CN107161962A - The preparation method and beta-silicon nitride nanowire of a kind of beta-silicon nitride nanowire - Google Patents
The preparation method and beta-silicon nitride nanowire of a kind of beta-silicon nitride nanowire Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of beta-silicon nitride nanowire and beta-silicon nitride nanowire, belong to technical field of nanometer material preparation.Wherein, preparation method comprises the following steps：As catalyst precursor, it will be put into containing one or more of binary in Fe, Co, Ni, Cu and Mo, ternary or quaternary layer dihydroxy metal hydroxides (LDH) after uniformly being mixed with silica flour in reactor；Mixture is warming up to pretreatment temperature under the protection of carrier gas, pre-processed with hydrogen；Pretreatment temperature is maintained, the gas containing nitrogen source is passed through in the reactor, nitridation reaction, by chemical vapor deposition processes, the grown silicon nitride nano wire on LDH is carried out；The product obtained after chemical vapor deposition is purified, beta-silicon nitride nanowire is obtained.Diameter, length and the appearance of effectively control beta-silicon nitride nanowire of the invention, yield are high.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, the preparation method and nitrogen of more particularly to a kind of beta-silicon nitride nanowire
SiClx nano wire.
Background technology
Silicon nitride Si3N4It is a kind of high temperature resistant, oxidation resistant high performance structure ceramic, while being also that a kind of broad-band gap is partly led
Body, can be in normal temperature and high-temperature field conduct with broad-band gap, high intensity, high rigidity, excellent thermal shock resistance and inoxidizability
Excellent semi-conducting material application.Si3N4Nano wire is the one-dimensional nano structure form of silicon nitride material, and it both has block material
The various excellent properties possessed are expected, while possessing many new characteristics as monodimension nanometer material.For example：Si3N4Nanometer
The bending strength (reaching 3.6GPa) of line is far above block materials with elastic model (reaching 570GPa), and with fabulous pliability,
It is a kind of excellent composite material reinforcement body.
At present, Si is prepared3N4The method of nano wire is more：Direct nitridation method, carbothermic method, chemical vapour deposition technique, combustion
Burn reaction method, organic precursor pyrolysismethod, solvent-thermal method, template etc..In preparation process, metal is introduced into reaction system
Catalyst, can not only increase reaction rate, improve feed stock conversion, can also effectively reduce reaction temperature, regulation and control nano wire
Appearance structure, thus be all widely adopted in different preparation methods.For example：Huang etc. is using silica flour as raw material, micron order Fe
Powder is catalyst, nitrogenizes the silicon nitride nano band for being prepared for d=300~1700nm at 1450 DEG C using chemical vapour deposition technique
With nano wire (Huang J et.al, Scientific reports, 2013,3:3504.).Gu etc. is deposited on Si powder surface
Co nano particles are as catalyst, and nitridation 2h is prepared for a diameter of 80~320nm at 1200-1400 DEG C, about 10 μm of length
Si3N4Nano wire (Gu Y et al.Journal of the American Ceramic Society, 2015,98 (6):
1762-1768.)。
However, using the Si prepared by metallic catalyst3N4Nano wire often exist diameter have a very wide distribution (50~
1000nm) and the problem of average diameter relatively thick (100~500nm) so that prepared Si3N4Relatively low (the ＜ of nano wire draw ratio
100).This is mainly due to conventional loaded catalyst, and the interaction force between its carrier and metallic catalyst is weaker,
And the method such as dipping, ion exchange, the co-precipitation taken in preparation process, easily cause the scattered inequality of catalyst.Therefore, exist
Si3N4In the preparation process of nano wire, easily migration occurs the metallic catalyst on carrier for (1100-1500 DEG C) simultaneously at high temperature
Coalescence is further sintered so that metal catalyst particles diameter significantly becomes big and skewness, so as to cause prepared Si3N4
There is also this problem for nano wire.
