CN107282942A - A kind of thermal decomposition method prepares the preparation method of the CuFe nano-particles of size adjustable - Google Patents
A kind of thermal decomposition method prepares the preparation method of the CuFe nano-particles of size adjustable Download PDFInfo
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Abstract
The preparation method that a kind of thermal decomposition method prepares the CuFe nano-particles of size adjustable is to be warming up to 110 140 DEG C after uniformly mixing mantoquita, molysite and reducing agent and stabilizer, purged with nitrogen, 150 190 DEG C of 10 60min of stop are warming up to again, 220 280 DEG C are warming up to again is reacted and flowed back 2 4h, it is cooled to room temperature, ethanol is added to be precipitated, washed afterwards with ethanol with n-hexane, resulting nano-particle n-hexane is disperseed again, then it is dried in vacuo, obtains CuFe nano-particles.The present invention, which has, realizes that nano particle diameter is controllable and homogeneous, controllable, good dispersion and the simple advantage of preparation process of nano-particles size.
Description
Technical field
The invention belongs to a kind of preparation method of nano material, and in particular to a kind of thermal decomposition method prepares size adjustable
The preparation method of CuFe nano-particles.
Background technology
Bimetallic nano material not only has monometallic characteristic, and with the property that many monometallics do not possess, has
Even up to or the characteristic close to noble metal in terms of certain, thus bimetallic nano material research gradually by research people
The concern of member.Bimetallic nano material catalyst is widely used in catalytic field.Bimetal nano material is due to expensive in replacement
Metal, improve important function in terms of catalytic activity and selectivity and by common concern.Constituted around bimetallic material,
The factors such as microstructure carry out the synthetically prepared different bimetallic material of regulation and control, study different bimetallic materials in different catalysis
Performance in reaction, it is intended to find the catalyst material with more high activity, selectivity and stability, and attempt to explore newly
Catalytic reaction and mechanism of catalytic reaction also turn into the hot issue of research.Simultaneously as bimetal nano material prepared by regulation and control
Pattern and size uniformity, can carry out modelling processing, so as to preferably study catalytic reaction by actual bimetallic catalyst
Mechanism.
The controlledly synthesis and preparation of nano material are to further investigate its property and the basic and key of development and application, and right
The research of the Related Mechanisms such as growth, assembling in nano-particle is also vital.Current bimetallic nano CuFe catalyst
Preparation commonly use coprecipitation, co-reducing process, the hot method of hydrothermal/solvent etc., but above method complex process and obtained nanometer
Particle aggregation is serious and particle diameter is larger, and the particle diameter of nano-particle can not be controlled effectively.
The content of the invention
Can realize that nano particle diameter is controllable and homogeneous it is an object of the invention to provide one kind, nano-particles size can
Control, good dispersion and the simple bimetallic nano CuFe of preparation process preparation method.
The present invention has used different aging temperature and different reducing agents and stabilizer ratio respectively, nano-particle
Size is different, shows the alternation of regularity.For the different and different reducing agent of aging temperature and stabilizer ratio
Particle size influence has been made and may reasonably explained.The influence of aging temperature is mainly reflected in the nano-particle stage of growth,
Temperature is higher to cause primary nano-particle to possess higher energy and go to continue to grow up, so temperature is higher, the size of nano-particle
It is bigger.The influence of Simultaneous Stabilization agent is mainly reflected in the stage of growth of nano-particle, and stabilizer is coated on primary nanoparticle sublist
Face, the nano-particle of prevention is further grown up, so the increase of the amount of stabilizer, the size of nano-particle can diminish.Therefore,
The bimetallic CuFe nano-particles prepared by thermal decomposition method have it is following some：(1) the nano-particle epigranular prepared, chi
Very little narrowly distributing；(2) purity is high；(3) it can be realized to bimetallic by changing the ratio of aging temperature, reducing agent and stabilizer
The controllable modulation of CuFe nano-particles sizes.
