CN1272244C - B6O nanowire and crystal whisker structure and its preparation method - Google Patents
B6O nanowire and crystal whisker structure and its preparation method Download PDFInfo
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- CN1272244C CN1272244C CN 200410009238 CN200410009238A CN1272244C CN 1272244 C CN1272244 C CN 1272244C CN 200410009238 CN200410009238 CN 200410009238 CN 200410009238 A CN200410009238 A CN 200410009238A CN 1272244 C CN1272244 C CN 1272244C
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- yttrium
- magnesium
- nano wire
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002070 nanowire Substances 0.000 title claims description 41
- 239000013078 crystal Substances 0.000 title abstract description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 20
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 31
- 238000005469 granulation Methods 0.000 claims description 16
- 230000003179 granulation Effects 0.000 claims description 16
- 238000007669 thermal treatment Methods 0.000 claims description 16
- 229910052723 transition metal Inorganic materials 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 15
- 229910052742 iron Inorganic materials 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- QYHKLBKLFBZGAI-UHFFFAOYSA-N boron magnesium Chemical compound [B].[Mg] QYHKLBKLFBZGAI-UHFFFAOYSA-N 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 238000007747 plating Methods 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract 2
- 239000012071 phase Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 229960000935 dehydrated alcohol Drugs 0.000 description 15
- 229910052796 boron Inorganic materials 0.000 description 11
- 239000000843 powder Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000002003 electron diffraction Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000619 electron energy-loss spectrum Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a B60 nanometer line and crystal whisker structure, and a preparing method thereof, which belongs to the technical field of ceramic material preparation. A solid phase reaction method and a chemical gas phase deposition method are adopted; in the preparation, metallic oxide in the IIA group, boron powder, and transition group metal or metallic oxide thereof are used as initial raw materials, wherein the quality ratio of the transition group metal or the metallic oxide thereof is controlled between 20% and 70%; the proportion of the metallic oxide in the IIA family is controlled between 10% and 50%; after the initial raw materials are mixed, the mixed materials are pressed into test pieces under the pressure of 2 to 10MPa; after being granulated, the test pieces are sieved; and in Ar gas and at a temperature of 1350 to 1500 DEG C, the heat treatment is performed. Through regulating the proportion of the raw materials, B6O nanometer lines with 20 nm to 600 nm of diameters can be prepared; B6O crystal whisker materials can be prepared by the method, and the yield and the purify are high. After samples are extracted, the shape of the prepared nanometer line is observed in a scanning electron microscope to find that the prepared B6O nanometer line has good uniformity.
Description
Technical field
The present invention relates to a kind of B
6O nano wire and whisker structure and preparation method thereof belong to ceramic materials preparation technology field.
Background technology
Boride material has the high characteristics of high-melting-point, high strength and chemical stability, wherein many also have special functional, as: low electronic work function, more constant than resistance, in certain temperature range the thermal expansion value be zero, dissimilar magnetic order and high neutron uptake factor etc.These high-performances determine it to have wide practical use in the various device constituent elements of modern technologies, and many countries have carried out the research of such material in succession.Because such material also has other outstanding performance, as chemistry, electricity and thermal property etc., the unusual physicals that especially this type of material showed more makes boride material become the interested material system of researchist.Object lesson is as ZrB
2TiB
2The good electric of performance is led and the thermal conductance characteristic, and its electricity is led with thermal conductivity and exceeded more than the magnitude than parent metal; Fusing point exceeds 1000 ℃ than parent metal; The thermionic emission character of the excellence that rare-earth hexboride compound showed; Phosphorus boride and arsenic boride then may be a kind of high temperature semiconductors materials with potential use; And AsB
6Or the ballistic material of a kind of good chemically-resistant; In addition, the hardness of BN cubic structure even be better than diamond, MgB
2Be the high temperature superconducting materia of discovered in recent years, its Curie-point temperature is up to 39K.So the physicals of the many novelties of boride material becomes the very interested material of researchist.
B
6O is the boride material that a class has a lot of potential application.The hardness of this material can match in excellence or beauty with diamond; Its Vickers' hardness of bibliographical information can reach 45GPa.In addition, this material may have semiconductor property, so, can be used as optics or electricity original paper raw material.B
6The preparation of O block materials is mainly adopted under the High Temperature High Pressure and is prepared, and its mould material mainly adopts sputter or chemical Vapor deposition process preparation.Up to now, the B that does not also possess nano wire or whisker structure
6The report of O material preparation.
Summary of the invention
The purpose of this invention is to provide a kind of technology simple (need not high pressure), low, the workable preparation B of production cost
6O nano wire and whisker structure material and preparation method thereof.In this method, we are by the variation of proportion scheme, and the adjustment of sintering schedule can be implemented in synthetic B under the lesser temps
6O nano thread structure, and controllable diameter.
