CN105693285B - A kind of method that hafnium carbide nano wire is prepared in 2D acupuncture carbon felts - Google Patents
A kind of method that hafnium carbide nano wire is prepared in 2D acupuncture carbon felts Download PDFInfo
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- CN105693285B CN105693285B CN201610037886.6A CN201610037886A CN105693285B CN 105693285 B CN105693285 B CN 105693285B CN 201610037886 A CN201610037886 A CN 201610037886A CN 105693285 B CN105693285 B CN 105693285B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
Abstract
The present invention relates to a kind of method that hafnium carbide nano wire is prepared in 2D acupuncture carbon felts, the method for preparing HfC nano wires in 2D acupuncture carbon felts using catalyst auxiliary polyalcohol polymer pyrolysis technology, it can simply and efficiently synthesize HfC nano wires using this method.This method is reaction raw materials from HfC polymer precursors PHC, and nickel nitrate is catalyst, and high-purity argon gas is protective atmosphere, and hydrogen is reducing gas.By adjusting process of thermal treatment parameter, once property prepares HfC nano wires in 2D acupuncture carbon felts.The beneficial effects of the invention are as follows：Synthesis technique is simple, cost is low, short preparation period, it is not necessary to pre-synthesis technique (preparing CNT etc.)；HfC nano wires are made at ambient pressure, and the requirement to equipment is low；And the pattern and purity that can effectively control the HfC of synthesis by adjusting heat treatment parameter.These advantages make this method have the potentiality for developing into large-scale industrial production.
Description
Technical field
The invention belongs to the preparation method of hafnium carbide (HfC) nano wire, and in particular to one kind is prepared in 2D acupuncture carbon felts
The method of hafnium carbide nano wire.
Background technology
HfC fusing point is up to 3900 DEG C, is the superhigh temperature ceramics for the most infusibility being currently known, while conductance and thermal conductivity
Well, there is high rigidity, fabulous wear-resisting and decay resistance, particularly remained in extremely harsh superhigh temperature aerobic environment
Keep good heat endurance and thermal shock resistance.This series of excellent properties makes HfC turn into preferable high-temperature structural material,
Applied in national defences such as Aero-Space, including superhigh temperature ceramics ablation resistant material, the anti-yaw damper of carbon/carbon compound material
Coating, matrix modification additive etc..Since Japanese scholars (Lijima) find CNT since 1991, monodimension nanometer material is just
Receive much concern.HfC nano wires have the excellent resistance to elevated temperatures of traditional HfC block materials and the excellent mechanics of monodimension nanometer material concurrently
Performance, it is incorporated into all kinds of matrixes in the form of the second phase prepare HfC nano wires enhancing composite be increasingly becoming it is new
Study hotspot.
It is however, very few by the preparation report currently on HfC nano wires.
" Xuanke Li, Aidan Westwood, Andy Brown, Rik Brydson, the Brian Rand.A of document 1
convenient,general synthesis of carbide nanofibres via templated reactions on
carbon nanotubes in molten salt media.Carbon 2009；47:201-208 " discloses one kind and uses carbon
The method that nanotube template prepares HfC nanofibers.This method is existed by adding LiCl, KCl and KF of certain mass ratio
950-960 DEG C obtains a liquid-phase fused salts reaction media and promotes metal Hf powder to react system at such a temperature with multi-walled carbon nanotube
It is standby go out HfC nanofibers.It is several microns that length, which has been made, although with this method, a diameter of 40-90nm HfC nanofibers,
But because the nanofiber is that polycrystalline structure will influence its mechanical property.In addition, it is miscellaneous to introduce alkali metal cation in process
Matter, this will influence chemical stability of the HfC nanofibers under superhigh temperature.
