Barsoum by reaction hot-pressing technology synthesizing block Ti first
3SiC
2Since, M
N+1AX
nAttracting increasing in the world researcher with its unique characteristic.Specifically, it had both had the plurality of advantages of pottery, such as high-modulus, and high strength etc.Some performance that also has metal such as soft, can be processed, and the good conductive heat conductivility has higher damage tolerance and good thermal shock resistance.Get a good chance of being used for the novel texture/function integration material of occasions such as Aeronautics and Astronautics, electronic industry and nuclear industry.
Nb
2AlC is this class novel tertiary lamellar compound M
N+1AX
nA kind of in the pottery, its excellent high-temperature performance is subject to people's attention day by day.Though Nb
2AlC has many excellent comprehensive performances and wide potential application foreground, but Nb
2The preparation of AlC is extremely difficult, makes its related basic research and application be restricted.Ternary layered compound N b
2The AlC block mainly is to form by prepared such as hot pressing, hot isostatic pressings.As (alloy cpds, J.Alloy.Compd.347 (2002) 271) such as Barsoum with Nb, Al
4C
3With C be raw material, at 1600 ℃, hot isostatic pressing obtained high-purity Nb in 8 hours under the 100MPa
2The AlC block materials.Because with the Al in the raw material
4C
3Have water absorbability, making has a spot of Al in the product
2O
3Exist.(material news flashes, Script.Mater.57 (2007) 893) such as distribution spring is raw material with Nb, Al and C powder, and at 1600 ℃, Nb was successfully prepared in 30MPa hot pressing in 1 hour
2The single-phase block materials of AlC.This class preparation technology's common drawback is preparation temperature height (1100～1600 ℃), long reaction time (1～8 hour), is difficult to obtain the large size material, and production efficiency is low; In preparation process, need the long-time continuous heating, consumed a large amount of electric energy; Complex process needs vacuum environment or argon shield; Through heating for a long time, the microstructure coarsening of material causes its mechanical property relatively poor simultaneously.
Summary of the invention
The objective of the invention is in order to solve existing Nb
2Preparation method's long reaction time of AlC ceramic powder, big, the complex process of energy consumption, and the Nb that obtains
2The problem of AlC ceramic powder microstructure coarsening the invention provides a kind of Nb
2The preparation method of AlC ceramic powder.
A kind of Nb of the present invention
2The preparation method of AlC ceramic powder realizes by following steps: a, take by weighing niobium powder, aluminium powder and carbon dust respectively, put it in the resin ball grinder ball milling then 5～30 hours, perhaps add the wet mixing of dehydrated alcohol ball milling dry naturally after 5～30 hours mixed powder, wherein, the mol ratio of niobium powder and aluminium powder is 2: 0.7～1.3, and the mol ratio of niobium powder and carbon dust is 2: 0.6～1.2; B, mixed powder is packed in the graphite boat, graphite boat is put into the seal-off pressure container again, feed rare gas element then, keeping the pressure in the seal-off pressure container is 0.01～2MPa, and igniting makes mixed powder generation self-propagating reaction obtain loose shape Nb
2The AlC pottery, shape Nb will loosen after the cooling
2AlC pottery is pulverized, is sieved, drying obtains Nb
2The AlC ceramic powder.
The quality purity of niobium powder, aluminium powder and carbon dust in the step 1 of the present invention is more than 98%.
Add dehydrated alcohol in the step 1 of the present invention and make mixing of materials even, make the liquid level of dehydrated alcohol not have material 1～5mm as dispersion agent.
Nb of the present invention
2The preparation method of AlC ceramic powder utilizes combustion synthesis process, so that niobium powder, aluminium powder and carbon dust are that feedstock production goes out low cost, highly purified single-phase Nb cheaply
2The AlC ceramic powder; And preparation technology's cost is low, need not long-time heat, can save a large amount of energy, and energy consumption reduces; Speed of reaction is fast, and generated time is short, and production efficiency height, combustion synthesis reaction only can be finished in several minutes, and short soaking time has suppressed growing up of crystal grain, makes its synthetic Nb
2AlC has tiny crystal grain; Processing unit is simple, and floor space is little, and maintaining is convenient.
