CN105414558A - Preparation method of mono-dispersed spherical nano copper and ferrum - Google Patents
Preparation method of mono-dispersed spherical nano copper and ferrum Download PDFInfo
- Publication number
- CN105414558A CN105414558A CN201510764479.0A CN201510764479A CN105414558A CN 105414558 A CN105414558 A CN 105414558A CN 201510764479 A CN201510764479 A CN 201510764479A CN 105414558 A CN105414558 A CN 105414558A
- Authority
- CN
- China
- Prior art keywords
- preparation
- spherical nano
- nano copper
- copper iron
- copper
- 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.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of mono-dispersed spherical nano copper and ferrum. The preparation method comprises the steps that copper salt, ferric salt and a stabilizing agent are dissolved in organic solvent, the total metallic ion concentration of the copper and the ferrum is controlled to be 0.1-0.5 mol/L, the volume ratio of the stabilizing agent to the organic solvent is controlled to be 0.02-0.2, and the molar ratio of the copper salt to the ferric salt is controlled to be 0.2-5; a system is purged through N2 at the temperature of 110-140 DEG C for 0.5-1.5 hours, a reaction is conducted for 2-5 hours after the temperature is increased to 220-280 DEG C, the stirring speed is controlled to be 280-400 r/min, and the temperature is naturally decreased to the indoor temperature after the reaction is completed; and the nano system is deposited through ethyl alcohol, then washing is conducted three times through normal hexane, obtained sediment is re-dispersed through normal hexane, and mono-dispersed nano CuFe bi-metal particles are obtained after drying is conducted at the temperature of 60-80 DEG C for 16-24 hours in a vacuum drying box. The preparation method has the advantages that the sizes of the obtained particles are uniform, the dispersity is good, and the preparation process is simple.
Description
Technical field
The present invention relates to a kind of nano material preparation method, relate to the preparation method of a kind of monodisperse spherical nano CuFe specifically.
Background technology
Nano particle shows strong skin effect, quantum size effect due to less grain size and larger specific area, and this makes nano material have special chemistry, magnetic, the character such as optical, electrical, hot.Therefore, nano material is widely used in the fields such as catalysis, environment, the energy, sensing, photoelectric material.Bimetallic nano material not only has monometallic characteristic, and show due to the two synergy the character that many monometallics do not possess, have even reach or close to the serviceability of noble metal in certain, thus the research of bimetallic nano receives the concern of researcher gradually.Wherein, nanometer CuFe bimetallic is widely used in chlorine, nitrogen in selective catalysis removing waste water, and CO hydrogenation synthesizing low carbon alcohol etc.At present, coprecipitation, hydro-thermal method, sol-gal process, co-reducing process are commonly used in the preparation of nanometer CuFe bimetallic catalyst.But above method complex process and obtained nanoparticle agglomerates are serious, and granularity, pattern can not be controlled effectively.
Summary of the invention
The object of this invention is to provide the bimetallic preparation method of the simple nanometer CuFe of a kind of size uniformity, good dispersion and preparation process.
Concrete preparation method is: under high temperature inert atmospheric condition, utilizes organic solvent to be reduced by copper iron organic salt, is formed in conjunction with good nanometer CuFe bimetallic.
A preparation method for monodisperse spherical nano copper iron, its feature comprises the steps:
(1) mantoquita, molysite and stabilizing agent are dissolved in organic solvent, be stirred to and mix, controlling the total concentration of metal ions of copper iron is 0.1-0.5mol/L, and the volume ratio controlling stabilizing agent and organic solvent is 0.02-0.2, and the mol ratio controlling mantoquita and molysite is 0.2-5;
(2) by system at 110-140 DEG C with N
2purge 0.5-1.5 hour, be warming up to 220-280 DEG C and carry out reaction 2-5h, control stir speed (S.S.) is 280-400r/min, is naturally down to room temperature after completion of the reaction;
(3) with ethanol, nanometer system is precipitated, use n-hexane afterwards three times, obtained precipitation n-hexane is disperseed again, after the dry 16-24h of 60-80 DEG C of vacuum drying chamber, be mono-dispersed nano CuFe bimetal granule.