Document 2 " Jinshi Yuan, Han Zhang, Jie Tang, Norio Shinya, Kiyomi Nakajima, and
Lu-Chang Qin.Synthesis and characterization of single crystalline hafnium
carbide nanowires.J.Am.Ceram.Soc 2012；1-5 " is disclosed one kind and prepared using chemical vapour deposition technique
The method of HfC nano wires.This method is in 1280 DEG C of synthesis temperature and 10-1Under Pa negative pressure, using Ni nano particle conduct
Catalyst, in HfCl4-CH4-H2Reaction system in prepared the HfC nano wires of monocrystalline.Obtained nanowire length is several
Ten microns, a diameter of 20-80nm.But the preparation technology of this method is complex, the cycle is longer, and using nano level
Ni particles require higher as catalyst, therefore to process equipment, and corresponding increase prepares cost.
Research of the scholars to HfC nano wires in recent years has achieved some achievements, however, still suffering from such or such
Deficiency.MATECH Global Strategic Material companies of the U.S. are utilized using polymer precursor conversion method and simply set
Standby to have prepared a diameter of 5 μm, length is up to 30km monofilament polycrystalline HfC fibers, and prepared HfC fibers are with well resistance to
High-temperature behavior and mechanical property, can be as rocket nozzle and the reinforcement material of supersonic vehicle leading edge.But to being at present
Only, it yet there are no any report on preparing high quality HfC nano wires in 2D acupuncture carbon felts using polymer precursor conversion method
Road.
The content of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that one kind prepares hafnium carbide nanometer in 2D acupuncture carbon felts
The method of line, overcome the shortcomings of that existing method prepares HfC nano wires cost height, preparation technology complexity, while prepare high quality
HfC nano wires.
Technical scheme
A kind of method that hafnium carbide nano wire is prepared in 2D acupuncture carbon felts, it is characterised in that step is as follows：
Step 1：HfC presomas PHC and metallic catalyst nickel nitrate are mixed, pouring into acetone makes it be diluted to containing catalyst
HfC precursor solutions, room temperature be 15~30 DEG C under the conditions of be stirred, be configured to uniform mixed solution；Before the HfC
The mass fraction ratio for driving body PHC and metallic catalyst nickel nitrate is 99:1~90:10；
Step 2：The 2D acupuncture carbon fiber felts cleaned up are put into 30~40min of immersion in mixed solution, then taken out
Dry drying；
Step 3：The 2D acupuncture carbon fiber felts that step 2 treats are placed in corundum crucible and are pushed into tube furnace, will be managed
Formula stove evacuation degree reaches -0.09MPa, stands 10~30 minutes, leads to Ar gas to normal pressure, H2For reducing gas, this process repeats
Repeatedly；The gas flow of the Ar gas is 50~100ml/min；
Step 4：Furnace temperature is risen to 200~300 DEG C with 3~5 DEG C/min programming rate, makes precursor polymer in the temperature
2~4h of full cross-linked solidification under degree；400~500 DEG C are warming up to 3~5 DEG C/min programming rate again, is incubated 1.5~3.5h,
H is passed through in last 0.5h2, nickel nitrate is reduced to elemental nickel；Afterwards again with 5~10 DEG C/min programming rate by furnace temperature liter
To 1500~1600 DEG C, soaking time is 2~4h, heating power supply Temperature fall is closed after the completion of insulation, in the table of carbon fiber felt
Face obtains the HfC nano wires of one layer of light/dark balance.
Being stirred for the step 1 is stirred 2~4 hours using magnetic stirrer.
The drying drying of the step 2 is placed in drying box, and temperature is 80~100 DEG C.
The step 3 is repeatedly 3 times.
The nickel nitrate is pure, weight/mass percentage composition >=99.8% of analysis.
The Ar is the high-purity gas that purity is more than 99.999%.
The H2It is more than 99.999% high-purity gas for purity.
The purity of the acetone is more than 99.0%.
Beneficial effect
A kind of method that hafnium carbide nano wire is prepared in 2D acupuncture carbon felts proposed by the present invention, aided in using catalyst poly-
The method that compound polymer pyrolysis technology prepares HfC nano wires in 2D acupuncture carbon felts, can be simply and efficiently using this method
Synthesize HfC nano wires.This method is reaction raw materials from HfC polymer precursors PHC, and nickel nitrate is catalyst, high-purity argon
Gas is protective atmosphere, and hydrogen is reducing gas.By adjusting process of thermal treatment parameter, once prepared by property in 2D acupuncture carbon felts
Go out HfC nano wires.