A kind of preparation B that the present invention proposes
6The method of O nano wire or whisker structure adopts solid phase reaction method, it is characterized in that: material adopts IIA family metal oxide, boron powder and magnesium-yttrium-transition metal or its metal oxide among the described preparation method; Wherein the mass ratio of magnesium-yttrium-transition metal or its metal oxide is controlled at 20%～70%, and IIA family metal oxide ratio control is 10%～50%, and the ratio of boron powder is 20～70%; Described IIA family metal oxide is CaO, SrO or BaO, and described magnesium-yttrium-transition metal or its metal oxide are Fe, Co, Ni or Fe
3O
4, Fe
2O
3, CoO, NiO; Its concrete steps are:
(1) starting raw material is mixed, behind wet ball grinding, oven dry adds tackiness agent, granulation;
(2) material after the above-mentioned granulation is made sheet under the pressure of 2～10MPa;
(3) material step (2) compacting is in blocks is in Ar atmosphere, heat-treats insulation 1h～8h under 1300～1500 ℃.
A kind of preparation B that the present invention proposes
6The method of O nano wire or whisker structure adopts chemical Vapor deposition process, it is characterized in that: material adopts IIA family metal oxide, boron powder and magnesium-yttrium-transition metal or its metal oxide among the described preparation method; Wherein the mass ratio of magnesium-yttrium-transition metal or its metal oxide is controlled at 20%～70%, and IIA family metal oxide ratio control is 10%～50%, and the ratio of boron powder is 20～70%; Described IIA family metal oxide is CaO, SrO or BaO, and described magnesium-yttrium-transition metal or its metal oxide are Fe, Co, Ni or Fe
3O
4, Fe
2O
3, CoO, NiO; Its concrete steps are:
(1) starting raw material is mixed, behind wet ball grinding, oven dry adds tackiness agent, granulation;
(2) material after the above-mentioned granulation is made sheet under the pressure of 2～10MPa;
(3) material step (2) compacting is in blocks is in Ar atmosphere, heat-treats insulation 1h～8h under 1300～1500 ℃; In heat treatment process, Al is put in the compacting test piece
2O
3In the ceramic boat, below the Ar air-flow, put into a plating Fe simultaneously, the Al of Co or Ni
2O
3Or SiO
2Substrate in the test seals porcelain boat, after the thermal treatment, mixes in the test piece all can obtain B on substrate and after the thermal treatment
6O nano wire or its whisker.
The present invention can prepare the B of diameter at 20nm～600nm by the adjustment of proportioning raw materials
6The O nano wire.And the diameter of nano wire can be adjusted according to the variation of process system and batching.Can also prepare B with this method
6The O crystal whisker materials, and its output and purity are all very high.Sample is observed the nano wire pattern of preparation under scanning electronic microscope after separating, the B of visible preparation
6O nano wire output is very high, and nano wire has good consistence.
Description of drawings
The batching zone (black line is with interior zone) that Fig. 1 generates for boride nano wire of the present invention.
Fig. 2 prepares the EELS spectrum of nano wire and whisker for the present invention.
Fig. 3 is the high resolution and the electron diffraction spectrum analysis of nano wire of the present invention.
Fig. 4 is the high resolution and the electron diffraction spectrum analysis of whisker of the present invention.
Fig. 5 is the B of the embodiment of the invention 2 preparations
6O nano wire pattern.
Fig. 6 is the B of the present invention's preparation
6The O whisker morphology.
The B of Fig. 7 for generating on the Si substrate of the present invention
6O nano wire pattern.
The CaB of Fig. 8 for generating on the Si substrate of the present invention
6Whisker morphology.
Embodiment
The present invention will be further described below in conjunction with embodiment:
The present invention adopts solid phase reaction method and chemical gaseous phase depositing process, chooses IIA family metal oxide (CaO, SrO or BaO), boron powder and magnesium-yttrium-transition metal or its metal oxide in the preparation as starting raw material.Wherein the mass ratio of magnesium-yttrium-transition metal or its metal oxide is controlled at 20%～70%, and IIA family metal oxide ratio control is 10%～50%, in order to obtain the B of different scale
6The O nano wire can be controlled by the relative proportion of transferring magnesium-yttrium-transition metal or its metal oxide or IIA family metal oxide.Magnesium-yttrium-transition metal or its metal oxide are a kind of critical materialses for preparing the boride nano wire in test recipe, it mainly not only plays the effect that reduces sintering temperature and liquid phase is provided in sintering process, and it also may provide catalyst action for nanowire growth.In Fig. 1, adopt CaO, Fe
3O
4With the B powder as starting raw material, we delimited having the zone that nano wire generates.Starting raw material is mixed back (can adopt wet method or dry mixed), under the pressure of 2～10MPa, compound is pressed into test piece, certain intensity is arranged, can before compacting, add a little binder, after the granulation, cross 40 mesh sieves for making the compacting test piece.Under the Ar atmosphere, heat-treat under 1350～1500 ℃, soaking time is according to circumstances set, generally at 1h～8h.In heat treatment process, Al is put in the compacting test piece
2O
3In the ceramic boat, below the Ar air-flow, can put into the Al of a plating Fe simultaneously
2O
3Or SiO
2Substrate in the test seals porcelain boat.After the thermal treatment, mix in the test piece all can obtain B on substrate and after the thermal treatment
6O nano wire or its whisker.