Described mantoquita is the one in copper acetate, acetylacetone copper.
Described molysite is the one in ferrocenyl methyl ketone, ferric acetyl acetonade.
Described organic solvent is a kind of in oleyl amine (OAm), diphenyl ether (BE) or both mixtures, and in both mixtures, oleyl amine accounts for total organic solvent volume ratio and controls at 0.4-1.
Described stabilizing agent is one or several mixture of oleic acid (OA), trioctylphosphine oxide (TOPO) (TOPO), tri octyl phosphine (TOP), 1-octadecylene (ODE).
Tool of the present invention has the following advantages:
1. simple to operate, synthesis rate is fast, and one-step synthesis goes out the CuFe duplex metal nano granule of good dispersion.
2. obtained nano particle diameter size is at 8-14nm, and narrow diameter distribution.
Accompanying drawing illustrates:
The TEM figure of the typical CuFe bimetal nano particles of Fig. 1 prepared by embodiment 1.
Fig. 2 is the TEM figure of the typical CuFe bimetal nano particles prepared by embodiment 5.
Detailed description of the invention
Embodiment 1
Take 0.41g copper acetate, 0.35g acetic acid acetone iron, 1ml tri octyl phosphine be dissolved in 25ml oleyl amine, 50 DEG C of heating for dissolving obtain homogeneous phase solution, above-mentioned solution are placed in 110 DEG C of oil bath N
2purge 1 hour, be rapidly heated after purged to 220 DEG C of reactions 2 hours, stir speed (S.S.) is 300r/min, is naturally down to room temperature, obtains homogeneous nanometer system after reaction.Precipitated by above-mentioned nanometer system with 60ml ethanol, centrifugation, then use n-hexane 3 times, again disperseed by the precipitation n-hexane obtained, dry 24h in 65 DEG C of vacuum drying chambers, gained powder is 14nmCuFe duplex metal nano granule.
Embodiment 2
Take 0.60g copper acetate, 0.35g acetic acid acetone iron, 3ml1-octadecylene be dissolved in 35ml diphenyl ether (BE) and (volume ratio BE:OAm=1/6) in the mixed solution of oleyl amine (OAm), 50 DEG C of heating for dissolving obtain homogeneous phase solution, above-mentioned solution are placed in 140 DEG C of oil bath N
2purge 1 hour, be rapidly heated after purged to 245 DEG C of reactions 3.5 hours, stir speed (S.S.) is 400r/min, is naturally down to room temperature after completion of the reaction, obtains homogeneous nanometer system.Precipitated by above-mentioned nanometer system with 60ml ethanol, centrifugation, then use n-hexane 3 times, again disperseed by the precipitation n-hexane obtained, dry 22h in 80 DEG C of vacuum drying chambers, gained powder is 13.5nmCuFe duplex metal nano granule
Embodiment 3
Take 1.52g acetylacetone copper, 0.32g ferrocenyl methyl ketone, 4ml trioctylphosphine oxide (TOPO) be dissolved in 30ml diphenyl ether (BE) and (volume ratio BE:OAm=1/5) in oleyl amine (OAm) mixed solution; 50 DEG C of heating for dissolving obtain homogeneous phase solution, above-mentioned solution are placed in 120 DEG C of oil bath N
2purge 1.5 hours, be rapidly heated after having purged to 230 DEG C of reactions 3 hours, stir speed (S.S.) is 380r/min, is naturally down to room temperature after completion of the reaction, obtains homogeneous nanometer system.Precipitated by above-mentioned nanometer system with 60ml ethanol, centrifugation, then use n-hexane 3 times, again disperseed by the precipitation n-hexane obtained, dry 22h in 70 DEG C of vacuum drying chambers, gained powder is 12nmCuFe duplex metal nano granule.