The beneficial effects of the invention are as follows：Synthesis technique is simple, cost is low, short preparation period, it is not necessary to pre-synthesis technique
(preparing CNT etc.)；HfC nano wires are made at ambient pressure, and the requirement to equipment is low；And can be by adjusting heat treatment ginseng
The number effectively HfC of control synthesis pattern and purity.These advantages have this method to develop into the latent of large-scale industrial production
Power.
Brief description of the drawings
Fig. 1 is flow chart of the method for the present invention；
Fig. 2 is the HfC nano wire low power stereoscan photographs prepared by the embodiment of the present invention 1,2,3 respectively；
Fig. 3 is the high power scanned photograph for the HfC nano wires that the embodiment of the present invention 2 is prepared in 2D acupuncture carbon felts；
Fig. 4 is the X ray diffracting spectrum for the HfC nano wires that the embodiment of the present invention 2 is prepared in 2D acupuncture carbon felts.
Embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment 1：
1) the 2D acupunctures carbon fiber felt that size is 35mm × 30mm × 10mm is surpassed with deionized water and absolute ethyl alcohol respectively
Sound cleans 1h, and ultrasonic power is set to 90W, is put into 80~100 DEG C of baking oven and is dried for standby.
2) 10g HfC presoma PHC and 0.1g metallic catalyst nickel nitrates are weighed respectively in beaker, pour into 20g acetone
Solution, 2~4h is stirred using magnetic stirrer under the conditions of being 15~30 DEG C in room temperature, makes presoma and catalyst in acetone soln
In fully dissolve and be well mixed.The 2D acupuncture carbon fiber felts cleaned up are put into the solution and soak 30min, are then taken out
It is placed in 80~100 DEG C of baking oven and is dried for standby.
3) catalyst auxiliary polyalcohol polymer pyrolysis technique prepares HfC nano wires, and specific method is as follows：
2D acupuncture carbon fiber felts after being dried in step 2) are placed in corundum crucible and are slowly pushed into tube furnace, will be managed
Formula stove evacuation 15min makes vacuum reach -0.09MPa, stands 10~30min, leads to Ar gas to normal pressure, this process and repeats three
Secondary, Ar gas is protective gas, and the control of its gas flow is 50ml/min, H2Gas is reducing gas.With 3 DEG C/min programming rate
Furnace temperature is risen to 200 DEG C, makes precursor polymer full cross-linked solidification 2h at such a temperature.Again with 3 DEG C/min programming rate
400 DEG C are warming up to, 1.5h is incubated, H is passed through in last 0.5h2, the purpose of the process is that nickel nitrate is reduced into elemental nickel, it
Furnace temperature is risen to 1500 DEG C with 5 DEG C/min programming rate again afterwards, soaking time 2h.Heating power supply is closed after the completion of insulation certainly
So cooling.
It can be seen that the HfC nano wires that the embodiment is prepared in 2D acupuncture carbon felts are mostly linear from Fig. 2 a, it is fine along carbon
Dimension table face radial distribution, the uniform soilless sticking phenomenon of nano wire.Prepared nanowire diameter reaches several micro- in 300nm or so, length
Rice.
Embodiment 2：
1) the 2D acupunctures carbon fiber felt that size is 35mm × 30mm × 10mm is surpassed with deionized water and absolute ethyl alcohol respectively
Sound cleans 1h, and ultrasonic power is set to 90W, is put into 80~100 DEG C of baking oven and is dried for standby.
2) 10gHfC presoma PHC and 0.5g metallic catalyst nickel nitrates are weighed respectively in beaker, and it is molten to pour into 20g acetone
Liquid, 2~4h is stirred using magnetic stirrer under the conditions of being 15~30 DEG C in room temperature, makes presoma and catalyst in acetone soln
In fully dissolve and be well mixed.The 2D acupuncture carbon fiber felts cleaned up are put into the solution and soak 40min, are then taken out
It is placed in 80~100 DEG C of baking oven and is dried for standby.
