CN105834446B - A kind of synthetic method of ultra-thin stratiform NiO CoOx nanometer sheets load NiCo nano compositions - Google Patents
A kind of synthetic method of ultra-thin stratiform NiO CoOx nanometer sheets load NiCo nano compositions Download PDFInfo
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- CN105834446B CN105834446B CN201610221985.XA CN201610221985A CN105834446B CN 105834446 B CN105834446 B CN 105834446B CN 201610221985 A CN201610221985 A CN 201610221985A CN 105834446 B CN105834446 B CN 105834446B
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- 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
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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of ultra-thin stratiform NiO CoOxNanometer sheet loads the synthetic method of NiCo nano compositions, is specially：The first step is by Ni, Co inorganic salt solution is added in the pyroxylin film of conical flask pattern, it is put into after sealing in the beaker equipped with sodium carbonate liquor and carries out precipitation reaction, second step is at a certain temperature with the complete solution of unreacted in reducing agent reduction pyroxylin film, reaction is centrifuged sample after terminating, washing, dry, it is ultra-thin stratiform NiO CoO that calcining, which obtains final product,xNanometer sheet loads NiCo nano compositions.The big nano composite material of specific surface area is prepared using the inventive method, there is excellent magnetic and catalytic activity.The inventive method is simple to operation, and the processing of easy to control and product is simple, is adapted to medium-scale industrial production.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, more particularly to a kind of ultra-thin stratiform NiO-CoOxNanometer sheet loads
The synthetic method of NiCo nano compositions.
Background technology
Two-dimensional ultrathin nanometer sheet can will be microcosmic under excellent electricity, magnetics and optical property and the ultra-thin property under macroscopic view,
The transparency and pliability are organically combined together, so as to realize that device miniaturization and function maximize perfect unity.Two
The characteristics of dimension nano material is because of its thickness and two-dimension plane structure often has the electronics knot different from respective masses material
Structure, be not only able to influence its intrinsic performance, moreover it is possible to produce some new properties, while it have very high theoretical specific surface area and
Electron mobility so that it rapidly becomes material science and the active study hotspot of chemical field.Nanoalloy particle and two dimension
The compound performance that can further improve material of oxide thin layer thing, inorganic metal nano-particle and metal oxide are widened significantly
Application.Nanoalloy particle modifies dimensional thinlayer oxide, and this can not only overcome huge model moral between nanoscale twins
Hua Li, the reunion of nanometer sheet is prevented, the peculiar property of the ultra-thin layer structure of metal oxide is retained.Meanwhile obtain
Its many performance of composite are inherently more more superior than alloy, in chemically modified electrode, electrochmical power source, caltalyst and gas
Sensor etc. has important application value.By ultra-thin stratiform NiO-CoO in this experimentxNanometer sheet and NiCo nano-particles
Carry out effective compound, formation two-dimensional nano composite construction, first, ultra-thin stratiform NiO-CoOxThere is largely low match somebody with somebody on nanometer sheet surface
The undersaturated negative oxygen ion in position can decompose production hydrogen for Compounds with Hydrazine Hydrate Catalyzed and provide substantial amounts of basic site so as to improve the selection of reaction
Property；Secondly, the synergy of NiCo alloys can greatly improve the activity of catalytic reaction；Again, this two-dimensional film structure has
Larger specific surface area, the avtive spot of more catalytic reactions can be provided, improve catalytic efficiency.
The content of the invention
It is an object of the invention to provide a kind of ultra-thin stratiform NiO-CoOxNanometer sheet loads NiCo nano compositions
Synthetic method.
