CN110042468A - A kind of preparation method of micrometer silicon carbide zirconium whisker - Google Patents
A kind of preparation method of micrometer silicon carbide zirconium whisker Download PDFInfo
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- CN110042468A CN110042468A CN201910275391.0A CN201910275391A CN110042468A CN 110042468 A CN110042468 A CN 110042468A CN 201910275391 A CN201910275391 A CN 201910275391A CN 110042468 A CN110042468 A CN 110042468A
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- whisker
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
Abstract
The present invention relates to a kind of preparation methods of micrometer silicon carbide zirconium whisker, using ZrO2- C (carbon black)-Ni-NaF is reaction system, will be sieved after above-mentioned precursor material ball milling first, carbothermic reduction reaction is then carried out under high temperature argon environment, most obtain the good zirconium carbide whisker of pattern through pickling impurity removal technique afterwards.The utility model has the advantages that the parameter that carbothermic reduction reaction method is related to is easily controllable, reliability of technology and reproducible.Process whole process is easy to operate, and step is succinct, and the period is shorter, low in cost, not high to equipment requirement, is suitable for batch production zirconium carbide whisker.It is about 1~3 μm using zirconium carbide diameter of whiskers prepared by process in the present invention, length is about 30~100 μm, and major diameter is bigger (20~50), and impurity is less, and pattern is good.The zirconium carbide whisker that in the present invention prepared by process can be used as the reinforced phase of superhigh temperature complex phase ceramic or ultra-temperature ceramic-based composite material, and it is tough that enhancing benefit is carried out to it.
Description
Technical field
The invention belongs to the preparation methods of zirconium carbide whisker, are related to a kind of preparation method of micrometer silicon carbide zirconium whisker, master
To be applied to ultra-temperature ceramic-based composite material reinforcement preparation field.
Background technique
Silicon carbide whisker (SiCW) as reinforcement it can meet wanting for high-modulus, high intensity and low thermal expansion rate simultaneously
It asks, is most widely used at present, technology of preparing one of Researches On Whiskers the most mature, by such as gel injection-moulding and material system can be increased
It the methods of makes preparation and forms porous preform, it is subsequent pre- at this using such as precursor infiltration and pyrolysis and chemical vapor deposition technique
Matched boundary layer and matrix are prepared in body processed and form ceramic matric composite.Silicon carbide whisker can be sent out in the composite
Good bearing capacity and crack deflection effect are waved, effective activeness and quietness is played the role of.But silicon carbide whisker heat-resisting ability
Deficiency may make made ceramic matric composite that high temperature failure easily occur, and limit ceramic matric composite in more wide temperature
The application of range.Zirconium carbide has class sodium chloride face-centred cubic structure, itself has high intensity, high rigidity, high-modulus, low-heat swollen
A series of excellent properties such as swollen rate, high temperature resistant, anti-ablation, anti-thermal shock.So zirconium carbide whisker has large development potentiality
Reinforcement material can be used for preparing the emerging ultra-temperature ceramic-based composite material with isotropism feature.
Typical zirconium carbide crystal whisker preparation method is mainly chemical vapour deposition technique (CVD), mostly uses ZrCl4-H2-CH4
(C3H6) it is reaction system, Ar is protection diluent gas, and Ni substrate provides catalyst, is had in 1100~1400 DEG C of preparations certain
The zirconium carbide whisker of draw ratio.Since preparation process is related to considerably complicated thermodynamical reaction and dynamic process, need
Technological parameter it is relatively more, equipment requirement is more harsh, therefore technology controlling and process difficulty is larger, reliability of technology and repeatability
It is not high, not yet realize small-scale batch production.NOBUYUKI TAMARI et al. is in document " Catalytic effect of
nickel on the growth of zirconium carbide whiskers by chemical vapor
Deposition " in use chemical vapour deposition technique, with ZrCl4-H2-CH4- Ar is reaction system, in different metal and fire resisting oxygen
Zirconium carbide whisker is prepared on compound substrate, finds Ni substrate and mullite (2Al2O3·SiO2) life of the substrate to zirconium carbide whisker
At the dissimilarity for advantageously, comparing influence of the two substrates for whisker growth.Generally speaking, using chemical vapor deposition system
There are limits throughput, periods to ask compared with long, regulation parameter is more, equipment requirement height, experimental error are relatively large etc. for standby zirconium carbide whisker
Topic needs to develop deficiency of the new process to make up prior art.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of preparation method of micrometer silicon carbide zirconium whisker,
The relatively short period, which can stablize batch preparation, has certain draw ratio, the process of the good zirconium carbide whisker of pattern.