3) catalyst auxiliary polyalcohol pioneer body technology conversion prepares HfC nano wires, and specific method is as follows：
2D acupuncture carbon fiber felts after being dried in step 2) are placed in corundum crucible and are slowly pushed into tube furnace, will be managed
Formula stove evacuation 15min makes vacuum reach -0.09MPa, stands 10~30min, leads to Ar gas to normal pressure, this process and repeats three
Secondary, Ar gas is protective gas, and the control of its gas flow is 70ml/min, H2Gas is reducing gas.With 4 DEG C/min programming rate
Furnace temperature is risen to 250 DEG C, makes precursor polymer full cross-linked solidification 3h at such a temperature.Again with 4 DEG C/min programming rate
450 DEG C are warming up to, 2.5h is incubated, H is passed through in last 0.5h2, the purpose of the process is that nickel nitrate is reduced into elemental nickel, it
Furnace temperature is risen to 1550 DEG C with 7 DEG C/min programming rate again afterwards, soaking time 3h.Heating power supply is closed after the completion of insulation certainly
So cooling.
It can be seen that the HfC nano wires that the embodiment is prepared in 2D acupuncture carbon felts are mostly curve-like from Fig. 2 b, be orientated nothing
Regular distribution.Prepared nanowire diameter is 300nm, and length is more than ten microns.
Embodiment 3：
1) the 2D acupunctures carbon fiber felt that size is 35mm × 30mm × 10mm is surpassed with deionized water and absolute ethyl alcohol respectively
Sound cleans 1h, and ultrasonic power is set to 90W, is put into 80~100 DEG C of baking oven and is dried for standby.
2) 10gHfC presoma PHC and 1g metallic catalyst nickel nitrates are weighed respectively in beaker, and it is molten to pour into 20g acetone
Liquid, 2~4h is stirred using magnetic stirrer under the conditions of being 15~30 DEG C in room temperature, makes presoma and catalyst in acetone soln
In fully dissolve and be well mixed.The 2D acupuncture carbon fiber felts cleaned up are put into the solution and soak 1h, then takes out and puts
It is dried for standby in 80~100 DEG C of baking oven.
3) catalyst auxiliary polyalcohol polymer pyrolysis technique prepares HfC nano wires, and specific method is as follows：
2D acupuncture carbon fiber felts after being dried in step 2) are placed in corundum crucible and are slowly pushed into tube furnace, will be managed
Formula stove evacuation 15min makes vacuum reach -0.09MPa, stands 10min, leads to Ar gas to normal pressure, this process in triplicate, Ar
Gas is protective gas, and the control of its gas flow is 100ml/min, H2Gas is reducing gas.With 5 DEG C/min programming rate by stove
Temperature rise makes precursor polymer full cross-linked solidification 4h at such a temperature to 300 DEG C.Heated up again with 5 DEG C/min programming rate
To 500 DEG C, 3.5h is incubated, H is passed through in last 0.5h2, the purpose of the process is that nickel nitrate is reduced into elemental nickel, Zhi Houzai
Furnace temperature is risen to 1600 DEG C with 10 DEG C/min programming rate, soaking time 4h.It is natural that heating power supply is closed after the completion of insulation
Cooling.
It can be seen that the HfC nano wires that the embodiment is prepared in 2D acupuncture carbon felts are mostly curve-like from Fig. 2 c, be orientated nothing
Regular distribution, for the nanowire diameter of preparation in 500nm or so, length is more than ten microns.
In all embodiments, described nickel nitrate is to analyze pure (weight/mass percentage composition >=99.8%), Ar and H2It is
Purity is more than 99.999% high-purity gas, and the purity of acetone is more than 99.0%.