The Nb that preparation method of the present invention obtains
2The AlC ceramic powder is by single-phase Nb
2AlC forms, purity height, Nb
2The AlC ceramic powder belongs to hexagonal system, and spacer is P63/mmc, and Al and Nb-C chain cause Nb with weak covalent bonds in the crystalline structure
2AlC easily prolongs (0001) basal plane and produces shearing strain, thereby makes Nb
2AlC crystal grain is easy to produce kinking and slabbing, shows micro-plasticity on the microcosmic.
Preparation method of the present invention compares with traditional high temperature solid-state reactions method, advantage of the present invention has been to utilize the chemical energy of raw material, in reaction process, only need very little energy igniting to get final product, the required energy of combustion processes is from chemical energy that material combusting discharged, greatly reduce energy consumption, improved production efficiency; And burning synthetic temperature is very high, can reach 2000～3000 ℃, and high temperature helps the volatilization of impurity, thereby Nb
2The purity of AlC ceramic powder is very high.
In sum, the present invention adopts combustion synthesis technology to prepare Nb
2The method of AlC ceramic powder has the reaction times weak point, and speed of reaction is fast, and power consumption is few, the production efficiency height, and cost is low, and technology simply waits outstanding advantage, and the Nb that obtains
2The AlC ceramic powder is organized tiny, has a extensive future, and can be used for industries such as Aeronautics and Astronautics, electronic industry and nuclear industry, has obvious social and economic benefits.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of Nb of present embodiment
2The preparation method of AlC ceramic powder realizes by following steps: a, take by weighing niobium powder, aluminium powder and carbon dust respectively, put it in the resin ball grinder ball milling then 5～30 hours, perhaps add the wet mixing of dehydrated alcohol ball milling dry naturally after 5～30 hours mixed powder, wherein, the mol ratio of niobium powder and aluminium powder is 2: 0.7～1.3, and the mol ratio of niobium powder and carbon dust is 2: 0.6～1.2; B, mixed powder is packed in the graphite boat, graphite boat is put into the seal-off pressure container again, feed rare gas element then, keeping the pressure in the seal-off pressure container is 0.01～2MPa, and igniting makes mixed powder generation self-propagating reaction obtain loose shape Nb
2The AlC pottery, shape Nb will loosen after the cooling
2AlC pottery is pulverized, is sieved, drying obtains Nb
2The AlC ceramic powder.
Add dehydrated alcohol among the present embodiment step a and make mixing of materials even, make the liquid level of dehydrated alcohol not have material 1～5mm as dispersion agent.
The quality purity of niobium powder, aluminium powder and carbon dust among the present embodiment step a is more than 98%.
The present embodiment reaction times is short, and speed of reaction is fast, and power consumption is few, the production efficiency height, and cost is low, and technology is simple, the Nb that obtains
2The AlC ceramic powder is by single-phase Nb
2AlC forms, purity height, Nb
2The AlC ceramic powder belongs to hexagonal system, and spacer is P6
3/ mmc, Al and Nb-C chain cause Nb with weak covalent bonds in the crystalline structure
2AlC easily prolongs (0001) basal plane and produces shearing strain, thereby makes Nb
2AlC crystal grain is easy to produce kinking and slabbing, shows micro-plasticity on the macroscopic view.
Niobium powder, aluminium powder and carbon dust are the commercially available prod in the present embodiment, and three's quality purity is all more than 98%.
Embodiment two: present embodiment and embodiment one are different is that the mol ratio of niobium powder and aluminium powder is 2: 0.9～1.2 among the step a.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is that the mol ratio of niobium powder and aluminium powder is 2: 1.1 among the step a.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment and embodiment one, two or three are different is that the mol ratio of niobium powder and carbon dust is 2: 0.7～1.1 among the step a.Other step and parameter are identical with embodiment one, two or three.
Embodiment five: present embodiment and embodiment one, two or three are different is that the mol ratio of niobium powder and carbon dust is 2: 0.8 among the step a.Other step and parameter are identical with embodiment one, two or three.