Technical solution
A kind of preparation method of micrometer silicon carbide zirconium whisker, it is characterised in that steps are as follows:
Step 1, preparation raw material carry out ball milling: by ZrO2, carbon black, Ni, NaF powder mixing ball milling obtain it is uniformly mixed before
Drive body powder；The ZrO2, carbon black, Ni, NaF molar ratio be 1:3~5:0.1~0.3:0.1~0.9；Ball material when ball milling
Mass ratio is 3:1；
Step 2, sieving: presoma powder is subjected to 100 mesh sievings, obtains the consistent powder of uniform particle sizes；
Step 3, carbon thermal reduction: the powder that step 2 obtains is put into graphite crucible, and it is anti-that carbon thermal reduction is carried out in tube furnace
It answers, obtains zirconium carbide whisker；Reaction temperature: 1500 DEG C, soaking time: 2~4h, heating rate: 5K/min, atmosphere: Ar gas, stream
Amount: 20cc/min；Reaction prepares zirconium carbide whisker:
Step 4, pickling impurity removal: zirconium carbide whisker is put into progress magnetic agitation pickling 12h in sulfuric acid solution, is removed
ZrO2, Ni, NaF impurity, zirconium carbide whisker is dried.
Step 1 rotational speed of ball-mill is 70~90r/min, and the time is 4~7h.
Step 1 material molar ratio are as follows: ZrO2: C:Ni:NaF=1:3:0.2:0.1.
Step 1 material molar ratio are as follows: ZrO2: C:Ni:NaF=1:3:0.2:0.3.
Step 1 material molar ratio are as follows: ZrO2:C:Ni:NaF=1:4:0.2:0.3.
Step 1 material molar ratio are as follows: ZrO2:C:Ni:NaF=1:5:0.2:0.3.
The sulfuric acid solution is the sulfuric acid solution that mass fraction is 70%.
Beneficial effect
The preparation method of a kind of micrometer silicon carbide zirconium whisker proposed by the present invention, using ZrO2- C (carbon black)-Ni-NaF is anti-
System is answered, will be sieved after above-mentioned precursor material ball milling first, then carries out carbon heat also under high temperature argon environment
Original reaction, most obtains the good zirconium carbide whisker of pattern through pickling impurity removal technique afterwards.
Beneficial effects of the present invention include the following:
1, the parameter that carbothermic reduction reaction method is related to is easily controllable, reliability of technology and reproducible.Compared to chemical gas
Phase sedimentation does not need strictly to regulate and control the parameters such as pressure, intake method, gas flow.
2, process whole process proposed by the present invention is easy to operate, and step is succinct, and the period is shorter, low in cost, right
Equipment requirement is not high, is suitable for batch production zirconium carbide whisker.
It 3, is about 1~3 μm using zirconium carbide diameter of whiskers prepared by process in the present invention, length is about 30~100 μ
M, major diameter is bigger (20~50), and impurity is less, and pattern is good.
4, superhigh temperature complex phase ceramic can be used as using zirconium carbide whisker prepared by process in the present invention or superhigh temperature is made pottery
It is tough to carry out enhancing benefit to it for the reinforced phase of porcelain based composites.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 is scanning electron microscope (SEM) photo of 1 zirconium carbide whisker of the embodiment of the present invention.
Fig. 3 is selective electron diffraction (TEM) photo of 1 zirconium carbide whisker of the embodiment of the present invention.
Fig. 4 is X-ray diffraction (XRD) figure of 1 zirconium carbide whisker of the embodiment of the present invention.
Specific embodiment
Now in conjunction with embodiment, attached drawing, the invention will be further described:
Embodiment 1.
Step 1: preparation raw material carries out ball milling:
According to molar ratio ZrO2: C:Ni:NaF=1:3:0.2:0.1 preparation raw material 30g, according to ball material mass ratio=3:1,
Revolving speed 70r/min carries out ball milling, Ball-milling Time 5h.Obtain uniform presoma powder.
