CN104671245A - Preparation method of hafnium carbide nano-powder - Google Patents
Preparation method of hafnium carbide nano-powder Download PDFInfo
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- CN104671245A CN104671245A CN201510091845.0A CN201510091845A CN104671245A CN 104671245 A CN104671245 A CN 104671245A CN 201510091845 A CN201510091845 A CN 201510091845A CN 104671245 A CN104671245 A CN 104671245A
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Abstract
The invention relates to a preparation method of hafnium carbide nano-powder. The preparation method comprises steps as follows: 1) preparing hafnium-containing gel: dissolving HfCl4 and C6H8O7*H2O in deionized water, continuously stirring the mixture to fully dissolve the HfCl4 and the C6H8O7*H2O, then adjusting the pH value to range from 2 to 3 with an ammonia water solution, and performing magnetic stirring treatment at the constant temperature of 60-80 DEG C to obtain the hafnium-containing gel; 2) preparing precursor powder: placing the hafnium-containing gel into a low-temperature tube furnace for heat treatment to obtain the precursor powder; (3) preparing the hafnium carbide nano-powder: placing the precursor powder into a planetary ball-milling tank for high-energy ball milling, and placing obtained powder into a discharge plasma sintering furnace for reactions to obtain the hafnium carbide nano-powder. The method is simple in technology, low in energy consumption, good in repeatability and good in industrial prospect, and the prepared hafnium carbide nano-powder is a high-activity nano-scale product with hafnium carbide distributed evenly and is even in crystal grain distribution, high in purity and good in degree of crystallinity.
Description
Technical field
The invention belongs to ceramic powder preparing technical field, relate to a kind of preparation method of hafnium carbide nano-powder.
Background technology
HfC is the non-stoichiometric carbide of one that transition element Hf and C is formed, i.e. HfC
x(0.5≤x≤1), it belongs to a kind of superhard material.According to JCPDF card, its structure is the face-centred cubic structure of NaCl type, and its lattice parameter is that 0.46375nm, Hf atom forms cubic(al)grating closely, and C atom is in the octahedral interstice position of lattice.HfC crystal is that the atomic bond carbon hafnium key being a/2 by bond length connects, and this key is symmetrical.Atoms metal face adjacent between (111) face in HfC crystalline structure is connected by most strong bond energy atomic bond key with between C atomic plane, most strong bond must be destroyed during slippage, therefore slippage is very difficult, macroscopically show ultrahigh hardness characteristic, its Morse hardness is 9M.Due to the atomic bond that destruction height necessary during HfC crystal melting is symmetrical, thus very difficult, thus macroscopically show superelevation melting point property, and the bond energy E of the atomic bond of HfC
a=87.2163kJ/mol, therefore the fusing point of HfC is up to 3900 DEG C.Its volume specific resistance is 1.95 × 10
-4Ω cm (2900 DEG C), thermal expansivity is 6.73 × 10
-6/ DEG C, its oxidizing temperature is 400 DEG C.Because its high rigidity and high-melting-point cause the great interest of domestic and international researchist, be key position or the most promising ultrahigh-temperature candidate materials of parts such as parting tool, aircraft nose cone, the leading edge of a wing, numbers of hot-side engine, have immeasurable application prospect in fields such as nuclear rocket power plant, nuclear reactor, space ships.
At present, few to the method report of hafnium carbide synthesis both at home and abroad, the method of report mainly contains: (1) is carbothermic method directly, general needs could react more than 1900 DEG C, energy consumption is high, high to equipment requirements, and the particle size grown out is large, needs to reduce temperature of reaction by additive method is auxiliary.(2) liquid precursor conversion method, the people such as Wang Yanbin are with HfOCl
2, HCl, HNO
3, n-propyl alcohol, Virahol, ethanol, methyl ethyl diketones etc. are raw material, under 1500 DEG C of conditions, prepared that granule-morphology differs, size at the HfC powder of tens nanometers to hundreds of nanometer, and particle has serious agglomeration.(3) chemical Vapor deposition process, the people such as Karlsruhe GmbH, with HfCl
4with appropriate CH
4and H
2for raw material, utilize vapour deposition process, hafnium carbide successfully prepared by the substrate of atresia.This method long reaction time, consume energy high, output is little.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, a kind of sol-gel method is provided to prepare the method for hafnium carbide nano-powder in conjunction with being rapidly heated of discharge plasma sintering stove (SPS)-falling temperature technique, energy consumption is low, productive rate is high, and the hafnium carbide nano-powder purity of preparation is high, better crystallinity degree.