Embodiment 4
Taking 0.52g acetic acid acetone copper, 0.53g acetic acid acetone iron, 6ml oleic acid and 1.5ml tri octyl phosphine is dissolved in 30ml oleyl amine, and 50 DEG C of heating for dissolving obtain homogeneous system, above-mentioned system are placed in 110 DEG C of oil bath N
2purge 1.5h, be rapidly heated after purging to 260 DEG C of reactions 2 hours, stir speed (S.S.) is 280r/min, reacts complete and is naturally down to room temperature, obtains homogeneous nanometer system.Precipitated by above-mentioned nanometer system with 60ml ethanol, centrifugation, then use n-hexane 3 times, again disperseed by the precipitation n-hexane obtained, dry 18h in 80 DEG C of vacuum drying chambers, gained powder is 10nmCuFe duplex metal nano granule.
Embodiment 5
Take 0.32g acetylacetone copper, 0.42g ferrocenyl methyl ketone, 1ml tri octyl phosphine and 4ml1-octadecylene and be dissolved in 35ml diphenyl ether (BE) and (volume ratio BE:OAm=2/5) in oleyl amine (OAm) mixed solution; 50 DEG C of heating for dissolving obtain homogeneous phase solution, above-mentioned solution are placed in 135 DEG C of oil bath N
2purge 1 hour, be rapidly heated after having purged to 280 DEG C of reactions 3.5 hours, stir speed (S.S.) is 340r/min, is naturally down to room temperature after completion of the reaction, obtains homogeneous nanometer system.Precipitated by above-mentioned nanometer system with 60ml ethanol, centrifugation, then use n-hexane 3 times, again disperseed by the precipitation n-hexane obtained, dry 16h in 60 DEG C of vacuum drying chambers, gained powder is 8.5nmCuFe duplex metal nano granule.
Embodiment 6
Taking 0.62g acetic acid acetone copper, 0.45g acetic acid acetone iron, 4ml1-octadecylene and 2.5ml trioctylphosphine oxide (TOPO) is dissolved in 35ml oleyl amine, and 50 DEG C of heating for dissolving obtain homogeneous system, above-mentioned system are placed in 110 DEG C of oil bath N
2purge 1 hour, be rapidly heated after purging to 255 DEG C of reactions 2.5 hours, stir speed (S.S.) is 350r/min, reacts complete and is naturally down to room temperature, obtains homogeneous nanometer system.Precipitated by above-mentioned nanometer system with ethanol, centrifugation, then use n-hexane 3 times, again disperseed by the precipitation n-hexane obtained, dry 20h in 65 DEG C of vacuum drying chambers, gained powder is 12nm duplex metal nano granule.
Composition, the particle diameter of the CuFe duplex metal nano granule that the embodiment of the present invention obtains list in table one.
The particle diameter of the copper iron that obtains under the different controlled condition of table one mole when duplex metal nano granule
| Sample name | Copper iron mol ratio | Particle diameter nm/TEM |
| Embodiment 1 | 2.1 | 14 |
| Embodiment 2 | 3.0 | 13.5 |
| Embodiment 3 | 4.1 | 12 |
| Embodiment 4 | 1.35 | 10 |
| Embodiment 5 | 0.68 | 8.5 |
| Embodiment 6 | 1.9 | 12 |
Claims (6)
1. a preparation method for monodisperse spherical nano copper iron, is characterized in that comprising the steps:
(1) mantoquita, molysite and stabilizing agent are dissolved in organic solvent, be stirred to and mix, controlling the total concentration of metal ions of copper iron is 0.1-0.5mol/L, and the volume ratio controlling stabilizing agent and organic solvent is 0.02-0.2, and the mol ratio controlling mantoquita and molysite is 0.2-5;
(2) by system at 110-140 DEG C with N
2purge 0.5-1.5 hour, be warming up to 220-280 DEG C and carry out reaction 2-5h, control stir speed (S.S.) is 280-400r/min, is naturally down to room temperature after completion of the reaction;
(3) with ethanol, nanometer system is precipitated, use n-hexane afterwards three times, obtained precipitation n-hexane is disperseed again, after the dry 16-24h of 60-80 DEG C of vacuum drying chamber, be mono-dispersed nano CuFe bimetal granule.