Thermal decomposition method of the present invention prepares the preparation method of the CuFe nano-particles of size adjustable, comprises the following steps：
(1) mantoquita, molysite and reducing agent and stabilizer are uniformly mixed, mixing time 20-60min under normal temperature, controlled
The total concentration of metal ions of copper and iron is 0.1-0.5mol/L, and the mol ratio of copper and iron is 0.1-10：1, control molysite and reducing agent rub
You are than being 0.02-0.2：1, the mol ratio for controlling reducing agent and stabilizer is 1-15：1；
(2) mixed solution is warming up to 110-140 DEG C, purged 0.5-2 hours with nitrogen, then be warming up to 150-190
DEG C 10-60min is stopped, then be warming up to 220-280 DEG C and reacted and flowed back 2-4h, control stir speed (S.S.) for 280-400r/
Min, naturally cools to room temperature after completion of the reaction；
(3) add the ethanol isometric with solution in step (1) to be precipitated, afterwards with ethanol and n-hexane according to volume
Ratio 3-5:1 carries out washing 3-6 times, by resulting nano-particle with the n-hexane weight isometric with solution in step (1)
It is new scattered, then under 60-80 DEG C of vacuum drying chamber after 24h, obtain CuFe nano-particles.
Described mantoquita is one kind in copper oleate, acetylacetone copper.
Described molysite is one kind in iron oleate, ferric acetyl acetonade.
Described reducing agent is the mixing of one or both of oleyl amine, the carbon glycol of 1,2- 14, borine butylamine (BBA)
Thing, if both mixing, then the mol ratio of both reducing agents is controlled in 0.6-10.
Described stabilizer is octadecylene (ODE), oleic acid (OAC), the mixing of the one or both kind of tri octyl phosphine (TOP)
Thing, if both mixing, then the mol ratio of both stabilizers is controlled in 0.8-10.
The present invention has advantages below：
(1) transmission electron microscope be can see (see accompanying drawing 2), and CuFe nano-particles sizes (6-14nm) are prepared than other methods
Product is smaller also more homogeneous.
(2) preparation method only needs initiation material and simple synthetic route, and cost is low, and reproducible, can be in proportion
Expanding production.
(3) formation mechenism of the bimetal nano particles of thermal decomposition method preparation can theoretically be illustrated.
Brief description of the drawings：
Fig. 1 is different oleyl amines and the mol ratio of oleic acid at 245 DEG C of reaction temperature：(a)2:1；(b)3:1；(c)4:1；
(d)5:1；(e)6:1 transmission electron microscope photo.
Fig. 2 is oleyl amine and oleic acid molar ratio is 5:1, different reaction temperatures：(a)245℃；(b)255℃；(c)265
DEG C transmission electron microscope photo.
Embodiment
Embodiment 1
Weigh 0.26g acetic acid acetone copper, 0.71g acetic acid acetone iron, 100mmol oleic acid to be dissolved in 200mmol oleyl amines, 50 DEG C
Heating for dissolving obtains homogeneous phase solution, and the liquor capacity is 100ml, and above-mentioned solution is placed in into N in 110 DEG C of oil baths20.5h is purged, is blown
190 DEG C of stop 60min are being warming up to after inswept, then are being warming up to 245 DEG C and are being reacted and the 2h that flows back, stir speed (S.S.) is 300r/min, instead
Then room temperature should be down to naturally, obtain homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 100ml ethanol, centrifuged, then
It is 4 with n-hexane and ethanol volume ratio:1 (mixed volume is 30ml), carry out washing 3 times, by obtained precipitation with 100ml just
Hexane disperses again, and 20h is dried in 75 DEG C of vacuum drying chambers, and gained black powder is CuFe nano-particles, and nano-particle is put down
Equal size is 14.12nm.(a) seen in Fig. 1
Embodiment 2
Weigh 0.26g acetic acid acetone copper, 0.71g acetic acid acetone iron, 66.7mmol oleic acid to be dissolved in 200mmol oleyl amines, 50
DEG C heating for dissolving obtains homogeneous phase solution, and the liquor capacity is 90ml, and above-mentioned solution is placed in 120 DEG C of oil baths and uses N2Purge 1h,
150 DEG C of stop 10min are being warming up to after purged, then are being warming up to 245 DEG C and are being reacted and the 2h that flows back, stir speed (S.S.) is 280r/min,
It is down to room temperature naturally after completion of the reaction, obtains homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 90ml ethanol, centrifugation point
