CN101747048A - Preparation method of Nb2AlC blocky ceramic - Google Patents
Preparation method of Nb2AlC blocky ceramic Download PDFInfo
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Abstract
The invention relates to a preparation method of Nb2AlC blocky ceramic, which relates to a preparation method of ternary lamellar compound single-phase blocky ceramic. The invention solves the problems of high synthesis temperature, long reaction time, complex process, high cost, low production efficiency and rough texture of the obtained Nb2AlC blocky ceramic of the tradition preparation method of Nb2AlC blocky ceramic. The preparation method comprises the steps of: 1, ball-milling and mixing niobium powder, aluminum powder and carbon powder; 2, preparing a preform, then putting the preform and a die into a combustion synthesis reactor, igniting for combustion synthetic reaction; and 3, applying pressure after the combustion reaction is ended, then embedding quartz sand for cooling to obtain the Nb2AlC blocky ceramic. The method has high reaction speed, short synthesis time, low cost, high production efficiency and high purity of the obtained Nb2AlC blocky ceramic. The obtained Nb2AlC blocky ceramic of the invention can be used for the industries of aviation, aerospace, electronic industry, nuclear industry and the like.
Description
Technical field
The present invention relates to the preparation method of ternary layered compound single-phase block ceramic.
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 (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 synthesis temperature height of AlC block ceramic, long reaction time, complex process, with high costs, production efficiency is low, and the Nb that obtains
2The problem of AlC block ceramic microstructure coarsening the invention provides Nb
2The preparation method of AlC block ceramic.
Nb of the present invention
2The preparation method of AlC block ceramic realizes by following steps: one, 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, get 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; Two, apply pressure 10～20s of 15～45MPa to mixed powder, mixed powder is pressed into precast billet, then precast billet is put into mould, fill with quartz sand in space between mould and the precast billet, again mould and precast billet are put into the combustion synthesis reaction device together, in the upper surface centerfire of precast billet, the self-propagating combustion reaction takes place then; Three, begin to apply the pressure of 160～480MPa behind combustion reactions end 1～5s, pressurize 10～15s imbeds quartz sand with reaction product again and is cooled to room temperature, promptly obtains Nb
2The AlC block ceramic.
Nb of the present invention
2The preparation method of AlC block ceramic is characterized in that Nb
2The preparation method of AlC block ceramic realizes by following steps: one, 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, get 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; Two, mixed powder is put into steel die, apply pressure 20～25s of 15～45MPa, make mixed powder form a columniform base substrate, then at the upper surface central point of base substrate, perhaps place priming mixture and resistance wire on three of upper surface radius mid points that are hexagonal angle mutually, place a husky cake then on base substrate, placing thickness on husky cake is the steel cushion block of 30mm, and the resistance wire lead-in wire is drawn from the cushion block edge and with on portfire is connected; Three, open ignition device and make the resistance wire heating power precast billet of igniting, combustion reactions stops behind 1～5s immediately base substrate is applied the axle pressure 10～50 seconds of 2000kN～5000kN, takes out product, imbeds the quartz sand cooling in 30 seconds, cooled off 20～30 hours, and promptly obtained Nb
2The AlC block ceramic; The steel die of step 2 is that China Patent No. is the steel die in the patent " combustion synthesis reaction device " of ZL03132642.0.
The quality purity of niobium powder of the present invention, aluminium powder and carbon dust 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 as dispersion agent.
Nb of the present invention
2The preparation method of AlC block ceramic utilizes burning to synthesize/quasi-iso static pressing original position synthesis technique, so that niobium powder, aluminium powder and carbon dust are that feedstock production goes out highly purified single-phase Nb cheaply
2The AlC ceramic block; One step of synthetic and densification of block ceramic finishes, and preparation technology's cost is low, need not long-time heat, can save a large amount of energy, and energy consumption reduces; The production efficiency height, combustion synthesis reaction can be finished in 5 minutes, the Nb that obtains
2The AlC block ceramic is organized tiny, and compactness improves; Can obtain the Nb of diameter 50mm, 80～300mm
2The AlC block ceramic.