Fig. 3 prepares the compositional analysis result of nano wire and whisker structure with energy loss spectroscopy to this method, and as can be seen, its component of the nano wire of preparation is B and O element.Find that by high score power transformation sub-microscope and electron diffraction analysis the crystalline structure of this nano wire (Fig. 4) and whisker (Fig. 5) is B really
6O.
Embodiment 1
Choose 50%Fe
3O
4, 37%B powder and 13%CaO, are dried behind wet ball grinding (dehydrated alcohol is as medium) as starting raw material, and as tackiness agent, granulation is pressed into test piece under 2MPa pressure with 10% glycerol+90% dehydrated alcohol.Under Ar atmosphere, 1400 ℃ of thermal treatments are incubated 2 hours the test piece of compacting, after sheet sample is fired, becomes and have B
6O nano wire and Ca-B, Fe-B mixed powder sample can obtain B after separating
6The O nano wire.
The pulverized specimen of this example 1 preparation after separating, is observed the B of visible preparation to the nano wire pattern of preparation under scanning electronic microscope
6The very high (see figure 6) of O nano wire output, and nano wire has good consistence.
Embodiment 2
Choose 38%Fe
3O
4, 38%B powder and 24%CaO, are dried behind wet ball grinding (dehydrated alcohol is as medium) as starting raw material, and as tackiness agent, granulation is pressed into test piece under 4MPa pressure with 10% glycerol+90% dehydrated alcohol.Under Ar atmosphere, 1400 ℃ of thermal treatments are incubated 2 hours the test piece of compacting, after sheet sample is fired, becomes and have B
6O nano whisker and Ca-B, Fe-B mixed powder sample can obtain B after separating
6The O nano whisker.
On the Si substrate, prepare a large amount of B
6O nano thread structure, output are very high, and nano wire has good consistence (see figure 7), the CaB that also can prepare simultaneously
6The whisker (see figure 8).
Embodiment 3
Step is similar to embodiment 2, in sintering process, places the substrate (Al of plating Fe in the downstream that the Ar air communication is crossed
2O
3Or Si), the thermal treatment temp system can obtain B with embodiment 2 on substrate
6The O nano wire also has a small amount of CaB simultaneously
6Crystal whisker materials.
Embodiment 4
Choose 70%Fe
2O
3, 10%B powder and 20%BaO are as starting raw material, and behind wet ball grinding (dehydrated alcohol is as medium), oven dry is put into the aluminum oxide porcelain boat to mixed powder, and after the sealing, under Ar atmosphere, 1500 ℃ of thermal treatments are incubated 2 hours, and after the thermal treatment, formation has B
6The O nano wire.
Embodiment 5:
Choose 20%Fe
2O
3, 10%B powder and 70%SrO, are dried behind wet ball grinding (dehydrated alcohol is as medium) as starting raw material, and as tackiness agent, granulation is pressed into test piece under 10MPa pressure with 10% glycerol+90% dehydrated alcohol.Under Ar atmosphere, 1300 ℃ of thermal treatments are incubated 8 hours the test piece of compacting, after sheet sample is fired, becomes and have B
6O nano wire and B
6O whisker mixed powder.
Embodiment 6:
Choose 40%Fe, 20%B powder and 40%CaO, are dried behind wet ball grinding (dehydrated alcohol is as medium) as starting raw material, and as tackiness agent, granulation is pressed into test piece under 5MPa pressure with 10% glycerol+90% dehydrated alcohol.Under Ar atmosphere, 1500 ℃ of thermal treatments are incubated 1 hour the test piece of compacting, after sheet sample is fired, becomes and have B
6The O nano wire is placed the Si substrate that plates Fe in initial compound downstream, can find the B that has purity high on the Si substrate
6The O nano wire generates.
Embodiment 7
Choose 30%Ni, 35%B powder and 35%BaO, are dried behind wet ball grinding (dehydrated alcohol is as medium) as starting raw material, and as tackiness agent, granulation is pressed into test piece under 2MPa pressure with 10% glycerol+90% dehydrated alcohol.Under Ar atmosphere, 1400 ℃ of thermal treatments are incubated 8 hours the test piece of compacting, after sheet sample is fired, becomes and have B
6O nano thread structure and whisker structure thereof.