Step 2: sieving:
The presoma powder that step 1 is obtained carries out 100 mesh sievings, obtains the consistent powder of uniform particle sizes.
Step 3: carbon thermal reduction
The powder that 2g step 2 obtains is weighed, graphite crucible is put it into, carbothermic reduction reaction is carried out in tube furnace.Instead
Answer temperature: 1500 DEG C, soaking time: 4h, heating rate: 5K/min, atmosphere: Ar, Ar flow: 20cc/min, also using carbon heat
Former reaction prepares zirconium carbide whisker.
Step 4: pickling impurity removal
Prepare mass fraction be 70% sulfuric acid solution, by the zirconium carbide whisker that step 3 obtains be put into sulfuric acid solution into
Row stirring and pickling 12h removes ZrO2, the residual impurities such as Ni, NaF.Finally the zirconium carbide whisker after pickling is dried.
Embodiment 2.
Step 1: preparation raw material carries out ball milling:
According to molar ratio ZrO2: C:Ni:NaF=1:3:0.2:0.3 prepare ball milling raw material 30g, according to ball material mass ratio=
3:1, revolving speed 90r/min carry out ball milling, Ball-milling Time 4h.Obtain uniform presoma powder.
Step 2: sieving:
The presoma powder that step 1 is obtained carries out 100 mesh sievings, obtains the consistent powder of uniform particle sizes.
Step 3: carbon thermal reduction
The powder that 2g step 2 obtains is weighed, graphite crucible is put it into, carbothermic reduction reaction is carried out in tube furnace.Instead
Answer temperature: 1500 DEG C, soaking time: 4h, heating rate: 5K/min, atmosphere: Ar, Ar throughput: 20cc/min utilizes carbon heat
Reduction reaction prepares zirconium carbide whisker.
Step 4: pickling impurity removal
Prepare mass fraction be 70% sulfuric acid solution, by the zirconium carbide whisker that step 3 obtains be put into sulfuric acid solution into
Row stirring and pickling 12h removes ZrO2, the residual impurities such as Ni, NaF.Finally the zirconium carbide whisker after pickling is dried.
Embodiment 3.
Step 1: preparation raw material carries out ball milling:
According to molar ratio ZrO2:C:Ni:NaF=1:4:0.2:0.3 preparation raw material 30g, according to ball material mass ratio=3:1,
Revolving speed 90r/min carries out ball milling, Ball-milling Time 5h.Obtain uniform presoma powder.
Step 2: sieving:
The presoma powder that step 1 is obtained carries out 100 mesh sievings, obtains the consistent powder of uniform particle sizes.
Step 3: carbon thermal reduction
The powder that 2g step 2 obtains is weighed, graphite crucible is put into, carbothermic reduction reaction is carried out in tube furnace.Reaction temperature
Degree: 1500 DEG C, soaking time: 4h, heating rate: 5K/min, atmosphere: Ar, Ar throughput: 20cc/min utilizes carbon thermal reduction
Reaction prepares zirconium carbide whisker.
Ni
Step 4: pickling impurity removal
Prepare mass fraction be 70% sulfuric acid solution, by the zirconium carbide whisker that step 3 obtains be put into sulfuric acid solution into
Row stirring and pickling 12h removes the residual impurities such as ZrO2, Ni, NaF.Finally the zirconium carbide whisker after pickling is dried.
Embodiment 4.
Step 1: preparation raw material carries out ball milling
According to molar ratio ZrO2:C:Ni:NaF=1:5:0.2:0.3 prepare ball milling raw material 30g, according to ball material mass ratio=
3:1, revolving speed 80r/min carry out ball milling, Ball-milling Time 4h.Obtain uniform presoma powder.
Step 2: sieving
The presoma powder that step 1 is obtained carries out 100 mesh sievings, obtains the consistent powder of uniform particle sizes.
Step 3: carbon thermal reduction
The powder that 2g step 2 obtains is weighed, graphite crucible is put into, carbothermic reduction reaction is carried out in tube furnace.Reaction temperature
Degree: 1500 DEG C, soaking time: 4h, heating rate: 5K/min, atmosphere: Ar, Ar throughput: 20cc/min utilizes carbon thermal reduction
Reaction prepares zirconium carbide whisker.