The Nb that preparation method of the present invention obtains
2The AlC block ceramic is by single-phase Nb
2AlC forms, purity height, Nb
2The AlC block ceramic 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.Can be used for industries such as Aeronautics and Astronautics, electronic industry and nuclear industry.
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 chemical reaction, 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 block ceramic is very high.
In sum, the present invention adopts combustion synthesis technology to prepare Nb
2The method of AlC block ceramic 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 block ceramic is organized tiny, has a extensive future, and the use of this technology will have 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: present embodiment Nb
2The preparation method of AlC block ceramic realizes by following steps: one, niobium powder, aluminium powder and carbon dust were put into resin ball grinder ball milling 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; Two, apply pressure 12～20s of 15～45MPa to mixed powder, mixed powder is pressed into precast billet, then precast billet is put into mould, fill with quartz sand in space between mould and the precast billet, again mould and precast billet are put into the combustion synthesis reaction device together, in the upper surface centerfire of precast billet, carry out the self-propagating combustion reaction then; Three, begin to apply the pressure of 160～480MPa behind combustion reactions end 1～5s, pressurize 10～15s imbeds quartz sand with reaction product again and is cooled to room temperature, promptly obtains Nb
2The AlC block ceramic.
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 1～5mm as dispersion agent.
The quality purity of niobium powder, aluminium powder and carbon dust in the present embodiment step 1 is more than 98%.
Present embodiment utilization burning is synthesized/quasi-iso static pressing original position synthesis technique, so that niobium powder, aluminium powder and carbon dust are that feedstock production goes out highly purified single-phase Nb cheaply
2The AlC ceramic block; One step of synthetic and densification of block ceramic finishes, and preparation technology's cost is low, need not long-time heat, can save a large amount of energy, and energy consumption reduces; The production efficiency height, combustion synthesis reaction can be finished in 5 minutes, the Nb that obtains
2The AlC block ceramic is organized tiny, and compactness improves; The Nb that present embodiment obtains
2The diameter of AlC block ceramic is 50mm.
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 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.7～1.1.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 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.8.Other step and parameter are identical with embodiment one.
Embodiment four: what present embodiment and embodiment one, two or three were different is to put into resin ball grinder ball milling in the step 1 12～24 hours, perhaps adds dehydrated alcohol ball milling wet mixing 12～24 hours.Other step and parameter are identical with embodiment one, two or three.
Embodiment five: what present embodiment and embodiment one, two or three were different is to put into resin ball grinder ball milling in the step 1 16 hours, perhaps adds dehydrated alcohol ball milling wet mixing 16 hours.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 the pressure that applies 25～38MPa in the step 2 to mixed powder.Other step and parameter are identical with embodiment one to five.
Embodiment seven: what present embodiment and embodiment one to five were different is the pressure that applies 32MPa in the step 2 to mixed powder.Other step and parameter are identical with embodiment one to five.
Embodiment eight: what present embodiment and embodiment one to seven were different is the priming mixture that igniting need be placed 3～7g at firing point in the step 2, and priming mixture is that Ti and C are that 1: 1 blended mixed powder, Ti and B are 1: 2 blended mixed powder or Ti and B in molar ratio in molar ratio
4C is 3: 1 blended mixed powders in molar ratio.
In the present embodiment, Ti is that granularity is 99% Ti powder less than 300 purpose quality purities.
Embodiment nine: present embodiment and embodiment one to eight are different is that mould in the step 2 is the " TiC-TiB that delivers 2003 the 4th phases " Journal of Inorganic Materials "
2The self propagating high temperature study on the synthesis of/Cu matrix material " in mould.Other step and parameter are identical with embodiment one to eight.
Embodiment ten: what present embodiment and embodiment one to nine were different is the pressure that combustion synthesis reaction finishes after-applied 240～380MPa in the step 3, pressurize 11～14s.Other step and parameter are identical with embodiment one to nine.
Embodiment 11: what present embodiment and embodiment one to nine were different is the pressure that combustion synthesis reaction finishes after-applied 280～340MPa in the step 3, pressurize 12～13s.Other step and parameter are identical with embodiment one to nine.
Embodiment 12: what present embodiment and embodiment one to nine were different is the pressure that combustion synthesis reaction finishes after-applied 300MPa in the step 3, pressurize 12s.Other step and parameter are identical with embodiment one to nine.