2. the preparation method of a kind of monodisperse spherical nano copper iron as claimed in claim 1, is characterized in that described mantoquita is the one in copper acetate, acetylacetone copper.
3. the preparation method of a kind of monodisperse spherical nano copper iron as claimed in claim 1, is characterized in that described molysite is the one in ferrocenyl methyl ketone, ferric acetyl acetonade.
4. the preparation method of a kind of monodisperse spherical nano copper iron as claimed in claim 1, is characterized in that described organic solvent is a kind of in oleyl amine, diphenyl ether or both mixtures.
5. the preparation method of a kind of monodisperse spherical nano copper iron as claimed in claim 4, to is characterized in that in both mixtures that oleyl amine accounts for total mixture volume ratio and controls at 0.4-1.
6. the preparation method of a kind of monodisperse spherical nano copper iron as claimed in claim 1, is characterized in that described stabilizing agent is one or several mixture of oleic acid, trioctylphosphine oxide (TOPO), tri octyl phosphine, 1-octadecylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510764479.0A CN105414558A (en) | 2015-11-11 | 2015-11-11 | Preparation method of mono-dispersed spherical nano copper and ferrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510764479.0A CN105414558A (en) | 2015-11-11 | 2015-11-11 | Preparation method of mono-dispersed spherical nano copper and ferrum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105414558A true CN105414558A (en) | 2016-03-23 |
Family
ID=55493339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510764479.0A Pending CN105414558A (en) | 2015-11-11 | 2015-11-11 | Preparation method of mono-dispersed spherical nano copper and ferrum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105414558A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105833298A (en) * | 2016-03-24 | 2016-08-10 | 国家纳米科学中心 | Cu3BiS3 nano medicine, preparation method and application thereof |
| CN107282942A (en) * | 2017-06-14 | 2017-10-24 | 中国科学院山西煤炭化学研究所 | A kind of thermal decomposition method prepares the preparation method of the CuFe nano-particles of size adjustable |
| CN108083334A (en) * | 2018-01-09 | 2018-05-29 | 长江大学 | A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material |
| US11311939B2 (en) * | 2019-08-09 | 2022-04-26 | Honda Motor Co., Ltd. | Method for fabrication of copper-silver and copper-gold porous microsheets |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887485A (en) * | 2006-07-20 | 2007-01-03 | 同济大学 | Prepn process of monodisperse nanometer Fe-Pt alloy particle |
| CN101486103A (en) * | 2009-02-27 | 2009-07-22 | 天津商业大学 | Pt-Mn alloy nanoparticle and preparation method of colloid dispersion system thereof |
| CN101549888A (en) * | 2009-05-08 | 2009-10-07 | 中南大学 | Method for preparing monodisperse ferrate nanocrystalline |
| CN101817088A (en) * | 2009-02-27 | 2010-09-01 | 天津商业大学 | Preparation method of Pt-Ni alloy nano particle and colloidal dispersion system thereof |
| CN101992302A (en) * | 2009-08-21 | 2011-03-30 | 中国科学院大连化学物理研究所 | Method for preparing high-dispersion precious metal and alloy nanoparticles thereof |
| CN102228994A (en) * | 2011-06-20 | 2011-11-02 | 厦门大学 | Method for preparing monodisperse silver core-nickel shell nanoparticles |
-
2015
- 2015-11-11 CN CN201510764479.0A patent/CN105414558A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887485A (en) * | 2006-07-20 | 2007-01-03 | 同济大学 | Prepn process of monodisperse nanometer Fe-Pt alloy particle |
| CN101486103A (en) * | 2009-02-27 | 2009-07-22 | 天津商业大学 | Pt-Mn alloy nanoparticle and preparation method of colloid dispersion system thereof |
