CN101436640B - ZnO/beta-FeSi2 composite material and preparation method - Google Patents
ZnO/beta-FeSi2 composite material and preparation method Download PDFInfo
- Publication number
- CN101436640B CN101436640B CN200810209809XA CN200810209809A CN101436640B CN 101436640 B CN101436640 B CN 101436640B CN 200810209809X A CN200810209809X A CN 200810209809XA CN 200810209809 A CN200810209809 A CN 200810209809A CN 101436640 B CN101436640 B CN 101436640B
- Authority
- CN
- China
- Prior art keywords
- composite material
- zno
- fesi2
- beta
- fesi
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Compounds Of Iron (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a ZnO/beta-FeSi2 composite material and a method for preparing the same, in particular to a composite material and a method for preparing the same. The method solves the problem that beta-FeSi2 has poor oxidation resistance under a condition of long-term high temperature service. The ZnO/beta-FeSi2 composite material is prepared from a sodium oleate aqueous solution, the beta-FeSi2 and zinc acetate. The method for preparing the composite material comprises: step one, adding the beta-FeSi2 to the sodium oleate aqueous solution and stirring the mixture; step two, dissolving the zinc acetate in isopropyl alcohol, dripping ethylene alcohol amine to the isopropyl alcohol, heating the mixture through water bath, and stirring the mixture; step three, performing ultrasound treatment on the mixed liquid prepared in the step two, then adding the mixed liquid to the mixed liquid prepared in the step three, heating the mixture through the water bath, and stirring the mixture; and step four, performing drying and heat treatment to obtain the ZnO/beta-FeSi2 composite material. The ZnO/beta-FeSi2 composite material prepared by the method has good oxidation resistance under the condition of long-term high temperature service. The method has the advantages of simple process and convenient operation.
Description
Technical field
The present invention relates to relate to a kind of composite material and preparation method.。
Background technology
β-FeSi
2Be to be suitable for the thermoelectric material of in 200 ℃～900 ℃ temperature ranges, working, advantage such as it has high antioxidant, and is nontoxic, cheap.Just because of these features, β-FeSi2 has caused concern more and more widely.But β-FeSi
2Non-oxidizability is relatively poor under the Long-term Service under High Temperature condition, thereby makes its application be subjected to certain restriction.
Summary of the invention
The present invention seeks in order to solve β-FeSi
2The problem of non-oxidizability difference under the Long-term Service under High Temperature condition, and a kind of ZnO/ β-FeSi is provided
2Composite material and preparation method.
ZnO/ β-FeSi
2Composite material is by ratio of weight and the number of copies by 5～20 parts of aqueous solution sodium oleates, 4～8 parts of β-FeSi
2Make with 2～4 parts of zinc acetates.
ZnO/ β-FeSi
2Composite material prepares according to the following steps: one, add 4～8 parts of β-FeSi by ratio of weight and the number of copies in 5～20 parts of aqueous solution sodium oleates
2, low whipping speed is to stir 20～30min under the condition of 1～3r/s; Two, 2～4 parts of zinc acetates are dissolved in the isopropyl alcohol, drip ethylene glycol amine again, stir 20～30min in 40～50 ℃ water bath with thermostatic control, mixing speed is 1～3r/s; Three, with the mixed liquor sonicated 10～20min of step 1 preparation, join then in the mixed solution of step 2 preparation, in 50～60 ℃ water bath with thermostatic control, stir 1～2h, mixing speed is 1～3r/s; Four, the mixed liquor of step 3 preparation is dried 10～15h down at 80～120 ℃,, promptly get ZnO/ β-FeSi then at 500～550 ℃ of following heat treatment 1～3h
2Composite material; Wherein the volume ratio of isopropyl alcohol and ethylene glycol amine is 100～150: 1 in the step 2, and the weight of zinc acetate and the volume ratio of isopropyl alcohol are 1～2: 30.