Embodiment six: what present embodiment and embodiment one to five were different is that carbon dust is graphite or carbon black among the step a.Other step and parameter are identical with embodiment one to five.
The graphite and the carbon black of present embodiment are the commercially available prod.
Embodiment seven: what present embodiment and embodiment one to six were different is that rare gas element is argon gas or helium among the step b.Other step and parameter are identical with embodiment one to six.
Embodiment eight: present embodiment and embodiment one to seven are different is to keep among the step b that pressure is 0.1～1.0MPa in the seal-off pressure container.Other step and parameter are identical with embodiment one to seven.
Embodiment nine: present embodiment and embodiment one to seven are different is to keep among the step b that pressure is 0.3MPa in the seal-off pressure container.Other step and parameter are identical with embodiment one to seven.
Embodiment ten: what present embodiment and embodiment one to eight were different is that the Ni-Cr silk is adopted in igniting among the step b, and priming mixture is that mol ratio is 1: 1 titanium valve and a sooty mixture.Other step and parameter are identical with embodiment one to eight.
Titanium valve in the present embodiment in the priming mixture is that granularity is 99% titanium valve less than 300 purpose quality purities.Titanium valve and carbon black are the commercially available prod.
Embodiment 11: that present embodiment and embodiment one are different is Nb
2The preparation method of AlC ceramic powder realizes by following steps: a, take by weighing niobium powder, aluminium powder and carbon dust respectively, put it into then in the resin ball grinder, add then the wet mixing of dehydrated alcohol ball milling dry naturally after 30 hours mixed powder, wherein, the mol ratio of niobium powder and aluminium powder is 2: 1.1, and the mol ratio of niobium powder and carbon dust is 2: 0.8; B, mixed powder is packed in the graphite boat, graphite boat is put into the seal-off pressure container again, feed the rare gas element argon gas then, keeping the pressure in the seal-off pressure container is 0.3MPa, and igniting makes mixed powder generation self-propagating reaction obtain loose shape Nb
2The AlC pottery, shape Nb will loosen after the cooling
2AlC pottery is pulverized, is sieved, drying obtains Nb
2The AlC ceramic powder.
Add dehydrated alcohol in the present embodiment step 1 and make mixing of materials even, make the liquid level of dehydrated alcohol not have material 4mm as dispersion agent.
The quality purity of niobium powder, aluminium powder and carbon dust in the present embodiment step 1 is more than 98%.
The Ni-Cr silk is adopted in igniting in the present embodiment, and priming mixture is that mol ratio is 1: 1 titanium valve and a sooty mixture.
The Nb that obtains in the present embodiment
2The AlC ceramic powder is by single-phase Nb
2AlC forms, the purity height, and crystalline structure is tiny.
Embodiment 12: present embodiment Nb
2The preparation method of AlC ceramic powder realizes by following steps: a, take by weighing niobium powder, aluminium powder and carbon dust respectively, put it into then in the resin ball grinder ball milling 30 hours mixed powder, wherein, the mol ratio of niobium powder and aluminium powder is 2: 1.2, and the mol ratio of niobium powder and carbon dust is 2: 0.7; B, mixed powder is packed in the graphite boat, graphite boat is put into the seal-off pressure container again, feed the rare gas element argon gas then, keeping the pressure in the seal-off pressure container is 0.1MPa, and igniting makes mixed powder generation self-propagating reaction obtain loose shape Nb
2The AlC pottery, after the cooling with its pulverizing, sieve, drying obtains Nb
2The AlC ceramic powder.
The quality purity of niobium powder, aluminium powder and carbon dust in the present embodiment step 1 is more than 98%.
The Ni-Cr silk is adopted in igniting in the present embodiment, and priming mixture is that mol ratio is 1: 1 titanium valve and a sooty mixture.
The Nb that obtains in the present embodiment
2The AlC ceramic powder is by single-phase Nb
2AlC forms, the purity height, and crystalline phase is organized tiny.