To achieve these goals, technical scheme is as follows：
A kind of synthesis of ultra-thin stratiform NiO-CoOx nanometer sheets load NiCo nano compositions proposed by the present invention
Method, comprise the following steps that：
（1）By Ni, Co inorganic salt solution is added in the pyroxylin film of conical flask pattern, is put into after sealing equipped with carbonic acid
Precipitation reaction is carried out in the beaker of sodium solution；The mol ratio of Ni, Co inorganic salts is 7:3；The molal quantity of the Ni, Co inorganic salts
Summation and the mol ratio of sodium carbonate are 1:4；
（2）With complete solution is not precipitated in reducing agent reduction pyroxylin film at 0~25 DEG C, react sample after terminating
Centrifuged, washed, dried, calcining obtains final product, and NiCo nanoparticles are loaded for ultra-thin stratiform NiO-CoOx nanometer sheets
Sub- composite.
In the present invention, Ni is prepared, the solvent that Co inorganic salt solution uses is deionized water.
In the present invention, step（1）Described in Ni inorganic salts be nickel chloride, Co inorganic salts are cobalt chloride, and its concentration is equal
For 0.005~0.02mol/L.
In the present invention, step（1）Described in sodium carbonate liquor its concentration be 0.02~0.08mol/L.
In the present invention, step（1）Described in the precipitation reaction time be 20 minutes.
In the present invention, step（2）Described in reducing agent be the potassium borohydride aqueous solution, its concentration is 0.02~0.08mol/
L。
In the present invention, step（2）Described in the reduction reaction time be 30 minutes.
In the present invention, step（2）Described in washing be all using deionized water and absolute ethyl alcohol carry out alternately washing.
In the present invention, step（2）Described in centrifugation rotating speed be 6000 revs/min, the time be 5 minutes.
In the present invention, step（2）Described in drying be that 10h is dried at 60 DEG C of vacuum drying chamber.
In the present invention, step（2）Described in calcining be in argon gas atmosphere 1 DEG C/min be warming up to 400 DEG C insulation 1h.
Due to using such scheme, the invention has the advantages that：
1st, the present invention is realized using the presoma realized using common nickel chloride, cobalt chloride for reaction, by altogether
Precipitation-reducing process, ultra-thin stratiform NiO-CoO has been synthesized firstxNanometer sheet loads the composite of NiCo nano-particles.
2nd, method of the invention has very high control to the pattern of product.
3rd, the present invention has very strong versatility using simple inorganic salts as reactant.
4th, product prepared by the present invention has the performance that good Compounds with Hydrazine Hydrate Catalyzed decomposes production hydrogen, can be urged as high-performance
Agent, there are more vast potential for future development and application space.
5th, technique of the invention is simple, and preparation condition is general, and product morphology is stable, purity is high, and the convenient letter of product processing
It is clean, it is suitable for medium-scale industrial production.
6th, method of the invention has the characteristics that mild condition, efficient energy-saving, easily controllable.
Brief description of the drawings
Fig. 1 is the SEM photograph of the intermediate product obtained in embodiment 1 under 500nm multiple.
Fig. 2 is the SEM photograph of the product obtained in embodiment 1 under 200nm multiple.
Fig. 3 is the TEM photos of the intermediate product obtained in embodiment 1 under 20nm multiple.
Fig. 4 is the TEM photos of the product obtained in embodiment 1 under 50nm multiple.
Fig. 5 is the XRD spectrum of the products therefrom of embodiment 1 and intermediate product.
Fig. 6 is the EDS collection of illustrative plates of the products therefrom of embodiment 1 and intermediate product.
Fig. 7 is the SEM photograph of the intermediate product obtained in embodiment 2 under 500nm multiple.
Fig. 8 is the SEM photograph of the intermediate product obtained in embodiment 3 under 500nm multiple.
Fig. 9 is the SEM photograph of the product obtained in embodiment 4 under 500nm multiple.
Embodiment
The present invention is further detailed explanation for illustrated embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The first step, accurately weigh 0.1185gNiCl2·6H2O, 100ml solution is configured to deionized water, concentration is
5mmol/L, accurately weigh 0.1189gCoCl2·2H2O, 100ml solution is configured to deionized water, concentration 5mmol/L,
Ni2+：Co2+According to 7:3 mol ratios are mixed, and cumulative volume 100ml, are subsequently placed in the pyroxylin film of conical flask pattern,
It is placed on after sealing in 250ml beakers.