For solving the problems of the technologies described above, technical scheme provided by the invention is:
There is provided a kind of preparation method of hafnium carbide nano-powder, its step is as follows:
1) preparation is containing hafnium gel: by HfCl
4and C
6h
8o
7h
2o is dissolved in deionized water, HfCl
4be 0.20-0.25g/mL, wherein HfCl with the mass volume ratio of water
4and C
6h
8o
7h
2o mol ratio is 1:0.5-1.5, and constantly stirring makes it fully dissolve, and then regulates pH to 2-3 with ammonia soln, and 60-80 DEG C of constant temperature lower magnetic force stir process, obtains containing hafnium gel;
2) precursor powder is prepared: by step 1) gained puts into the thermal treatment of low temperature tube furnace containing hafnium gel, and with the ramp to 800 DEG C of 3-10 DEG C/min under room temperature, and be incubated 1-3h, atmosphere is Ar, obtains precursor powder;
3) hafnium carbide nano-powder is prepared: by step 2) gained precursor powder puts into planetary type ball-milling tank and carries out high-energy ball milling, gained powder is placed in discharge plasma sintering oven, under vacuum, under room temperature with the ramp of 200-400 DEG C/min to 1500-1800 DEG C, insulation 3-10min, then be cooled to room temperature with the speed of 100-200 DEG C/min and namely obtain hafnium carbide nano-powder.
Preferably, step 1) middle HfCl
4and C
6h
8o
7h
2o mol ratio is 1:1.
By such scheme, step 1) described ammonia soln mass concentration is 25%.
By such scheme, step 1) described magnetic agitation speed is 60-80r/min, the magnetic agitation time is 30-60min.
By such scheme, step 3) described high-energy-milling is: planetary type ball-milling tank revolution rotating speed is 200-250r/min, and rotation rotating speed is 400-500r/min, and Ball-milling Time is 1-3h.
By such scheme, step 3) described sintering process is: under vacuum, with the ramp to 1600 DEG C of 300 DEG C/min under room temperature, insulation 5min, then cool with the speed of 200 DEG C/min.
(1) beneficial effect of the present invention is: 1, the present invention prepares precursor powder by sol-gel method in conjunction with low temperature tube annealing method, then high-energy-milling pre-treatment precursor powder is adopted, C with Hf is fully contacted and is placed in discharge plasma sintering oven to be rapidly heated-to lower the temperature sintering, obtained hafnium carbide nano-powder at a lower temperature, the inventive method can reduce the growth that temperature of reaction is also conducive to final product HfC nanocrystal, technique is simple, energy consumption is low, reproducible, there is good industrialization prospect; 2, the hafnium carbide nano-powder that prepared by the present invention is other product of the equally distributed High-activity nano-grade of carbon hafnium, and crystal grain is evenly distributed, and purity is high, better crystallinity degree.
Accompanying drawing explanation
X-ray diffraction (XRD) collection of illustrative plates of the HfC nano-powder of Fig. 1 prepared by the embodiment of the present invention 1;
Field emission scanning electron microscope (FESM) photo of the HfC nano-powder of Fig. 2 prepared by embodiment 1;
The low resolution map of the transmission electron microscope (TEM) of the HfC nano-powder of Fig. 3 prepared by embodiment 1 (Fig. 3 a) and the high resolution collection of illustrative plates (Fig. 3 b) of transmission electron microscope;
The Raman spectrogram of the HfC nano-powder of Fig. 4 prepared by embodiment 1;
The infared spectrum of the HfC nano-powder of Fig. 5 prepared by embodiment 1.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment of the present invention HfCl used
4powder is analytical pure, and granularity is 200-300 order, and Citric acid monohydrate Food grade is analytical pure, and ammonia soln concentration is 25wt%.