Embodiment 13: the difference of present embodiment and embodiment one is: the mould in the step 2 is " TiC-TiB
2The self propagating high temperature study on the synthesis of/Cu matrix material " in mould.Other step and parameter are identical with embodiment one.
Embodiment 15: present embodiment Nb
2The preparation method of AlC block ceramic realizes by following steps: one, niobium powder, aluminium powder and carbon dust are put into the resin ball grinder, adding the wet mixing of dehydrated alcohol ball milling then dries after 24 hours naturally, get 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; Two, apply the pressure 20s of 32MPa to mixed powder, mixed powder is pressed into precast billet, then precast billet is put into mould, fill with quartz sand in space between mould and the precast billet, again mould and precast billet are put into the combustion synthesis reaction device together, in the upper surface centerfire of precast billet, carry out combustion reactions then; Three, begin to apply the pressure of 300MPa behind the combustion synthesis reaction end 5s, pressurize 12s imbeds quartz sand with reaction product again and is cooled to room temperature, promptly obtains Nb
2The AlC block ceramic.
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 5mm as dispersion agent.
The quality purity of niobium powder, aluminium powder and carbon dust in the present embodiment step 1 is more than 98%.
Light a fire in the step 2 in the present embodiment and need place the priming mixture of 5g at firing point, priming mixture is that Ti and C are 1: 1 blended mixed powder in molar ratio; Mould in the step 2 is " TiC-TiB
2The self propagating high temperature study on the synthesis of/Cu matrix material " in mould.
The Nb that present embodiment obtains
2The diameter of AlC block ceramic is that 50mm, height are 10～20mm.
The Nb that present embodiment obtains
2The AlC block ceramic is by single-phase Nb
2AlC forms, and the purity height has good micro-plasticity, and mechanical property is good.
Embodiment 16: what present embodiment and embodiment 15 were different is in the step 1 niobium powder, aluminium powder and carbon dust to be put into resin ball grinder ball milling 24 hours, get 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.Other step and parameter are identical with embodiment 15.
The quality purity of niobium powder, aluminium powder and carbon dust in the present embodiment step 1 is more than 98%.
Light a fire in the step 2 in the present embodiment and need place the priming mixture of 5g at firing point, priming mixture is that Ti and C are 1: 1 blended mixed powder in molar ratio; Mould in the step 2 is " TiC-TiB
2The self propagating high temperature study on the synthesis of/Cu matrix material " in mould.
The Nb that present embodiment obtains
2The diameter of AlC block ceramic is 50mm, and height is 10～20mm.
The Nb that present embodiment obtains
2The AlC block ceramic is by single-phase Nb
2AlC forms, and the purity height has good micro-plasticity, and mechanical property is good.
Embodiment 17: present embodiment Nb
2The preparation method of AlC block ceramic realizes by following steps: one, niobium powder, aluminium powder and carbon dust were put into resin ball grinder ball milling 30 hours, get 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; Two, mixed powder is put into steel die, apply pressure 20～25s of 15～45MPa to steel die, make mixed powder form a columniform base substrate, then at the upper surface central point of base substrate, perhaps place priming mixture and resistance wire on three of upper surface radius mid points that are hexagonal angle mutually, place a husky cake then on base substrate, placing thickness on husky cake is the steel cushion block of 30mm, and the resistance wire lead-in wire is drawn from the cushion block edge and with on portfire is connected; Three, open ignition device and make the resistance wire heating power precast billet of igniting, combustion reactions stops behind 1～5s immediately base substrate is applied the axle pressure 10～50 seconds of 2000kN～5000kN, take out product, imbed quartz sand cooling 20～30 hours in 30 seconds, promptly obtain Nb
2The AlC block ceramic; The steel die of step 2 is that China Patent No. is the steel die in the patent " combustion synthesis reaction device " of ZL03132642.0.
The quality purity of niobium powder of the present invention, aluminium powder and carbon dust is more than 98%.
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 1～5mm as dispersion agent.