Layer dihydroxy metal hydroxides (Layered Double Hydroxide, be abbreviated as LDH) is one kind by band
The laminate of positive charge has similar shepardite Mg (OH) with interlayer anion ordered fabrication2The two-dimensional nano material of structure
Material.LDH general expression is：M2+ 1-xM3+ x(OH)2An- x/n·mH2O, wherein M2 +And M3 +Divalence and trivalent metal are represented respectively
Cation；An -Represent interlayer anion；X is M3 +/(M2 ++M3 +) molar ratio, m be interlayer hydrone number.Section snow etc.
(patent publication No.：CN1718278) using catalyst of the layer dihydroxy metal hydroxides as carbon nano tube growth, find
Can with growth diameter 20~50nm agglomerate shape multi-walled carbon nanotube.(the patent publication No.s such as Wei Fei：) etc. CN101665248 adopt
With layer dihydroxy metal hydroxides as catalyst, single double-walled carbon nano-tube of the diameter in 3~5nm is prepared for.Inventor
Early stage finding shows, at home and abroad there is no and prepares one-dimensional Si based on LDH3N4The Patents and document report of nano material
Road.Based on this, the present invention is intended to provide a kind of prepare Si based on layer dihydroxy metal hydroxides3N4The method of nano wire, from
And abundant preparation Si3N4The catalyst type of nano wire, promotes Si3N4The application study of nano wire.
The content of the invention
It is existing to solve the embodiments of the invention provide a kind of preparation method of beta-silicon nitride nanowire and beta-silicon nitride nanowire
There is the silicon nitride nano linear diameter for preparing in technology to have a very wide distribution and the problem of average diameter is thick.In order to disclosure
Some aspects of embodiment have a basic understanding, shown below is simple summary.The summarized section is not extensive overview,
Nor to determine key/critical component or describe the protection domain of these embodiments.Its sole purpose is with simple
Some concepts are presented in form, in this, as the preamble of following detailed description.
First aspect according to embodiments of the present invention there is provided a kind of preparation method of beta-silicon nitride nanowire,
In some exemplary embodiments, the preparation method of beta-silicon nitride nanowire comprises the following steps：
1) by containing one or more of binary in Fe, Co, Ni, Cu and Mo, ternary or quaternary layer dihydroxy metallic hydrogen
Oxide LDH is put into reactor as catalyst precursor after uniformly being mixed with silicon Si powder；
2) mixture is warming up to pretreatment temperature under the protection of carrier gas, pre-processed with hydrogen；
3) pretreatment temperature is maintained, the gas containing nitrogen source is passed through in the reactor, nitridation reaction is carried out, passes through chemical gaseous phase
Deposition process, the grown silicon nitride Si on LDH3N4Nano wire；
4) product obtained after chemical vapor deposition is purified, obtains Si3N4Nano wire.
Above embodiments describe and prepare Si using LDH3N4The technological process of nano wire, and indicate LDH should be containing Fe,
One or more of binary, ternary or quaternary LDH in Co, Ni and Mo.In experimentation, several metals containing more than are found
The LDH of element catalytic effect is good, the Si prepared3N4Nano wire is directly thin and distribution is homogeneous, better than other common metal elements
Such as Ca, Mn and Cu.
Further, carrier gas is one or both of argon gas and helium mixture.
In some optional embodiments,
LDH chemical composition formula is M2+ 1-xM3+ x(OH)2An- x/n·mH2O；Wherein, M2+With M3+Molar ratio for 1~
4, x be M3+With (M2++M3+) molar ratio；M is the number of interlayer hydrone；M2+For Mg2+、Fe2+、Co2+、Ni2+One with
Plant or several, M3+For Al3+、Co3+、Fe3+, in one or more, An-For n valency anion, corresponding anion is Cl-、OH-、
NO3-、SO4 2-And CO3 2-In one or more, corresponding anion also includes isopolyacid containing Mo or heteropolyacid anions；
Fe, Co, Ni, Cu or Mo account for the 0.1~30% of LDH mass.