Step 4: pickling impurity removal
Prepare mass fraction be 70% sulfuric acid solution, by the zirconium carbide whisker that step 3 obtains be put into sulfuric acid solution into
Row stirring and pickling 12h removes ZrO2, the residual impurities such as Ni, NaF.Finally the zirconium carbide whisker after pickling is dried.
Claims (7)
1. a kind of preparation method of micrometer silicon carbide zirconium whisker, it is characterised in that steps are as follows:
Step 1, preparation raw material carry out ball milling: by ZrO2, carbon black, Ni, NaF powder mixing ball milling obtain uniformly mixed presoma
Powder；The ZrO2, carbon black, Ni, NaF molar ratio be 1:3~5:0.1~0.3:0.1~0.9；The quality of ball material when ball milling
Than for 3:1；
Step 2, sieving: presoma powder is subjected to 100 mesh sievings, obtains the consistent powder of uniform particle sizes；
Step 3, carbon thermal reduction: the powder that step 2 obtains is put into graphite crucible, and carbothermic reduction reaction is carried out in tube furnace, is obtained
To zirconium carbide whisker；Reaction temperature: 1500 DEG C, soaking time: 2~4h, heating rate: 5K/min, atmosphere: Ar gas, flow:
20cc/min；
Step 4, pickling impurity removal: zirconium carbide whisker is put into progress magnetic agitation pickling 12h in sulfuric acid solution, removes ZrO2、Ni、
NaF impurity dries zirconium carbide whisker.
2. the preparation method of micrometer silicon carbide zirconium whisker according to claim 1, it is characterised in that: step 1 rotational speed of ball-mill
For 70~90r/min, the time is 4~7h.
3. the preparation method of micrometer silicon carbide zirconium whisker according to claim 1, it is characterised in that: step 1 feed molar
Than are as follows: ZrO2: C:Ni:NaF=1:3:0.2:0.1.
4. the preparation method of micrometer silicon carbide zirconium whisker according to claim 1, it is characterised in that: step 1 feed molar
Than are as follows: ZrO2: C:Ni:NaF=1:3:0.2:0.3.
5. the preparation method of micrometer silicon carbide zirconium whisker according to claim 1, it is characterised in that: step 1 feed molar
Than are as follows: ZrO2:C:Ni:NaF=1:4:0.2:0.3.
6. the preparation method of micrometer silicon carbide zirconium whisker according to claim 1, it is characterised in that: step 1 feed molar
Than are as follows: ZrO2:C:Ni:NaF=1:5:0.2:0.3.
7. the preparation method of micrometer silicon carbide zirconium whisker according to claim 1, it is characterised in that: the sulfuric acid solution is quality
The sulfuric acid solution that score is 70%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110592674A (en) * | 2019-10-15 | 2019-12-20 | 中国民航大学 | Micron-sized Cr3C2Preparation method of whisker |
| CN112195503A (en) * | 2020-09-24 | 2021-01-08 | 西北工业大学 | Method for synthesizing hafnium carbide crystal whisker with large length-diameter ratio by carbothermic reduction method |
| CN114959905A (en) * | 2022-03-07 | 2022-08-30 | 西北工业大学 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
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| CN102051676A (en) * | 2010-10-29 | 2011-05-11 | 山东大学 | In-situ grown tantalum carbide whisker material and preparation method thereof |
| CN106045549A (en) * | 2016-05-30 | 2016-10-26 | 西北工业大学 | Method using sol-gel method to synthesize spiral ZrC whiskers in in-situ manner |
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2019
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| CN102051676A (en) * | 2010-10-29 | 2011-05-11 | 山东大学 | In-situ grown tantalum carbide whisker material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110592674A (en) * | 2019-10-15 | 2019-12-20 | 中国民航大学 | Micron-sized Cr3C2Preparation method of whisker |
| CN112195503A (en) * | 2020-09-24 | 2021-01-08 | 西北工业大学 | Method for synthesizing hafnium carbide crystal whisker with large length-diameter ratio by carbothermic reduction method |
| CN112195503B (en) * | 2020-09-24 | 2022-07-26 | 西北工业大学 | Method for synthesizing hafnium carbide crystal whisker with large length-diameter ratio by carbothermic reduction method |
| CN114959905A (en) * | 2022-03-07 | 2022-08-30 | 西北工业大学 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
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Application publication date: 20190723 |