Present embodiment utilization burning is synthesized/quasi-iso static pressing original position synthesis technique, so that niobium powder, aluminium powder and carbon dust are that feedstock production goes out highly purified single-phase Nb cheaply
2The AlC ceramic block; One step of synthetic and densification of block ceramic finishes, and preparation technology's cost is low, need not long-time heat, can save a large amount of energy, and energy consumption reduces; The production efficiency height, combustion synthesis reaction can be finished in 5 minutes, the Nb that obtains
2The AlC block ceramic is organized tiny, and compactness is higher; The Nb that present embodiment obtains
2The diameter of AlC block ceramic is 80mm～300mm, and height is 10mm～300mm.
Embodiment 18: present embodiment and embodiment 17 are different is that the mol ratio of niobium powder and aluminium powder is 2: 0.9～1.2 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.7～1.1.Other step and parameter are identical with embodiment 17.
Embodiment 19: present embodiment and embodiment 17 are different is that the mol ratio of niobium powder and aluminium powder is 2: 1.1 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.8.Other step and parameter are identical with embodiment 17.
Embodiment 20: what present embodiment and embodiment 17,18 or 19 were different is to put into resin ball grinder ball milling in the step 1 12～24 hours, perhaps adds dehydrated alcohol ball milling wet mixing 12～24 hours.Other step and parameter are identical with embodiment 17,18 or 19.
Embodiment 21: what present embodiment and embodiment 17,18 or 19 were different is to put into resin ball grinder ball milling in the step 1 16 hours, perhaps adds dehydrated alcohol ball milling wet mixing 16 hours.Other step and parameter are identical with embodiment 17,18 or 19.
Embodiment 22: what present embodiment and embodiment 17 to 21 were different is the pressure that applies 25～38MPa in the step 2 to steel die.Other step and parameter are identical with embodiment 17 to 21.
Embodiment 23: what present embodiment and embodiment 17 to 21 were different is the pressure that applies 32MPa in the step 2 to steel die.Other step and parameter are identical with embodiment 17 to 21.
Embodiment 24: what present embodiment and embodiment 17 to 23 were different is the priming mixture that igniting need be placed 3～7g at firing point in the step 2, and priming mixture is that Ti and C are that 1: 1 blended mixed powder, Ti and B are 1: 2 blended mixed powder or Ti and B in molar ratio in molar ratio
4C is 3: 1 blended mixed powders in molar ratio.Other step and parameter are identical with embodiment 17 to 23.
Embodiment 25: present embodiment and embodiment 17 to 24 are different is the diameter of the husky cake placed on base substrate in the step 2 and the diameter unanimity of cylindrical base substrate.Other step and parameter are identical with embodiment 17 to 24.
Embodiment 26: present embodiment and embodiment 17 to 25 are different is that the portfire of step 2 is provided up to the power supply and the copper conductor of the electric current of 100A by energy moment and forms, and copper conductor connects resistance wire.Other step and parameter are identical with embodiment 17 to 25.
Embodiment 27: present embodiment and embodiment 17 to 26 are different is the axle pressure 15～35 seconds that immediately base substrate is applied 2800kN～4200kN after burning stops in the step 3.Other step and parameter are identical with embodiment 17 to 26.
Embodiment 28: present embodiment and embodiment 17 to 26 are different is the axle pressure 30 seconds that immediately base substrate is applied 3600kN after burning stops in the step 3.Other step and parameter are identical with embodiment 17 to 26.
Embodiment 29: what present embodiment and embodiment 17 to 28 were different is to imbed quartz sand cooling 22～28 hours in the step 3.Other step and parameter are identical with embodiment 17 to 28.
Embodiment 30: the difference of present embodiment and embodiment 17 to 28 is: imbed quartz sand cooling 25 hours in the step 3.Other step and parameter are identical with embodiment 17 to 28.