Embodiment 1
Take 15g HfCl
4, 9.84g C
6h
8o
7h
2o (HfCl
4and C
6h
8o
7h
2o mol ratio is 1:1) put into 1000mL beaker, add 65mL deionized water, constantly stir with glass stick, make HfCl
4and C
6h
8o
7h
2o fully dissolves in deionized water, then adds appropriate NH with drop-burette
3h
2the pH of O solution (mass concentration is 25%) regulator solution is 2-3, and carries out magnetic agitation process under 80 DEG C of constant temperature, and magnetic agitation speed is 60r/min, and churning time is 30min, obtains containing hafnium gel.To be placed in alumina crucible containing hafnium gel to put into the thermal treatment of low temperature tube furnace and obtain precursor powder, annealing process is be raised to 800 DEG C with the heat-up rate of 4 DEG C/min under room temperature, and insulation 2h, atmosphere is high-purity Ar, and Ar flow is 0.5L/min.Taken out by the precursor powder obtained after anneal, put into planetary type ball-milling tank, ball milling revolution 250r/min, rotation 500r/min, Ball-milling Time is 3 hours.Ball milling material is taken out, be placed in graphite jig, put into discharge plasma sintering oven to synthesize, vacuum tightness is 10Pa, with the ramp to 1600 DEG C of 300 DEG C/min under room temperature, soaking time is 5min, then is cooled to room temperature with the speed of 200 DEG C/min, can obtain grey HfC nano-powder 11.356g, product yield is 87.3%.
Be illustrated in figure 1 the XRD figure spectrum of embodiment of the present invention gained HfC nano-powder, as seen from the figure, X-ray diffraction peak and HfC standard diffraction card PDF#65-8748 match.Diffraction peak d value 2.6650,2.3076,1.6322,1.3937,
place, correspond respectively to (111), (200), (220) of hafnium carbide, (311), (222) crystal face, by XRD each crystal face d value, calculating product lattice constant is a=0.4619nm, basically identical with standard card a=0.4621nm, show that product is hafnium carbide.Can find out that from XRD spectra diffraction peak is very strong, illustrate that product crystallinity is fine; Find the diffraction peak that there are not other materials such as crystalline carbon in diffraction peak simultaneously, illustrate that product purity is very high.
Be illustrated in figure 2 the FESM photo of the present embodiment gained HfC nano-powder, as seen from the figure, powder granule size 150-350nm, median size 250nm, particle presents irregularly shaped, even particle distribution, does not find obvious amorphous carbon.
Be illustrated in figure 3 the TEM picture of the HfC nano-powder prepared by the present embodiment, Fig. 3 a is the TEM picture of HfC nano sized powder sample, and as seen from the figure, powder granule size median size is at about 250nm.Because Hf element belongs to heavy metal, so demonstrate deep black back end in TEM electromicroscopic photograph.Fig. 3 b is the HRTEM photo of sample, and as seen from the figure, sample crystallinity is good, and spacing is 0.268nm, corresponding to (111) crystal face of HfC crystal.
Be illustrated in figure 4 the Raman spectrogram of the HfC nano-powder prepared by the present embodiment, similar with ZrC, HfC is also non-stoichiometric compound, in HfC lattice, there is carbon room, therefore may contain uncombined carbon in the product, adopt Raman spectrum to measure uncombined carbon, D peak and G peak is there is in figure, containing uncombined carbon in known product, but D peak and G are relatively milder, illustrate that free carbon content is less.
Be illustrated in figure 5 the infared spectrum of the HfC nano-powder prepared by the present embodiment, three obvious absorption peaks can be observed in figure, lay respectively at 3442,1635 and 1036cm
-1place.Wherein 3442cm
-1and 1635cm
-1absorption peak owing to the vibration peak of-OH group in planar water and H-O-H key, and can be positioned at 1036cm
-1the absorption peak gone out is caused by the vibration due to Hf-C-O key.
The chemical composition analysis result of the HfC nano-powder prepared by the present embodiment is as follows:
Plasma emission spectrum (ICP) result shows, hafnium element mass percent is 90.05%, and sulphur carbon analyzer result shows, in sample, total carbon content is 6.08%, and free carbon content is 0.94%, and oxygen nitrogen analysis shows that in sample, oxygen level is 1.27%.This absolutely proves, has the feature of high purity, low oxygen content, low uncombined carbon with hafnium carbide prepared by this method.
Embodiment 2
Take 15g HfCl
4, 6.27g C
6h
8o
7h
2o (HfCl
4and C
6h
8o
7h
2o mol ratio is 1:0.64) put into 1000mL beaker, add 60mL deionized water, constantly stir with glass stick, make HfCl
4and C
6h
8o
7h
2o fully dissolves in deionized water, then adds appropriate NH with drop-burette
3h
2the pH of O solution regulator solution is 2-3, and carries out magnetic agitation process under 60 DEG C of constant temperature, and magnetic agitation speed is 60r/min, and churning time is 30min, obtains containing hafnium gel.To be placed in alumina crucible containing hafnium gel to put into the thermal treatment of low temperature tube furnace and obtain precursor powder, annealing process is be raised to 800 DEG C with the heat-up rate of 3 DEG C/min under room temperature, and insulation 1h, atmosphere is high-purity Ar, and Ar flow is 0.5L/min.Taken out by the precursor powder obtained after anneal, put into planetary type ball-milling tank, ball milling revolution 200r/min, rotation 400r/min, Ball-milling Time is 1 hour.Ball milling material is taken out, is placed in graphite jig, puts into discharge plasma sintering oven and synthesize, vacuum tightness is 10Pa, and with the ramp to 1800 DEG C of 200 DEG C/min under room temperature, soaking time is 10min, be cooled to room temperature with the speed of 100 DEG C/min again, grey powder 8.657g can be obtained.