The inventive method makes β-FeSi
2Operation temperature area broaden ZnO/ β-FeSi that the present invention obtains
2Composite material and uncoated β-FeSi
2Particle is compared antioxygenic property and is obviously strengthened, uncoated β-FeSi
2Particle has tangible weightening finish after 400 ℃ of sintering, through the β-FeSi of ZnO coating
2Particle does not have tangible weightening finish after 400 ℃ of sintering, continuing to heat up has tangible weightening finish after 600 ℃ of sintering, and the reason that weightening finish occurs is because β-FeSi
2Under hot conditions with the oxygen generation oxide that reacts.Uncoated β-FeSi
2The particle thermal conductivity has tangible rising after 600 ℃, and the β-FeSi that coats through ZnO
2Particle thermal conductivity in 0～800 ℃ all increases with temperature and reduces.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: present embodiment ZnO/ β-FeSi
2Composite material is by ratio of weight and the number of copies by 5～20 parts of aqueous solution sodium oleates, 4～8 parts of β-FeSi
2Make with 2～4 parts of zinc acetates.
Embodiment two: that present embodiment and embodiment one are different is ZnO/ β-FeSi
2Composite material is by ratio of weight and the number of copies by 10 parts of aqueous solution sodium oleates, 6 parts of β-FeSi
2Make with 3 parts of zinc acetates.Other is identical with embodiment one.
Embodiment three: present embodiment is different with embodiment one or two is that the molar concentration of aqueous solution sodium oleate is 0.2～0.4mol/L.Other is identical with embodiment one or two.
Embodiment four: present embodiment ZnO/ β-FeSi
2Composite material prepares according to the following steps: one, add 4～8 parts of β-FeSi by ratio of weight and the number of copies in 5～20 parts of aqueous solution sodium oleates
2, low whipping speed is to stir 20～30min under the condition of 1～3r/s; Two, 2～4 parts of zinc acetates are dissolved in the isopropyl alcohol, drip ethylene glycol amine again, stir 20～30min in 40～50 ℃ water bath with thermostatic control, mixing speed is 1～3r/s; Three, with the mixed liquor sonicated 10～20min of step 1 preparation, join then in the mixed solution of step 2 preparation, in 50～60 ℃ water bath with thermostatic control, stir 1～2h, mixing speed is 1～3r/s; Four, the mixed liquor of step 3 preparation is dried 10～15h down at 80～120 ℃,, promptly get ZnO/ β-FeSi then at 500～550 ℃ of following heat treatment 1～3h
2Composite material; Wherein the volume ratio of isopropyl alcohol and ethylene glycol amine is 100～150: 1 in the step 2, and the weight of zinc acetate and the volume ratio of isopropyl alcohol are 1～2: 30.
It is pure that used zinc acetate, isopropyl alcohol and the ethylene glycol amine of present embodiment is analysis.
ZnO/ β-FeSi that present embodiment makes
2Oxidation just takes place in composite material under condition more than 600 ℃, thermal conductivity all reduces with the temperature increase in 0～800 ℃
Embodiment five: present embodiment and embodiment four are different is that the molar concentration of aqueous solution sodium oleate in the step 2 is 0.2～0.4mol/L.Other step is identical with embodiment four with parameter.
Embodiment six: present embodiment and embodiment four are different is that mixing time in the step 1 is 22～28min.Other step and parameter are identical with embodiment four.
Embodiment seven: present embodiment and embodiment four are different is that mixing time in the step 1 is 20min.Other step and parameter are identical with embodiment four.
Embodiment eight: present embodiment and embodiment four are different is that mixing time in the step 1 is 30min.Other step and parameter are identical with embodiment four.
Embodiment nine: present embodiment and embodiment four are different is that mixing time in the step 1 is 25min.Other step and parameter are identical with embodiment four.
Embodiment ten: present embodiment is different with embodiment four or six is that mixing time in the step 2 is 22～28min.Other step and parameter are identical with embodiment four or six.
Embodiment 11: present embodiment is different with embodiment four or six is that mixing time in the step 2 is 20min.Other step and parameter are identical with embodiment four or six.
Embodiment 12: present embodiment is different with embodiment four or six is that mixing time in the step 2 is 30min.Other step and parameter are identical with embodiment four or six.
Embodiment 13: present embodiment is different with embodiment four or six is that mixing time in the step 2 is 25min.Other step and parameter are identical with embodiment four or six.
Embodiment 14: present embodiment and embodiment ten are different is that ultrasonic time in the step 3 is 12～18min.Other step and parameter are identical with embodiment ten.