Embodiment hentriaconta-: present embodiment Nb
2The preparation method of AlC block ceramic realizes by following steps: one, niobium powder, aluminium powder and carbon dust were put into resin ball grinder ball milling 24 hours, 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; Two, mixed powder is put into steel die, apply the pressure 20s of 32MPa to steel die, make mixed powder form a columniform base substrate, place priming mixture and resistance wire at the upper surface central point of base substrate then, on base substrate, place a husky cake then, placing thickness on husky cake is the steel cushion block of 30mm, and the resistance wire lead-in wire is drawn from the cushion block edge and with on portfire is connected; Three, open ignition device and make the resistance wire heating power, immediately base substrate is applied the axle pressure 25 seconds of 3600kN after burning stops, taking out product, imbed quartz sand cooling 25 hours in 30 seconds, promptly obtain Nb
2The AlC block ceramic; The steel die of step 2 is that China Patent No. is the steel die in the patent " combustion synthesis reaction device " of ZL03132642.0.
The quality purity of niobium powder of the present invention, aluminium powder and carbon dust is more than 98%.
Igniting need be placed the priming mixture of 7g at firing point in the present embodiment step 2, and priming mixture is that Ti and C are 1: 1 blended mixed powder in molar ratio.
The Nb that present embodiment obtains
2The diameter of AlC block ceramic is 300mm, and height is 20mm.
The Nb that present embodiment obtains
2The AlC block ceramic is by single-phase Nb
2AlC forms, and the purity height has good micro-plasticity, good mechanical property.
Embodiment 32: what present embodiment was different with the embodiment hentriaconta-is in the step 1 niobium powder, aluminium powder and carbon dust to be put into the resin ball grinder, adding the wet mixing of dehydrated alcohol ball milling then dries after 24 hours naturally, get 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.Other step and parameter are identical with embodiment 32.
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 3mm as dispersion agent.
The Nb that present embodiment obtains
2The diameter of AlC block ceramic is 300mm, and height is 20mm.
The Nb that present embodiment obtains
2The AlC block ceramic is by single-phase Nb
2AlC forms, and the purity height has good micro-plasticity, good mechanical property.
Claims (10)
1.Nb
2The preparation method of AlC block ceramic is characterized in that Nb
2The preparation method of AlC block ceramic realizes by following steps: one, 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, get 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; Two, apply pressure 10～20s of 15～45MPa to mixed powder, mixed powder is pressed into precast billet, then precast billet is put into mould, fill with quartz sand in space between mould and the precast billet, again mould and precast billet are put into the combustion synthesis reaction device together, in the upper surface centerfire of precast billet, the self-propagating combustion reaction takes place then; Three, begin to apply the pressure of 160～480MPa behind combustion reactions end 1～5s, pressurize 10～15s imbeds quartz sand with reaction product again and is cooled to room temperature, promptly obtains Nb
2The AlC block ceramic.
2. Nb according to claim 1
2The preparation method of AlC block ceramic is characterized in that the mol ratio of niobium powder and aluminium powder is 2: 0.9～1.2 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.7～1.1.
3. Nb according to claim 1
2The preparation method of AlC block ceramic is characterized in that the mol ratio of niobium powder and aluminium powder is 2: 1.1 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.8.
4. according to claim 1,2 or 3 described Nb
2The preparation method of AlC block ceramic is characterized in that the mould in the step 2 is the " TiC-TiB that delivers 2003 the 4th phases " Journal of Inorganic Materials "
2The self propagating high temperature study on the synthesis of/Cu matrix material " in mould.
5. Nb according to claim 4
2The preparation method of AlC block ceramic is characterized in that combustion synthesis reaction in the step 3 finishes the pressure of after-applied 240～380MPa, pressurize 11～14s.
6.Nb
2The preparation method of AlC block ceramic is characterized in that Nb
2The preparation method of AlC block ceramic realizes by following steps: one, 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, get 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; Two, mixed powder is put into steel die, apply pressure 20～25s of 15～45MPa, make mixed powder form a columniform base substrate, then at the upper surface central point of base substrate, perhaps on being the radius mid point of hexagonal angle mutually, three of upper surface place priming mixture and resistance wire, place a husky cake then on base substrate, placing thickness on husky cake is the steel cushion block of 30mm, and the resistance wire lead-in wire is drawn from the cushion block edge and with on portfire is connected; Three, open ignition device and make the resistance wire heating power precast billet of igniting, combustion reactions stops behind the 1-5s immediately base substrate is applied the axle pressure 10～50 seconds of 2000kN～5000kN, take out product, in 30 seconds, imbed quartz sand cooling 20～30 hours, promptly obtain Nb
2The AlC block ceramic; The steel die of step 2 is that China Patent No. is the steel die in the patent " combustion synthesis reaction device " of ZL03132642.0.