Through XRD, FSEM and tem analysis, the present embodiment products therefrom is only containing a small amount of HfC, most of HfO
2not reaction, this illustrates that in reactant, C content is very few, and not having can complete reaction HfO
2, the median size of product is 600nm.Due to when colloidal sol, the amount that citric acid adds is very few, causes the carbon source of the presoma produced very few, and the carbon content of presoma is not enough, makes reaction incomplete.
Embodiment 3
Take 15g HfCl
4, 14.7g C
6h
8o
7h
2o (HfCl
4and C
6h
8o
7h
2o mol ratio is 1:1.5) put into 1000mL beaker, add 70mL deionized water, constantly stir with glass stick, make HfCl
4and C
6h
8o
7h
2o fully dissolves in deionized water, then adds appropriate NH with drop-burette
3h
2the pH of O solution regulator solution is 2-3, and carries out magnetic agitation process under 80 DEG C of constant temperature, and magnetic agitation speed is 80r/min, and churning time is 60min, obtains containing hafnium gel.To be placed in alumina crucible containing hafnium gel to put into the thermal treatment of low temperature tube furnace and obtain precursor powder, annealing process is be raised to 800 DEG C with the heat-up rate of 10 DEG C/min under room temperature, and insulation 3h, atmosphere is high-purity Ar, and Ar flow is 0.4L/min.Taken out by the precursor powder obtained after anneal, put into planetary type ball-milling tank, ball milling revolution 500r/min, rotation 250r/min, Ball-milling Time is 3 hours.Ball milling material is taken out, is placed in graphite jig, puts into discharge plasma sintering oven and synthesize, vacuum tightness is 10Pa, and with the ramp to 1500 DEG C of 400 DEG C/min under room temperature, soaking time is 3min, be cooled to room temperature with the speed of 200 DEG C/min again, grey powder 13.542g can be obtained.
Through XRD, FESEM and tem analysis, the present embodiment products therefrom is pure HfC powder, but because carbon hafnium is than excessive, uncombined carbons residual a large amount of in product, and uncombined carbon is wrapped in HfC particle, observe in FESEM and can see, hafnium carbide granular size is about 60nm.
Claims (5)
1. a preparation method for hafnium carbide nano-powder, is characterized in that step is as follows:
1) preparation is containing hafnium gel: by HfCl
4and C
6h
8o
7h
2o is dissolved in deionized water, HfCl
4be 0.20-0.25g/mL, wherein HfCl with the mass volume ratio of water
4and C
6h
8o
7h
2o mol ratio is 1:0.5-1.5, and constantly stirring makes it fully dissolve, and then regulates pH to 2-3 with ammonia soln, and 60-80 DEG C of constant temperature lower magnetic force stir process, obtains containing hafnium gel;
2) precursor powder is prepared: by step 1) gained puts into the thermal treatment of low temperature tube furnace containing hafnium gel, and with the ramp to 800 DEG C of 3-10 DEG C/min under room temperature, and be incubated 1-3h, atmosphere is Ar, obtains precursor powder;
3) hafnium carbide nano-powder is prepared: by step 2) gained precursor powder puts into planetary type ball-milling tank and carries out high-energy ball milling, gained powder is placed in discharge plasma sintering oven, under vacuum, under room temperature with the ramp of 200-400 DEG C/min to 1500-1800 DEG C, insulation 3-10min, then be cooled to room temperature with the speed of 100-200 DEG C/min and namely obtain hafnium carbide nano-powder.
2. the preparation method of hafnium carbide nano-powder according to claim 1, is characterized in that: step 1) described ammonia soln mass concentration is 25%.
3. the preparation method of hafnium carbide nano-powder according to claim 1, is characterized in that: step 1) described magnetic agitation speed is 60-80r/min, the magnetic agitation time is 30-60min.