It is preferred that, Fe, Co, Ni, Cu or Mo account for 10%, 15% and the 25% of LDH mass.
In order to further be optimized to LDH, LDH selection details, including different prices gold are above embodiments described
Belong to the information such as ratio, the range of choice of metallic element, the range of choice of anion of element.And disclose metallic element Fe, Co,
Ni, Cu or Mo account for the optimum valuing range of LDH mass.Further effectively implement the present invention for technical staff and preferred LDH side is provided
Case.
Wherein, in LDH, metal active constituent is evenly distributed in main layer board on atom level, can be by coprecipitated
Shallow lake method prepares the catalyst precursor.
In some optional embodiments, in the mixture, the mass ratio of LDH and Si powder is 0.01~0.1.
It is preferred that, the mass ratio of LDH and Si powder is 0.01,0.05,0.1.
Further, the particle diameter of Si powder is 0.1~100 μm, and purity is 99.5~99.998%.
In some optional embodiments, pretreatment temperature is 1000~1400 DEG C；The time of pretreatment be 10~
20min。
It is preferred that, pretreatment temperature is 1100 DEG C, 1150 DEG C, 1200 DEG C, 1250 DEG C and 1300 DEG C.
In some optional embodiments, the gas containing nitrogen source also contains hydrogen；Wherein, hydrogen：The gas volume of nitrogen source
Than less than or equal to 1.
In some optional embodiments, during mixture is warming up into pretreatment temperature, heating rate control
In 1~20 DEG C/min.
In some optional embodiments, nitrogen source is the mixture of one or both of nitrogen, ammonia.
In some optional embodiments, reactor use fixed bed, moving bed, fluid bed or combinations thereof.
Second aspect according to embodiments of the present invention there is provided a kind of beta-silicon nitride nanowire,
In some exemplary embodiments, Si3N4Nano wire is prepared according to the preparation method of any of the above-described embodiment
, catalyst precursor is used as using layer dihydroxy metal hydroxides LDH.
In some optional embodiments, Si3N4A diameter of 30~50nm of nano wire；Si3N4Nano wire draw ratio is more than
1000。
Although having patent at present and document disclosing and prepares CNT using LDH, application mechanism is not equivalent
It is not approximate.During CNT is prepared, reaction temperature is generally less than 900 DEG C, nano-metal particle migration group thereon
It is poly- relatively light, therefore prepared carbon nanotube diameter is homogeneous, and growth mechanism is vapour-liquid-solid growth mechanism.And utilized in the present invention
LDH prepares Si3N4Temperature range at 1110-1300 DEG C, close to nano metal Fe, Ni etc. fusing point, the migration of nano metal
Reunite and volatilize even more serious, and there is a certain degree of volatilization, thus needed in course of reaction strict controlling reaction temperature,
The migration that LDH compositions could suppress nano metal is reunited, Si3N4The growth mechanism of nano wire is gas-liquid-solid and gas-liquid mechanism coexistence.
Technical scheme provided in an embodiment of the present invention can include the following benefits：
The present invention can be by controlling the component and size of reaction condition and LDH effectively to control Si3N4Nano wire it is straight
Footpath, length and appearance, and yield is higher.Wherein, Si3N4The controlled diameter system of nano wire is to 30~50nm, Si3N4Nanometer line length
Footpath ratio is more than 1000.The LDH that is used in technical scheme, nitrogen source are cheap and easy to get, are easy to engineering to amplify and produce in batches, are Si3N4
The mass production of nano wire is laid a good foundation.
It should be appreciated that the general description of the above and detailed description hereinafter are only exemplary and explanatory, not
Can the limitation present invention.
Brief description of the drawings
Accompanying drawing herein is merged in specification and constitutes the part of this specification, shows the implementation for meeting the present invention
Example, and for explaining principle of the invention together with specification.
The stereoscan photograph of Fig. 1 Fe/Mg/Al LDH ternary hydrotalcite class intercalation materials.