7. Nb according to claim 6
2The preparation method of AlC block ceramic is characterized in that the mol ratio of niobium powder and aluminium powder is 2: 0.9～1.2 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.7～1.1.
8. Nb according to claim 6
2The preparation method of AlC block ceramic is characterized in that the mol ratio of niobium powder and aluminium powder is 2: 1.1 in the step 1, and the mol ratio of niobium powder and carbon dust is 2: 0.8.
9. according to claim 6,7 or 8 described Nb
2The preparation method of AlC block ceramic is characterized in that after combustion reactions stops in the step 3 immediately base substrate is applied the axle pressure 15～35 seconds of 2800kN～4200kN.
10. according to claim 6,7 or 8 described Nb
2The preparation method of AlC block ceramic is characterized in that in the step 3 immediately base substrate being applied after burning stops the axle pressure 30 seconds of 3600kN.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102321473A (en) * | 2011-02-16 | 2012-01-18 | 钟贤龙 | Method for manufacturing fluorescent material with Mg-alpha-SiAlON as main crystal lattice |
| CN103274695A (en) * | 2013-05-31 | 2013-09-04 | 哈尔滨工业大学 | Burning, synthesizing and casting method of non-oxide eutectic ceramics |
| CN103288436A (en) * | 2013-05-31 | 2013-09-11 | 哈尔滨工业大学 | Method for synthetizing fused cast by combustion of MgAl2O4 ceramic |
| CN104150906A (en) * | 2014-07-01 | 2014-11-19 | 河海大学 | Method for preparing Ta2AlC ceramic powder by virtue of combustion synthesis |
| CN104628386A (en) * | 2015-02-05 | 2015-05-20 | 河海大学 | Preparation method of Ta2AlC block ceramic |
| CN106187194A (en) * | 2016-07-20 | 2016-12-07 | 哈尔滨师范大学 | A kind of Ti2the preparation method of SnC block ceramic |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2901721B1 (en) * | 2006-05-30 | 2008-08-22 | Commissariat Energie Atomique | MAX PHASE POWDERS AND PROCESS FOR PRODUCING SAID POWDERS |
| CN101186294B (en) * | 2007-12-12 | 2010-06-09 | 哈尔滨工业大学 | Method of preparing high purity Ti2AlC block material |
| CN101186295B (en) * | 2007-12-12 | 2010-12-01 | 哈尔滨工业大学 | Method of preparing high purity Ti2AlC block material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321473A (en) * | 2011-02-16 | 2012-01-18 | 钟贤龙 | Method for manufacturing fluorescent material with Mg-alpha-SiAlON as main crystal lattice |
| CN103274695A (en) * | 2013-05-31 | 2013-09-04 | 哈尔滨工业大学 | Burning, synthesizing and casting method of non-oxide eutectic ceramics |
| CN103288436A (en) * | 2013-05-31 | 2013-09-11 | 哈尔滨工业大学 | Method for synthetizing fused cast by combustion of MgAl2O4 ceramic |
| CN103288436B (en) * | 2013-05-31 | 2014-10-08 | 哈尔滨工业大学 | Method for synthetizing fused cast by combustion of MgAl2O4 ceramic |
| CN103274695B (en) * | 2013-05-31 | 2014-10-08 | 哈尔滨工业大学 | Burning, synthesizing and casting method of non-oxide eutectic ceramics |
| CN104150906A (en) * | 2014-07-01 | 2014-11-19 | 河海大学 | Method for preparing Ta2AlC ceramic powder by virtue of combustion synthesis |
| CN104150906B (en) * | 2014-07-01 | 2016-09-14 | 河海大学 | A kind of conbustion synthesis prepares Ta2the method of AlC ceramic powder |
| CN104628386A (en) * | 2015-02-05 | 2015-05-20 | 河海大学 | Preparation method of Ta2AlC block ceramic |
| CN106187194A (en) * | 2016-07-20 | 2016-12-07 | 哈尔滨师范大学 | A kind of Ti2the preparation method of SnC block ceramic |
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