| CN101817088A (en) * | 2009-02-27 | 2010-09-01 | 天津商业大学 | Preparation method of Pt-Ni alloy nano particle and colloidal dispersion system thereof |
| CN101549888A (en) * | 2009-05-08 | 2009-10-07 | 中南大学 | Method for preparing monodisperse ferrate nanocrystalline |
| CN101992302A (en) * | 2009-08-21 | 2011-03-30 | 中国科学院大连化学物理研究所 | Method for preparing high-dispersion precious metal and alloy nanoparticles thereof |
| CN102228994A (en) * | 2011-06-20 | 2011-11-02 | 厦门大学 | Method for preparing monodisperse silver core-nickel shell nanoparticles |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105833298A (en) * | 2016-03-24 | 2016-08-10 | 国家纳米科学中心 | Cu3BiS3 nano medicine, preparation method and application thereof |
| CN107282942A (en) * | 2017-06-14 | 2017-10-24 | 中国科学院山西煤炭化学研究所 | A kind of thermal decomposition method prepares the preparation method of the CuFe nano-particles of size adjustable |
| CN108083334A (en) * | 2018-01-09 | 2018-05-29 | 长江大学 | A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material |
| US11311939B2 (en) * | 2019-08-09 | 2022-04-26 | Honda Motor Co., Ltd. | Method for fabrication of copper-silver and copper-gold porous microsheets |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105414558A (en) | Preparation method of mono-dispersed spherical nano copper and ferrum | |
| Sivaraman et al. | Room-temperature synthesis of gold nanoparticles—Size-control by slow addition | |
| JP2008013846A (en) | Method for producing metal nanoparticle, and metal nanoparticle | |
| Chen et al. | Size-controlled synthesis of Ru nanoparticles by ethylene glycol reduction | |
| CN103192086A (en) | Preparation method for controllable duplex metal alloy nano particle | |
| CN105127441B (en) | A kind of preparation method of platinum nano microcrystalline dispersion | |
| CN106268900A (en) | A kind of g C3n4quantum dot sensitized AgVO3the preparation method of nano wire | |
| Yang et al. | Preparation and characterization of positively charged ruthenium nanoparticles | |
| CN107537517A (en) | A kind of alloy colloid and preparation method and application | |
| CN110368826B (en) | Preparation method of pickering emulsion with dual responses of magnetic field and redox | |
| TW201235130A (en) | Metal particle powder and paste composition using same | |
| TW201902601A (en) | Silver particles and method of preparing the same | |
| CN105776249A (en) | Manganese hexacyanoferrate nano cube and preparation method thereof | |
| KR20190049276A (en) | Pt-CoO NANO PARTICLE, MANUFACTURING METHOD OF THE SAME AND CATALYST COMPRISING THE SAME | |
| CN105290417A (en) | Synthetic method of nano-silver capable of being highly scattered in organic system | |
| CN111659400B (en) | Preparation method of supported CuNi bimetallic catalyst and application of supported CuNi bimetallic catalyst in reduction reaction | |
| JP2012251222A (en) | Method for producing silver nanoparticle, and ink | |
| Mantella et al. | Shaping non-noble metal nanocrystals via colloidal chemistry | |
| CN105215347B (en) | A kind of Zinc Oxide and gold nano grain composite and preparation method thereof | |
| CN106311223A (en) | Preparation method of precious metal/graphene nanocomposite | |
| CN106623975A (en) | Nanoscale platinum-rhodium alloy powder and preparing method thereof | |
| CN113318753A (en) | Preparation of supported CuPd bimetallic catalyst and application thereof in oxidative coupling reaction | |
| CN109100405A (en) | A kind of adjustable N doping porous C@CeO of oxygen vacancy concentration2-xThe preparation method and application of nanocomposite | |
| JP2009102716A (en) | Method for producing silver nanoparticle | |
| WO2014108841A1 (en) | Synthesis method of precursors to produce molybdenum oxide moo3 and related materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160323 |