Embodiment 8
Choose 20%CoO, 45%B powder and 35%CaO, are dried behind wet ball grinding (dehydrated alcohol is as medium) as starting raw material, and as tackiness agent, granulation is pressed into test piece under 6MPa pressure with 10% glycerol+90% dehydrated alcohol.Under Ar atmosphere, 1450 ℃ of thermal treatments are incubated 6 hours the test piece of compacting, after sheet sample is fired, becomes and have B
6O nano thread structure and whisker structure thereof.
Embodiment 9
Choose 30%NiO, 35%B powder and 35%BaO, are dried behind wet ball grinding (dehydrated alcohol is as medium) as starting raw material, and as tackiness agent, granulation is pressed into test piece under 8MPa pressure with 10% glycerol+90% dehydrated alcohol.Airtight porcelain boat is put in test piece, placed the substrate (Al of plating Ni in the downstream that the Ar air communication is crossed
2O
3Or Si), the thermal treatment temp system is 1400 ℃ of insulations 4 hours, can obtain B on substrate
6O nano wire and whisker structure.
Claims (2)
1, a kind of preparation B
6The method of O nano wire or whisker structure adopts solid phase reaction method, it is characterized in that: material adopts IIA family metal oxide, boron powder and magnesium-yttrium-transition metal or its metal oxide among the described preparation method; Wherein the mass ratio of magnesium-yttrium-transition metal or its metal oxide is controlled at 20%～70%, and IIA family metal oxide ratio control is 10%～50%, and the ratio of boron powder is 20～70%; Described IIA family metal oxide is CaO, SrO or BaO, and described magnesium-yttrium-transition metal or its metal oxide are Fe, Co, Ni or Fe
3O
4, Fe
2O
3, CoO, NiO; Its concrete steps are:
(1) starting raw material is mixed, behind wet ball grinding, oven dry adds tackiness agent, granulation;
(2) material after the above-mentioned granulation is made sheet under the pressure of 2～10MPa;
(3) material step (2) compacting is in blocks is in Ar atmosphere, heat-treats insulation 1h～8h under 1300～1500 ℃.
2, a kind of preparation B
6The method of O nano wire or whisker structure adopts chemical Vapor deposition process, it is characterized in that: material adopts IIA family metal oxide, boron powder and magnesium-yttrium-transition metal or its metal oxide among the described preparation method; Wherein the mass ratio of magnesium-yttrium-transition metal or its metal oxide is controlled at 20%～70%, and IIA family metal oxide ratio control is 10%～50%, and the ratio of boron powder is 20～70%; Described IIA family metal oxide is CaO, SrO or BaO, and described magnesium-yttrium-transition metal or its metal oxide are Fe, Co, Ni or Fe
3O
4, Fe
2O
3, CoO, NiO; Its concrete steps are:
(1) starting raw material is mixed, behind wet ball grinding, oven dry adds tackiness agent, granulation;
(2) material after the above-mentioned granulation is made sheet under the pressure of 2～10MPa;
(3) material step (2) compacting is in blocks is in Ar atmosphere, heat-treats insulation 1h～8h under 1300～1500 ℃; In heat treatment process, Al is put in the compacting test piece
2O
3In the ceramic boat, below the Ar air-flow, put into a plating Fe simultaneously, the Al of Co or Ni
2O
3Or SiO
2Substrate in the test seals porcelain boat, after the thermal treatment, mixes in the test piece all can obtain B on substrate and after the thermal treatment
6O nano wire or its whisker.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410009238 CN1272244C (en) | 2004-06-22 | 2004-06-22 | B6O nanowire and crystal whisker structure and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410009238 CN1272244C (en) | 2004-06-22 | 2004-06-22 | B6O nanowire and crystal whisker structure and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1594083A CN1594083A (en) | 2005-03-16 |
| CN1272244C true CN1272244C (en) | 2006-08-30 |
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ID=34662398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410009238 Expired - Fee Related CN1272244C (en) | 2004-06-22 | 2004-06-22 | B6O nanowire and crystal whisker structure and its preparation method |
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|---|---|
| CN (1) | CN1272244C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101668717B (en) * | 2007-04-26 | 2013-05-29 | 六号元素（产品）（控股）公司 | Boron suboxide composite material |
| CN101381887B (en) * | 2007-09-05 | 2012-02-15 | 中国科学院物理研究所 | Single crystal boron nanotaper, method for preparing same and applications in electricity and field emission device |
| CN101531374B (en) * | 2008-03-12 | 2011-06-01 | 中国科学院物理研究所 | Method for producing boron nanowire |
| CN104876273B (en) * | 2015-04-30 | 2016-08-24 | 昆明理工大学 | A kind of preparation method of Mn oxide whisker |
| CN108946751B (en) * | 2018-07-13 | 2021-04-13 | 湘潭大学 | Preparation method and application of boron hexa-oxygen |
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