The X-ray diffraction (XRD, X-ray diffraction) of Fig. 2 Fe/Mg/Al LDH ternary hydrotalcite class intercalation materials
Spectrogram.
Fig. 3 Fe/Mg/Al LDH are as catalyst precursor, with N2For nitrogen source, the Si prepared using the method for the present invention3N4
The typical low power stereoscan photograph at nanowire growth initial stage.
Fig. 4 Fe/Mg/Al LDH are as catalyst precursor, with N2For nitrogen source, the Si prepared using the method for the present invention3N4
Typical low power stereoscan photograph after nano wire is purified.
Fig. 5 Fe/Mg/Al LDH are as catalyst precursor, with N2For nitrogen source, the Si prepared using the method for the present invention3N4
XRD spectra after nano wire is purified
Fig. 6 Fe/Mg/Al LDH are as catalyst precursor, with N2For nitrogen source, the Si prepared using the method for the present invention3N4
The typical transmission electromicroscopic photograph of nano wire.
Fig. 7 is as catalyst precursor, with N with Fe/Mg/Al LDH2For nitrogen source, prepared using the method for the present invention
Si3N4The typical high-resolution-ration transmission electric-lens photo of nano wire.
Embodiment
The following description and drawings fully show specific embodiments of the present invention, to enable those skilled in the art to
Put into practice them.
Embodiment 1：Based on Fe/Mg/Al LDH, Si is prepared in fixed bed3N4Nano wire.
Be 2.5% by Fe contents, Fe, Mg, Al atomic ratio for 0.1: 2: 1 Fe/Mg/Al LDH as catalyst,
50mg is taken to be placed in after uniformly being mixed with 1g silica flours in tubular fixed-bed reactor.The catalyst pattern is referring to Fig. 1, it is known that its is main
Structure is uniform sheet hexagon.Fig. 2 XRD spectra shows that the catalyst is typical layer dihydroxy metal hydroxides
Structure, its crystallinity is high.The use of argon gas is carrier gas, its flow is 1000sccm.With 10 DEG C/min heating speed under the atmosphere
Temperature of reactor is raised to 1150 DEG C of pretreatment temperature by rate by room temperature, then passes to 1sccm H2Carry out pretreatment 10min；It
Reaction temperature is maintained 1150 DEG C afterwards, the gaseous mixture for being passed through nitrogen and hydrogen carries out nitridation reaction, wherein nitrogen：The body of hydrogen
Product is than being 1000：1, total gas flow rate is 1000sccm, carries out chemical vapor deposition processes.Reaction gas is closed after 2h, in argon gas
It is cooled under atmosphere after room temperature and takes out solid product.Fig. 3 is to nitrogenize after 20min with Si3N4The LDH patterns of nano wire, Fig. 4 is
Si3N4Product morphology after nano wire is purified, understands nanowire diameter in 30-50nm, length is 20-100 μm from figure.Fig. 5 is
Si after purification3N4The XRD spectrum of nano wire, as a result shows that nano wire purity is higher, (is more than 95%) based on а phases, containing few
Measure β phases.Fig. 6 and Fig. 7 is Si3N4The TEM photos and high resolution scanning electromicroscopic photograph of nano wire, it can be seen that prepared
Si3N4Unformed SiO on the outside of nano wire2Layer, crystallinity is good.
Embodiment 2：Based on Fe/Mg/Al LDH, Si is prepared in fluid bed3N4Nano wire.
It is 10% by Fe contents, the Fe/Mg/Al LDH that Fe, Mg, Al atomic ratio are 0.4: 2: 1 take as catalyst
0.5g is placed in corundum fluidized-bed reactor after uniformly being mixed with 5g silica flours.The use of argon gas is carrier gas, its flow is 2000sccm.