Embodiment 15: present embodiment and embodiment ten are different is that ultrasonic time in the step 3 is 10min.Other step and parameter are identical with embodiment ten.
Embodiment 16: present embodiment and embodiment ten are different is that ultrasonic time in the step 3 is 20min.Other step and parameter are identical with embodiment ten.
Embodiment 17: present embodiment and embodiment ten are different is that ultrasonic time in the step 3 is 15min.Other step and parameter are identical with embodiment ten.
Embodiment 18: present embodiment and embodiment four, six or 14 are different is that mixing time in the step 3 is 1.5h.Other step and parameter are identical with embodiment four, six or 14.
Embodiment 19: present embodiment and embodiment four, six or 14 are different is that mixing time in the step 3 is 1h.Other step and parameter are identical with embodiment four, six or 14.
Embodiment 20: present embodiment and embodiment four, six or 14 are different is that mixing time in the step 3 is 2h.Other step and parameter are identical with embodiment four, six or 14.
Embodiment 21: what present embodiment and embodiment 18 were different is that drying time is 12～14h in the step 4.Other step and parameter are identical with embodiment 18.
Embodiment 22: what present embodiment and embodiment 18 were different is that drying time is 10h in the step 4.Other step and parameter are identical with embodiment 18.
Embodiment 23: what present embodiment and embodiment 18 were different is that drying time is 15h in the step 4.Other step and parameter are identical with embodiment 18.
Embodiment 24: what present embodiment and embodiment 18 were different is that drying time is 13h in the step 4.Other step and parameter are identical with embodiment 18.
Embodiment 25: what present embodiment and embodiment four, six, 14 or 21 were different is that heat treatment time is 2h in the step 4.Other step and parameter are identical with embodiment four, six, 14 or 21.
Embodiment 26: what present embodiment and embodiment four, six, 14 or 21 were different is that heat treatment time is 1h in the step 4.Other step and parameter are identical with embodiment four, six, 14 or 21.
Embodiment 27: what present embodiment and embodiment four, six, 14 or 21 were different is that heat treatment time is 3h in the step 4.Other step and parameter are identical with embodiment four, six, 14 or 21.
Embodiment 28: present embodiment ZnO/ β-FeSi
2The preparation method of composite material realizes according to the following steps: one, add 4 parts of β-FeSi by ratio of weight and the number of copies in 10 parts of aqueous solution sodium oleates
2, low whipping speed is to stir 20min under the condition of 1～3r/s; Two, 2 parts of zinc acetates are dissolved in the isopropyl alcohol, drip ethylene glycol amine again, stir 20min in 40 ℃ water bath with thermostatic control, mixing speed is 1～3r/s; Three, with the mixed liquor sonicated 20min of step 1 preparation, join then in the mixed solution of step 2 preparation, in 50 ℃ water bath with thermostatic control, stir 1h, mixing speed is 1～3r/s; Four, the mixed liquor of step 3 preparation is dried 10h down at 100 ℃,, promptly get ZnO/ β-FeSi then at 500 ℃ of following heat treatment 1h
2Composite material; Wherein the volume ratio of isopropyl alcohol and ethylene glycol amine is 100: 1 in the step 2, and the weight of zinc acetate and the volume ratio of isopropyl alcohol are 1: 30.
ZnO/ β-FeSi that present embodiment makes
2Oxidation just takes place in composite material under condition more than 600 ℃, thermal conductivity all reduces with the temperature increase in 0～800 ℃.
Claims (3)
1.ZnO/ β-FeSi
2Composite material is characterized in that ZnO/ β-FeSi
2Composite material is by ratio of weight and the number of copies by 5～20 parts of aqueous solution sodium oleates, 4～8 parts of β-FeSi
2Make with 2～4 parts of zinc acetates.
2. ZnO/ β-FeSi according to claim 1
2Composite material is characterized in that ZnO/ β-FeSi
2Composite material is by ratio of weight and the number of copies by 10 parts of aqueous solution sodium oleates, 6 parts of β-FeSi
2Make with 3 parts of zinc acetates.