From, then with n-hexane and ethanol volume ratio be 3:1 (mixed volume is 30ml), carries out washing 3 times, and obtained precipitation is used
90ml n-hexanes disperse again, and 20h is dried in 75 DEG C of vacuum drying chambers, and gained black powder is CuFe nano-particles, nanometer
Particle average size is 13.01nm.(b) seen in Fig. 2
Embodiment 3
Weigh 0.26g acetic acid acetone copper, 0.71g acetic acid acetone iron, 50mmol oleic acid to be dissolved in 200mmol oleyl amines, 50 DEG C
Heating for dissolving obtains homogeneous phase solution, and the liquor capacity is 84ml, and above-mentioned solution is placed in 140 DEG C of oil baths and uses N22h is purged, is blown
180 DEG C of stop 10min are being warming up to after inswept, then are being warming up to 245 DEG C and are being reacted and the 2h that flows back, stir speed (S.S.) is 400r/min, instead
Room temperature is down to naturally after should finishing, and obtains homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 84ml ethanol, centrifugation point
From, then with n-hexane and ethanol volume ratio be 5:1 (mixed volume is 30ml), carries out washing 3 times, and obtained precipitation is used
84ml n-hexanes disperse again, and 20h is dried in 75 DEG C of vacuum drying chambers, and gained black powder is CuFe nano-particles, nanometer
Particle average size is 9.61nm.(c) seen in Fig. 1
Embodiment 4
Weigh 0.26g acetic acid acetone copper, 0.71g acetic acid acetone iron, 40mmol oleic acid to be dissolved in 200mmol oleyl amines, 50 DEG C
Heating for dissolving obtains homogeneous phase solution, and the liquor capacity is 81ml, and above-mentioned solution is placed in 130 DEG C of oil baths and uses N2Purge 0.5 small
When, it is purged after be warming up to 180 DEG C of stop 30min, then be warming up to 245 DEG C and react and the 2h that flows back, stir speed (S.S.) is 360r/
Min, is down to room temperature naturally after completion of the reaction, obtains homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 40ml ethanol, from
The heart is separated, then with n-hexane and ethanol volume ratio is 4:1 (mixed volume is 30ml), carries out washing 3 times, by obtained precipitation
Disperseed again with 81ml n-hexanes, 20h is dried in 80 DEG C of vacuum drying chambers, gained black powder is CuFe nano-particles, is received
Rice corpuscles average-size is 7.23nm.(d) seen in Fig. 1
Embodiment 5
Weigh 0.26g acetic acid acetone copper, 0.71g acetic acid acetone iron, 33mmol oleic acid to be dissolved in 200mmol oleyl amines, 50 DEG C
Heating for dissolving obtains homogeneous phase solution, and the liquor capacity is 79ml, and above-mentioned solution is placed in 120 DEG C of oil baths and uses N21h is purged, is blown
180 DEG C of stop 60min are being warming up to after inswept, then are being warming up to 245 DEG C and are being reacted and the 2h that flows back, stir speed (S.S.) is 480r/min, instead
Room temperature is down to naturally after should finishing, and obtains homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 40ml ethanol, centrifugation point
From, then with n-hexane and ethanol volume ratio be 4:1 (mixed volume is 30ml), carries out washing 3 times, and obtained precipitation is used
79ml n-hexanes disperse again, and 20h is dried in 80 DEG C of vacuum drying chambers, and gained black powder is CuFe nano-particles, nanometer
Particle average size is 7.01nm.(e) seen in Fig. 1
Embodiment 6
Weigh 2.1g acetic acid acetone copper, 2.8g acetic acid acetone iron, 40mmol oleic acid to be dissolved in 200mmol oleyl amines, 50 DEG C add
Heat of solution obtains homogeneous phase solution, and the liquor capacity is 81ml, and above-mentioned solution is placed in 110 DEG C of oil baths and uses N2Purging 2 hours, blows
150 DEG C of stop 60min are being warming up to after inswept, then are being warming up to 245 DEG C and are being reacted and the 2h that flows back, stir speed (S.S.) is 320r/min, instead
Room temperature is down to naturally after should finishing, and obtains homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 81ml ethanol, centrifugation point
From, then with n-hexane and ethanol volume ratio be 5:1 (mixed volume is 30ml), carries out washing 3 times, and obtained precipitation is used
81ml n-hexanes disperse again, and 20h is dried in 80 DEG C of vacuum drying chambers, and gained black powder is CuFe nano-particles, nanometer
Particle average size is 6.75nm.(a) seen in Fig. 2.