Temperature of reactor is raised to by room temperature by 1250 DEG C of pretreatment temperature with 20 DEG C/min heating rate under the atmosphere, then passed to
5sccm H2Carry out pretreatment 10min；Reaction temperature is maintained 1250 DEG C afterwards, nitrogen is passed through and carries out nitridation reaction, gas
Total flow is 2000sccm, carries out chemical vapor deposition processes.Nitrogen is closed after 1h, is cooled to after room temperature and takes under an argon atmosphere
Go out solid product, obtain being grown in the Si on flaky material surface3N4Nano wire.
Embodiment 3：Based on Fe/Mg/Al-Mo LDH, Si is prepared in fixed bed3N4Nano wire.
It is 2.5% by Fe contents, Mo, Fe, Mg, Al atomic ratio are 0.01：0.1: 2: 1 Fe/Mg/Al LDH conducts
Catalyst, takes 100mg to be placed in after uniformly being mixed with 1g silica flours in tubular fixed-bed reactor.The use of helium is carrier gas, its flow
For 500sccm.Temperature of reactor is raised to by pretreatment temperature 1200 by room temperature with 20 DEG C/min heating rate under the atmosphere
DEG C, then pass to 1sccm H2Carry out pretreatment 20min；Reaction temperature is maintained 1200 DEG C afterwards, nitrogen and hydrogen is passed through
Gaseous mixture carry out nitridation reaction, wherein nitrogen：The volume ratio of hydrogen is 500：1, total gas flow rate is 1000sccm, is changed
Learn vapor deposition processes.Reaction gas is closed after 3h, obtains being grown in the Si on flaky material surface3N4Nano wire.
Embodiment 4：Based on Fe/Mg/Al LDH, Si is prepared in fixed bed3N4Nano wire
It is 5% by Fe contents, the Fe/Mg/Al LDH that Fe, Mg, Al atomic ratio are 0.2: 2: 1 take as catalyst
10mg is placed in tubular fixed-bed reactor after uniformly being mixed with 1g silica flours.The use of argon gas is carrier gas, its flow is 600sccm.
Temperature of reactor is raised to by room temperature by 1150 DEG C of pretreatment temperature with 15 DEG C/min heating rate under the atmosphere, then passed to
2sccm H2Carry out pretreatment 10min；Reaction temperature is maintained 1150 DEG C afterwards, ammonia is passed through and carries out nitridation reaction, gas
Total flow is 1000sccm, carries out chemical vapor deposition processes.Reaction gas is closed after 4h, is cooled under an argon atmosphere after room temperature
Solid product is taken out, obtains being grown in the Si on flaky material surface3N4Nano wire.
Embodiment 5：Based on Co/Mg/Al LDH, Si is prepared in fixed bed3N4Nano wire.
It is 2.5% by Co contents, Mo, Fe, Mg, Al atomic ratio are 0.01：0.1: 2: 1 Co/Mg/Al LDH conducts
Catalyst, takes 100mg to be placed in after uniformly being mixed with 1g silica flours in tubular fixed-bed reactor.The use of helium is carrier gas, its flow
For 500sccm.Temperature of reactor is raised to by pretreatment temperature 1300 by room temperature with 20 DEG C/min heating rate under the atmosphere
DEG C, then pass to 1sccm H2Carry out pretreatment 20min；Reaction temperature is maintained 1300 DEG C afterwards, nitrogen and hydrogen is passed through
Gaseous mixture carry out nitridation reaction, wherein nitrogen：The volume ratio of hydrogen is 500：1, total gas flow rate is 1000sccm, is changed
Learn vapor deposition processes.Reaction gas is closed after 3h, obtains being grown in the Si on flaky material surface3N4Nano wire.
Embodiment 6：Based on Ni/Mg/Al LDH, Si is prepared in fixed bed3N4Nano wire.
It is 10% by Ni contents, the Ni/Mg/Al LDH that Ni, Mg, Al atomic ratio are 0.4: 2: 1 take as catalyst
50mg is placed in tubular fixed-bed reactor after uniformly being mixed with 1g silica flours.The use of argon gas is carrier gas, its flow is 750sccm.