4. the preparation method of hafnium carbide nano-powder according to claim 1, it is characterized in that: step 3) described high-energy-milling is: planetary type ball-milling tank revolution rotating speed is 200-250r/min, rotation rotating speed is 400-500r/min, and Ball-milling Time is 1-3h.
5. the preparation method of hafnium carbide nano-powder according to claim 1, it is characterized in that: step 3) described sintering process is: under vacuum, with the ramp to 1600 DEG C of 300 DEG C/min under room temperature, insulation 5min, then cool with the speed of 200 DEG C/min.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753477A (en) * | 2016-01-22 | 2016-07-13 | 中国人民解放军国防科学技术大学 | Preparation method and application of HfC ceramic precursor |
| CN105780123A (en) * | 2016-02-04 | 2016-07-20 | 武汉科技大学 | Hafnium-carbide nanometer whiskers and preparing method thereof |
| CN106588018A (en) * | 2016-11-15 | 2017-04-26 | 上海交通大学 | Method for preparing superhigh temperature carbonized hafnium ceramic nano-powder |
| CN107601508A (en) * | 2017-09-12 | 2018-01-19 | 江苏理工学院 | A kind of hafnium carbide nano material and preparation method thereof |
| WO2020133928A1 (en) * | 2018-12-23 | 2020-07-02 | 上海交通大学 | Preparation method for dense hfc(si)-hfb2 composite ceramics |
| CN113924270A (en) * | 2019-04-15 | 2022-01-11 | 中部电力株式会社 | Hafnium carbide powder for plasma electrode, method for producing same, hafnium carbide sintered body, and plasma electrode |
| CN115151358A (en) * | 2019-12-24 | 2022-10-04 | 俄罗斯国立科技大学莫斯科钢铁合金研究所 | Method for manufacturing ultrahigh-temperature ceramic material based on hafnium carbide and hafnium carbonitride |
| CN116854092A (en) * | 2023-07-28 | 2023-10-10 | 北京华威锐科化工有限公司 | Hafnium carbide precursor production system and preparation method |
| CN116835986B (en) * | 2023-06-15 | 2024-04-19 | 西北工业大学 | Method for preparing hafnium carbide ceramic by precursor conversion method and hafnium carbide of ceramic block material |
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| CN105753477A (en) * | 2016-01-22 | 2016-07-13 | 中国人民解放军国防科学技术大学 | Preparation method and application of HfC ceramic precursor |
| CN105753477B (en) * | 2016-01-22 | 2018-08-14 | 中国人民解放军国防科学技术大学 | A kind of preparation method of HfC ceramic precursors and application |
| CN105780123A (en) * | 2016-02-04 | 2016-07-20 | 武汉科技大学 | Hafnium-carbide nanometer whiskers and preparing method thereof |
| CN105780123B (en) * | 2016-02-04 | 2018-02-09 | 武汉科技大学 | A kind of hafnium carbide nano whisker and preparation method thereof |
| CN106588018A (en) * | 2016-11-15 | 2017-04-26 | 上海交通大学 | Method for preparing superhigh temperature carbonized hafnium ceramic nano-powder |
| CN107601508A (en) * | 2017-09-12 | 2018-01-19 | 江苏理工学院 | A kind of hafnium carbide nano material and preparation method thereof |
| WO2020133928A1 (en) * | 2018-12-23 | 2020-07-02 | 上海交通大学 | Preparation method for dense hfc(si)-hfb2 composite ceramics |
| US11180419B2 (en) | 2018-12-23 | 2021-11-23 | Shanghai Jiao Tong University | Method for preparation of dense HfC(Si)—HfB2 composite ceramic |
| CN113924270A (en) * | 2019-04-15 | 2022-01-11 | 中部电力株式会社 | Hafnium carbide powder for plasma electrode, method for producing same, hafnium carbide sintered body, and plasma electrode |
| CN115151358A (en) * | 2019-12-24 | 2022-10-04 | 俄罗斯国立科技大学莫斯科钢铁合金研究所 | Method for manufacturing ultrahigh-temperature ceramic material based on hafnium carbide and hafnium carbonitride |
| CN116835986B (en) * | 2023-06-15 | 2024-04-19 | 西北工业大学 | Method for preparing hafnium carbide ceramic by precursor conversion method and hafnium carbide of ceramic block material |
| CN116854092A (en) * | 2023-07-28 | 2023-10-10 | 北京华威锐科化工有限公司 | Hafnium carbide precursor production system and preparation method |
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