Embodiment 7
Weigh 2.1g acetic acid acetone copper, 2.8g acetic acid acetone iron, 40mmol oleic acid to be dissolved in 200mmol oleyl amines, 50 DEG C add
Heat of solution obtains homogeneous phase solution, and the liquor capacity is 81ml, and above-mentioned solution is placed in 120 DEG C of oil baths and uses N2Purging 1 hour, blows
170 DEG C of stop 10min are being warming up to after inswept, then are being warming up to 255 DEG C and are being reacted and the 2h that flows back, stir speed (S.S.) is 360r/min, instead
Room temperature is down to naturally after should finishing, and obtains homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 81ml ethanol, centrifugation point
From, then with n-hexane and ethanol volume ratio be 3:1 (mixed volume is 30ml), carries out washing 3 times, and obtained precipitation is used
81ml n-hexanes disperse again, and 20h is dried in 80 DEG C of vacuum drying chambers, and gained black powder is CuFe nano-particles, nanometer
Particle average size is 7.89nm.(b) seen in Fig. 2.
Embodiment 8
Weigh 2.1g acetic acid acetone copper, 2.8g acetic acid acetone iron, 40mmol oleic acid to be dissolved in 200mmol oleyl amines, 50 DEG C add
Heat of solution obtains homogeneous phase solution, and the liquor capacity is 81ml, and above-mentioned solution is placed in 120 DEG C of oil baths and uses N20.5h is purged, is blown
180 DEG C of stop 30min are being warming up to after inswept, then are being warming up to 265 DEG C and are being reacted and the 2h that flows back, stir speed (S.S.) is 320r/min, instead
Room temperature is down to naturally after should finishing, and obtains homogeneous nanometer system.Above-mentioned nanometer system is precipitated with 81ml ethanol, centrifugation point
From, then with n-hexane and ethanol volume ratio be 4:1 (mixed volume is 30ml), carries out washing 3 times, and obtained precipitation is used
81ml n-hexanes disperse again, and 20h is dried in 80 DEG C of vacuum drying chambers, and gained black powder is CuFe nano-particles, nanometer
Particle average size is 9.24nm.(c) seen in Fig. 2.
Embodiment 9
3.6g acetic acid acetone copper, 0.82g acetic acid acetone iron and the mixing of 300mmol oleyl amines are weighed, 50 DEG C of heating for dissolving are obtained
Homogeneous phase solution, the liquor capacity is 102ml, and above-mentioned solution is placed in 140 DEG C of oil baths and uses N2Purge 2h, it is purged after heating
50min are stopped to 160 DEG C, then are warming up to 280 DEG C and are reacted and the 2h that flows back, stir speed (S.S.) is 480r/min, natural after completion of the reaction
Room temperature is down to, homogeneous nanometer system is obtained.Above-mentioned nanometer system is precipitated with 102ml ethanol, centrifuged, then use n-hexane
It is 5 with ethanol volume ratio:1 (mixed volume is 30ml), carry out washing 3 times, by obtained precipitation with 102ml n-hexanes again
It is scattered, 20h is dried in 80 DEG C of vacuum drying chambers, gained black powder is CuFe nano-particles, and nano-particle average-size is
10.12nm。
Table one at 245 DEG C of reaction temperature, different oleyl amines duplex metal nano granule corresponding with the mol ratio of oleic acid
Particle diameter
| Sample name | Oleyl amine and oleic acid mol ratio | Particle diameter nm/TEM |
| Embodiment 1 | 2:1 | 14.12 |
| Embodiment 2 | 3:1 | 13.01 |
| Embodiment 3 | 4:1 | 9.61 |
| Embodiment 4 | 5:1 | 7.23 |
| Embodiment 5 | 6:1 | 7.01 |
Table two is 5 in oleyl amine and oleic acid molar ratio:Under 1, the corresponding duplex metal nano granule of different reaction temperatures
Particle diameter
| Sample name | Temperature (DEG C) | Particle diameter nm/TEM |
| Embodiment 6 | 245 | 6.75 |
| Embodiment 7 | 255 | 7.89 |
| Embodiment 8 | 265 | 9.24 |
Claims (7)
1. a kind of thermal decomposition method prepares the preparation method of the CuFe nano-particles of size adjustable, it is characterised in that including following step
Suddenly：
（1）Mantoquita, molysite and reducing agent and stabilizer are uniformly mixed, mixing time 20-60min under normal temperature, control copper and iron
Total concentration of metal ions is 0.1-0.5mol/L, and the mol ratio of copper and iron is 0.1-10：1, control the mol ratio of molysite and reducing agent
For 0.02-0.2：1, the mol ratio for controlling reducing agent and stabilizer is 1-15：1；
（2）Mixed solution is warming up to 110-140 DEG C, is purged 0.5-2 hours with nitrogen, then is warming up to 150-190 DEG C and stopped
10-60min is stayed, then is warming up to 220-280 DEG C and is reacted and flowed back 2-4h, it is 280-400r/min to control stir speed (S.S.), instead
Room temperature is naturally cooled to after should finishing；
（3）Add and step（1）The isometric ethanol of middle solution is precipitated, afterwards with ethanol and n-hexane according to volume ratio
3-5:1 carries out washing 3-6 times, and resulting nano-particle is used and step（1）The isometric n-hexane of middle solution divides again
Dissipate, then under 60-80 DEG C of vacuum drying chamber after 24h, obtain CuFe nano-particles.