Temperature of reactor is raised to by room temperature by 1100 DEG C of pretreatment temperature with 20 DEG C/min heating rate under the atmosphere, then passed to
1sccm H2Carry out pretreatment 20min；Reaction temperature is maintained 1100 DEG C afterwards, the gaseous mixture for being passed through nitrogen and hydrogen enters
Row nitridation reaction, wherein nitrogen：The volume ratio of hydrogen is 1000：1, total gas flow rate is 1000sccm, carries out chemical vapor deposition
Product process.Reaction gas is closed after 3h, obtains being grown in the Si on flaky material surface3N4Nano wire.
The not Si prepared in be the same as Example of table 13N4The quality of nano wire
| Diameter (nm) | Length (μm) | Draw ratio | |
| Embodiment 1 | 30-50 | 20-100 | 1000-5000 |
| Embodiment 2 | 30-50 | 30-80 | 1000-1500 |
| Embodiment 3 | 20-40 | 10-100 | 2000-8000 |
| Embodiment 4 | 15-30 | 50-100 | 5000-10000 |
| Embodiment 5 | 20-40 | 40-150 | 2000-5000 |
| Embodiment 6 | 30-60 | 30-80 | 1000-2000 |
As known from Table 1, Si prepared in all embodiments3N4Wire diameter distribution is homogeneous, and draw ratio is more than 1000.
The present invention can be by controlling the component and size of reaction condition and LDH effectively to control Si3N4The diameter of nano wire, length with
Appearance, and yield is higher.Wherein, Si3N4The controlled diameter system of nano wire is to 30~50nm, Si3N4Nano wire draw ratio is more than
1000.The LDH that is used in technical scheme, nitrogen source are cheap and easy to get, are easy to engineering to amplify and produce in batches, are Si3N4Nano wire
Mass production is laid a good foundation.
It should be appreciated that the invention is not limited in the flow and structure for being described above and being shown in the drawings,
And various modifications and changes can be being carried out without departing from the scope.The scope of the present invention is only limited by appended claim
System.
Claims (10)
1. a kind of preparation method of beta-silicon nitride nanowire, it is characterised in that comprise the following steps：
1) by containing one or more of binary in Fe, Co, Ni, Cu and Mo, ternary or quaternary layer dihydroxy metal hydroxide
Thing LDH is put into reactor as catalyst precursor after uniformly being mixed with silicon Si powder；
2) mixture is warming up to pretreatment temperature under the protection of carrier gas, pre-processed with hydrogen；
3) pretreatment temperature is maintained, the gas containing nitrogen source is passed through in the reactor, nitridation reaction is carried out, passes through chemical vapor deposition
Process, the grown silicon nitride Si on LDH3N4Nano wire；
4) product obtained after chemical vapor deposition is purified, obtains Si3N4Nano wire.
2. preparation method as claimed in claim 1, it is characterised in that
LDH chemical composition formula is M2+ 1-xM3+ x(OH)2An- x/n·mH2O；Wherein, M2+With M3+Molar ratio be for 1~4, x
M3+With (M2++M3+) molar ratio；M is the number of interlayer hydrone；M2+For Mg2+、Fe2+、Co2+、Ni2+One kind with or
It is several, M3+For Al3+、Co3+、Fe3+, in one or more, An-For n valency anion, corresponding anion is Cl-、OH-、NO3-、
SO4 2-And CO3 2-In one or more, corresponding anion also includes isopolyacid containing Mo or heteropolyacid anions；
Fe, Co, Ni, Cu or Mo account for the 0.1~30% of LDH mass.
3. the mass ratio of preparation method as claimed in claim 1, it is characterised in that in the mixture, LDH and Si powder is 0.01~1.
4. preparation method as claimed in claim 1, it is characterised in that pretreatment temperature is 1000~1400 DEG C；The time of pretreatment
For 10~20min.
5. preparation method as claimed in claim 1, its characteristic is, the gas containing nitrogen source also contains hydrogen；Wherein, hydrogen：Nitrogen source
Gas volume ratio be less than or equal to 1.