3. ZnO/ β-FeSi according to claim 1 and 2
2Composite material, the molar concentration that it is characterized in that aqueous solution sodium oleate is 0.2～0.4mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810209809XA CN101436640B (en) | 2008-12-26 | 2008-12-26 | ZnO/beta-FeSi2 composite material and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810209809XA CN101436640B (en) | 2008-12-26 | 2008-12-26 | ZnO/beta-FeSi2 composite material and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101436640A CN101436640A (en) | 2009-05-20 |
| CN101436640B true CN101436640B (en) | 2011-08-10 |
Family
ID=40710961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810209809XA Expired - Fee Related CN101436640B (en) | 2008-12-26 | 2008-12-26 | ZnO/beta-FeSi2 composite material and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101436640B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102496677B (en) * | 2011-11-24 | 2014-12-10 | 上海第二工业大学 | Preparation method of poly(p-phenylene) nanoparticle composite ZnO-based thermoelectric material system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5547598A (en) * | 1993-08-04 | 1996-08-20 | Technova, Inc. | Thermoelectric semiconductor material |
| CN1438202A (en) * | 2003-03-04 | 2003-08-27 | 浙江大学 | P-type and beta-type FeSi2-base thermalelectric material containing dispersion-distribution nitride granule |
| JP2004103951A (en) * | 2002-09-11 | 2004-04-02 | Univ Saitama | Manufacturing method of thermoelectric material |
-
2008
- 2008-12-26 CN CN200810209809XA patent/CN101436640B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5547598A (en) * | 1993-08-04 | 1996-08-20 | Technova, Inc. | Thermoelectric semiconductor material |
| JP2004103951A (en) * | 2002-09-11 | 2004-04-02 | Univ Saitama | Manufacturing method of thermoelectric material |
| CN1438202A (en) * | 2003-03-04 | 2003-08-27 | 浙江大学 | P-type and beta-type FeSi2-base thermalelectric material containing dispersion-distribution nitride granule |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101436640A (en) | 2009-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105239060B (en) | A kind of hot-spraying coating anti-reflection layer and preparation method thereof absorbed suitable for solar selectively | |
| CN104086150B (en) | A kind of heat insulation aerogel material of building heat preservation and preparation method | |
| CN104109493B (en) | Formula and preparation technology of methyl cellulose-casein mixed label adhesive | |
| CN105440821A (en) | Antirust paint for pump valve | |
| CN101436640B (en) | ZnO/beta-FeSi2 composite material and preparation method | |
| CN106866992A (en) | A kind of preparation method of the titania modified polyacrylate dispersion of hollow spheres | |
| CN104403329A (en) | Heat-conducting silicone rubber | |
| CN105624443A (en) | Preparation method for ultra-thin Al2O3 dispersion strengthened copper materials | |
| CN105714356A (en) | Sealant for aluminum alloy anode oxide film and preparing method for sealant | |
| CN101798497B (en) | Composite phase-change energy-storage material and preparation method thereof | |
| CN102723203A (en) | Preparation method of electrolyte for aluminum electrolytic capacitor | |
| CN101775656B (en) | Microwave hydrothermal preparation method of NiTiO3 nano film | |
| CN106832697A (en) | The preparation method of corrosion-resistant PTFE base hydraulic seal | |
| CN103642455B (en) | A kind of non-drying sealing compound | |
| CN101693601A (en) | Method for preparing copper oxide film | |
| CN103922705B (en) | A kind of low-temperature sintering Zirconia reinforced alumina material and preparation method thereof | |
| CN101767081A (en) | Preparation method of metal-dielectric solar spectral selective absorbing coating | |
| CN103757895A (en) | Finishing fluid for cotton dress and preparation method thereof | |
| CN103512939B (en) | Preparation method of 3, 5-dibromo salicylaldehyde Schiff base nickel complex-graphene oxide electrochemical immunosensor | |
| CN104194687A (en) | Formula and preparation process of styrene and polyether urethane copolymer adhesive | |
| CN112725854A (en) | Processing method for electroplating pretreatment | |
| CN105120536A (en) | Preparation method of nano material heating element | |
| CN104631121B (en) | The insulating moulding coating and its preparation technology of a kind of heat-insulation and heat-preservation fiber | |
| CN103643509A (en) | Antibacterial finishing technique of knitted fabric | |
| CN101665329A (en) | Preparation method of tricobalt tetraoxide film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110810 Termination date: 20141226 |
|
| EXPY | Termination of patent right or utility model |