Claims (8)
- A kind of 1. method that hafnium carbide nano wire is prepared in 2D acupuncture carbon felts, it is characterised in that step is as follows：Step 1：HfC presomas PHC and metallic catalyst nickel nitrate are mixed, pouring into acetone makes it be diluted to containing catalyst HfC precursor solutions, it is stirred under the conditions of being 15~30 DEG C in room temperature, is configured to uniform mixed solution；The HfC forerunner The mass fraction of body PHC and metallic catalyst nickel nitrate ratio is 99:1~90:10；Step 2：The 2D acupuncture carbon fiber felts cleaned up are put into 30~40min of immersion in mixed solution, then take out drying Drying；Step 3：The 2D acupuncture carbon fiber felts that step 2 treats are placed in corundum crucible and are pushed into tube furnace, by tube furnace Suction reaches -0.09MPa, stands 10~30 minutes, leads to Ar gas to normal pressure, H2For reducing gas, this process is repeatedly； The gas flow of the Ar gas is 50~100ml/min；Step 4：Furnace temperature is risen to 200~300 DEG C with 3~5 DEG C/min programming rate, makes precursor polymer at such a temperature 2~4h of full cross-linked solidification；400~500 DEG C are warming up to 3~5 DEG C/min programming rate again, 1.5~3.5h is incubated, most 0.5h afterwards is passed through H2, nickel nitrate is reduced to elemental nickel；Furnace temperature is risen to 5~10 DEG C/min programming rate again afterwards 1500~1600 DEG C, soaking time is 2~4h, heating power supply Temperature fall is closed after the completion of insulation, on the surface of carbon fiber felt Obtain the HfC nano wires of one layer of light/dark balance.
- 2. the method for hafnium carbide nano wire is prepared in 2D acupuncture carbon felts according to claim 1, it is characterised in that：The step Rapid 1 be stirred is stirred 2~4 hours using magnetic stirrer.
- 3. the method for hafnium carbide nano wire is prepared in 2D acupuncture carbon felts according to claim 1, it is characterised in that：The step Rapid 2 drying drying is placed in drying box, and temperature is 80~100 DEG C.
- 4. the method for hafnium carbide nano wire is prepared in 2D acupuncture carbon felts according to claim 1, it is characterised in that：The step Rapid 3 repeatedly be 3 times.
- 5. the method for hafnium carbide nano wire is prepared in 2D acupuncture carbon felts according to claim 1, it is characterised in that：The nitre Sour nickel is pure, weight/mass percentage composition >=99.8% of analysis.
- 6. the method for hafnium carbide nano wire is prepared in 2D acupuncture carbon felts according to claim 1, it is characterised in that：The Ar It is more than 99.999% high-purity gas for purity.
- 7. the method for hafnium carbide nano wire is prepared in 2D acupuncture carbon felts according to claim 1, it is characterised in that：The H2 It is more than 99.999% high-purity gas for purity.
- 8. the method for hafnium carbide nano wire is prepared in 2D acupuncture carbon felts according to claim 1, it is characterised in that：Described third The purity of ketone is more than 99.0%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730685A (en) * | 2012-07-03 | 2012-10-17 | 西北工业大学 | Method for preparing one-dimensional hafnium carbide nanometer material |
| CN103194734A (en) * | 2013-04-15 | 2013-07-10 | 西北工业大学 | Preparation method of self-assembled three-dimensional hafnium carbide whisker network structure |
| CN103951470A (en) * | 2014-04-04 | 2014-07-30 | 西北工业大学 | Hafnium carbide nanowire-toughened ceramic coating layer of surface of carbon/carbon composites and preparation method thereof |
| CN103964883A (en) * | 2014-04-25 | 2014-08-06 | 西北工业大学 | Preparation method for thin wall or tapered member made from one-dimensional nanofiber reinforced and toughened carbon-ceramic composite |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730685A (en) * | 2012-07-03 | 2012-10-17 | 西北工业大学 | Method for preparing one-dimensional hafnium carbide nanometer material |
| CN103194734A (en) * | 2013-04-15 | 2013-07-10 | 西北工业大学 | Preparation method of self-assembled three-dimensional hafnium carbide whisker network structure |
| CN103951470A (en) * | 2014-04-04 | 2014-07-30 | 西北工业大学 | Hafnium carbide nanowire-toughened ceramic coating layer of surface of carbon/carbon composites and preparation method thereof |
| CN103964883A (en) * | 2014-04-25 | 2014-08-06 | 西北工业大学 | Preparation method for thin wall or tapered member made from one-dimensional nanofiber reinforced and toughened carbon-ceramic composite |
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