6. preparation method as claimed in claim 1, it is characterised in that during mixture is warming up into pretreatment temperature, rises
Warm speed control is in 1~20 DEG C/min.
7. preparation method as claimed in claim 1, it is characterised in that nitrogen source is the mixture of one or both of nitrogen, ammonia.
8. such as any one of claim 1-7 preparation method, it is characterised in that reactor uses fixed bed, moving bed, fluidisation
Bed or combinations thereof.
9. a kind of beta-silicon nitride nanowire, it is characterised in that silicon nitride Si3N4Nano wire is as claimed in one of claims 1-9
Prepared by preparation method, catalyst precursor is used as using layer dihydroxy metal hydroxides LDH.
10. beta-silicon nitride nanowire as claimed in claim 9, it is characterised in that Si3N4A diameter of 30~50nm of nano wire；Si3N4Receive
Rice noodles draw ratio is more than 1000.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710524203.4A CN107161962B (en) | 2017-06-30 | 2017-06-30 | A kind of preparation method and beta-silicon nitride nanowire of beta-silicon nitride nanowire |
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| CN201710524203.4A CN107161962B (en) | 2017-06-30 | 2017-06-30 | A kind of preparation method and beta-silicon nitride nanowire of beta-silicon nitride nanowire |
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| Publication Number | Publication Date |
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| CN107161962A true CN107161962A (en) | 2017-09-15 |
| CN107161962B CN107161962B (en) | 2019-02-22 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110436934A (en) * | 2019-07-09 | 2019-11-12 | 南昌大学 | A kind of preparation method of alpha-phase silicon nitride powder, overlength beta-silicon nitride nanowire |
| CN110484998A (en) * | 2019-07-09 | 2019-11-22 | 南昌大学 | A kind of preparation method of overlength silica cladding beta-silicon nitride nanowire |
| CN112607715A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of high-purity alpha-phase silicon nitride nanowire |
| CN115151512A (en) * | 2020-03-02 | 2022-10-04 | 日本碍子株式会社 | Layered double hydroxide, method for producing same, and air electrode and metal-air secondary battery using same |
| CN116535238A (en) * | 2023-04-27 | 2023-08-04 | 西北工业大学 | Radial SiC nanowire grown on surface of one-dimensional micro-nano silicon-based ceramic substrate in situ and preparation method |
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| CN101665248A (en) * | 2009-09-11 | 2010-03-10 | 清华大学 | Method for preparing single-walled and double-walled carbon nanotubes based on layered dihydroxy metal hydroxide |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110436934A (en) * | 2019-07-09 | 2019-11-12 | 南昌大学 | A kind of preparation method of alpha-phase silicon nitride powder, overlength beta-silicon nitride nanowire |
| CN110484998A (en) * | 2019-07-09 | 2019-11-22 | 南昌大学 | A kind of preparation method of overlength silica cladding beta-silicon nitride nanowire |
| CN110436934B (en) * | 2019-07-09 | 2022-02-11 | 南昌大学 | Preparation method of high alpha-phase silicon nitride powder and ultra-long silicon nitride nanowire |
| CN115151512A (en) * | 2020-03-02 | 2022-10-04 | 日本碍子株式会社 | Layered double hydroxide, method for producing same, and air electrode and metal-air secondary battery using same |
| CN115151512B (en) * | 2020-03-02 | 2024-02-06 | 日本碍子株式会社 | Layered double hydroxide, method for producing same, and air electrode and metal-air secondary battery using same |
| CN112607715A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of high-purity alpha-phase silicon nitride nanowire |
| CN112607715B (en) * | 2020-12-29 | 2021-12-10 | 哈尔滨工业大学 | Preparation method of high-purity alpha-phase silicon nitride nanowire |
| CN116535238A (en) * | 2023-04-27 | 2023-08-04 | 西北工业大学 | Radial SiC nanowire grown on surface of one-dimensional micro-nano silicon-based ceramic substrate in situ and preparation method |
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