Claims (9)
1. Nb
2The preparation method of AlC ceramic powder is characterized in that Nb
2The preparation method of AlC ceramic powder realizes by following steps: a, niobium powder, aluminium powder and carbon dust were put into resin ball grinder ball milling 5～30 hours, perhaps adding the wet mixing of dehydrated alcohol ball milling dries after 5～30 hours naturally, obtain mixed powder, wherein, the mol ratio of niobium powder and aluminium powder is 2: 0.7～1.3, and the mol ratio of niobium powder and carbon dust is 2: 0.6～1.2; B, mixed powder is packed in the graphite boat, graphite boat is put into the seal-off pressure container again, feed rare gas element then, keeping the pressure in the seal-off pressure container is 0.01～2MPa, and igniting makes mixed powder generation self-propagating reaction obtain loose shape Nb
2The AlC pottery, shape Nb will loosen after the cooling
2AlC pottery is pulverized, is sieved, drying obtains Nb
2The AlC ceramic powder.
2. a kind of Nb according to claim 1
2The preparation method of AlC ceramic powder is characterized in that the mol ratio of niobium powder and aluminium powder is 2: 0.9～1.2 among the step a.
3. a kind of Nb according to claim 1
2The preparation method of AlC ceramic powder is characterized in that the mol ratio of niobium powder and aluminium powder is 2: 1.1 among the step a.
4. a kind of Nb according to claim 1 and 2
2The preparation method of AlC ceramic powder is characterized in that the mol ratio of niobium powder and carbon dust is 2: 0.7～1.1 among the step a.
5. a kind of Nb according to claim 1 and 2
2The preparation method of AlC ceramic powder is characterized in that the mol ratio of niobium powder and carbon dust is 2: 0.8 among the step a.
6. a kind of Nb according to claim 4
2The preparation method of AlC ceramic powder is characterized in that carbon dust is graphite or carbon black among the step a.
7. according to claim 1,2 or 6 described a kind of Nb
2The preparation method of AlC ceramic powder is characterized in that rare gas element is argon gas or helium among the step b.
8. a kind of Nb according to claim 7
2The preparation method of AlC ceramic powder is characterized in that among the step b keeping that pressure is 0.1～1.0MPa in the seal-off pressure container.
9. according to claim 1,2,6 or 8 described a kind of Nb
2The preparation method of AlC ceramic powder is characterized in that the Ni-Cr silk is adopted in igniting among the step b, and priming mixture is that mol ratio is 1: 1 titanium valve and a sooty mixture.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910073099A CN101747042A (en) | 2009-10-27 | 2009-10-27 | Method for preparing Nb2AlC ceramic powders |
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|---|---|---|---|
| CN200910073099A CN101747042A (en) | 2009-10-27 | 2009-10-27 | Method for preparing Nb2AlC ceramic powders |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179418A (en) * | 2018-11-05 | 2019-01-11 | 大连理工大学 | A kind of low temperature preparation method of niobium aluminized carbon |
| CN110041075A (en) * | 2019-05-21 | 2019-07-23 | 哈尔滨师范大学 | A kind of fast preparation method of high-purity N b2SnC ceramic powder |
| CN110357103A (en) * | 2019-07-01 | 2019-10-22 | 武汉科技大学 | Niobium carbide based on aluminium carbide niobium-aluminium nitride composite granule and preparation method thereof |
-
2009
- 2009-10-27 CN CN200910073099A patent/CN101747042A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179418A (en) * | 2018-11-05 | 2019-01-11 | 大连理工大学 | A kind of low temperature preparation method of niobium aluminized carbon |
| CN110041075A (en) * | 2019-05-21 | 2019-07-23 | 哈尔滨师范大学 | A kind of fast preparation method of high-purity N b2SnC ceramic powder |
| CN110041075B (en) * | 2019-05-21 | 2021-05-28 | 哈尔滨师范大学 | Rapid preparation method of high-purity Nb2SnC ceramic powder |
| CN110357103A (en) * | 2019-07-01 | 2019-10-22 | 武汉科技大学 | Niobium carbide based on aluminium carbide niobium-aluminium nitride composite granule and preparation method thereof |
| CN110357103B (en) * | 2019-07-01 | 2022-06-14 | 武汉科技大学 | Niobium carbide-aluminum nitride composite powder based on aluminum niobium carbide and preparation method thereof |
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Application publication date: 20100623 |