2. a kind of thermal decomposition method as claimed in claim 1 prepares the preparation method of the CuFe nano-particles of size adjustable, it is special
Levy and be that described mantoquita is one kind in copper oleate, acetylacetone copper.
3. a kind of thermal decomposition method as claimed in claim 1 prepares the preparation method of the CuFe nano-particles of size adjustable, it is special
Levy and be that described molysite is one kind in iron oleate, ferric acetyl acetonade.
4. a kind of thermal decomposition method as claimed in claim 1 prepares the preparation method of the CuFe nano-particles of size adjustable, it is special
Levy the mixture for being described reducing agent for one or both of oleyl amine, the carbon glycol of 1,2- 14, borine butylamine.
5. a kind of thermal decomposition method as claimed in claim 4 prepares the preparation method of the CuFe nano-particles of size adjustable, it is special
Levy be oleyl amine, the carbon glycol of 1,2- 14, the mol ratio of two kinds of mixtures in borine butylamine is controlled between 0.6-10.
6. a kind of thermal decomposition method as claimed in claim 1 prepares the preparation method of the CuFe nano-particles of size adjustable, it is special
Levy and be that described stabilizer is octadecylene, oleic acid, the mixture of the one or both kind of tri octyl phosphine.
7. a kind of thermal decomposition method as claimed in claim 6 prepares the preparation method of the CuFe nano-particles of size adjustable, it is special
Levy and be that the octadecylene, oleic acid, the mol ratio of two kinds of mixtures of tri octyl phosphine are controlled between 0.8-10.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586953A (en) * | 2018-06-12 | 2019-12-20 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| CN110976903A (en) * | 2019-11-11 | 2020-04-10 | 中国科学院金属研究所 | Bimetal nano-particles with controllable components and sizes and uniform appearance and preparation method thereof |
| CN113981256A (en) * | 2021-11-05 | 2022-01-28 | 中冶赛迪工程技术股份有限公司 | Nano-particle copper-iron composite alloy and preparation and application thereof |
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| CN103170287A (en) * | 2013-03-22 | 2013-06-26 | 中国科学院山西煤炭化学研究所 | Synthesis method of CuFe nano spherical particles with components in concentration gradient distribution |
| CN103191741A (en) * | 2013-03-22 | 2013-07-10 | 中国科学院山西煤炭化学研究所 | Copper-iron core-shell catalyst for lower alcohol synthesis as well as preparation method and application thereof |
| CN105414558A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院山西煤炭化学研究所 | Preparation method of mono-dispersed spherical nano copper and ferrum |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103170287A (en) * | 2013-03-22 | 2013-06-26 | 中国科学院山西煤炭化学研究所 | Synthesis method of CuFe nano spherical particles with components in concentration gradient distribution |
| CN103191741A (en) * | 2013-03-22 | 2013-07-10 | 中国科学院山西煤炭化学研究所 | Copper-iron core-shell catalyst for lower alcohol synthesis as well as preparation method and application thereof |
| CN105414558A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院山西煤炭化学研究所 | Preparation method of mono-dispersed spherical nano copper and ferrum |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586953A (en) * | 2018-06-12 | 2019-12-20 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| CN110586953B (en) * | 2018-06-12 | 2022-09-16 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| CN110976903A (en) * | 2019-11-11 | 2020-04-10 | 中国科学院金属研究所 | Bimetal nano-particles with controllable components and sizes and uniform appearance and preparation method thereof |
| CN110976903B (en) * | 2019-11-11 | 2021-08-17 | 中国科学院金属研究所 | Bimetal nano-particles with controllable components and sizes and uniform appearance and preparation method thereof |
| CN113981256A (en) * | 2021-11-05 | 2022-01-28 | 中冶赛迪工程技术股份有限公司 | Nano-particle copper-iron composite alloy and preparation and application thereof |
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