Second step, 0.166g sodium carbonate is accurately weighed, 100ml solution, concentration 20mmol/ are configured to deionized water
L, then it is poured into the beaker of the first step and is sealed beaker mouth with preservative film and reacted.
3rd step, after reacting 20 minutes, collect the solution in pyroxylin film and precipitation is poured into 250 ml beakers, add
Enter magneton stirring to be placed in reaching 0 DEG C in mixture of ice and water.
4th step, 0.1079g potassium borohydride is accurately weighed, be configured to 100ml solution with deionized water, concentration is
20mmol/L, and put it into refrigerator and treat that it reaches 0 DEG C, then it is slowly added drop-wise in the beaker of the 3rd step and carried out instead
Should.
5th step, react 30 minutes, take out magneton, centrifuge and washed for several times with absolute ethyl alcohol and deionized water, be placed in true
Dried in empty drying box.
6th step, the powder sample that will be obtained after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to
400 DEG C and 1h is incubated, obtains final ultra-thin stratiform NiO-CoOxNanometer sheet loads the composite of NiCo nano-particles.
Fig. 1 is the intermediate product NiO-CoO obtained in embodiment 1 under 200nm multiplexThe SEM pictures of nanometer sheet；Figure
2 be the SEM pictures of the product obtained in embodiment 1 under 500nm multiple；Fig. 3 is the gained intermediate product NiO- of embodiment 1
CoOxThe TEM pictures of nanometer sheet；Fig. 4 is the TEM pictures of the products therefrom of embodiment 1；Fig. 5 is the products therefrom of embodiment 1（a）With in
Between product (b) XRD spectrum, it was demonstrated that NiO-CoOxNanometer sheet and NiCo nano-particles it is compound；Fig. 6 is to be produced in embodiment 1
Thing（a）Indicate wherein Ni with the EDS collection of illustrative plates of intermediate product (b), Co, the presence of O elements, at the same in product oxygen atomic ratio
Less than intermediate product, the synthesis of composite has further been proved.
Embodiment 2
The first step, accurately weigh 0.2370gNiCl2·6H2O, 100ml solution is configured to deionized water, concentration is
10mmol/L, accurately weigh 0.2378gCoCl2·2H2O, 100ml solution is configured to deionized water, concentration 10mmol/L,
Ni2+：Co2+According to 7:3 mol ratios are mixed, and cumulative volume 100ml, are subsequently placed in the pyroxylin film of conical flask pattern,
It is placed on after sealing in 250ml beakers.
Second step, 0.332g sodium carbonate is accurately weighed, 100ml solution, concentration 40mmol/ are configured to deionized water
L, then it is poured into the beaker of the first step and is sealed beaker mouth with preservative film and reacted.
3rd step, after reacting 20 minutes, collect the solution in pyroxylin film and precipitation is poured into 250 ml beakers, add
Enter magneton stirring to be placed in reaching 0 DEG C in mixture of ice and water.
4th step, 0.2158g potassium borohydride is accurately weighed, be configured to 100ml solution with deionized water, concentration is
40mmol/L, and put it into refrigerator and treat that it reaches 0 DEG C, then it is slowly added drop-wise in the beaker of the 3rd step and carried out instead
Should.
5th step, react 30 minutes, take out magneton, centrifuge and washed for several times with absolute ethyl alcohol and deionized water, be placed in true
Dried in empty drying box.
6th step, the powder sample that will be obtained after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to
400 DEG C and 1h is incubated, obtains final ultra-thin stratiform NiO-CoOxNanometer sheet loads the composite of NiCo nano-particles.
Fig. 7 is the intermediate product NiO-CoO obtained in embodiment 2 under 500nm multiplexThe SEM photograph of nanometer sheet.By
Picture can be seen that can still form dimensional thinlayer structure on this condition, and simply the amount of crimp of film is larger, and compare table
Area is smaller.
Embodiment 3
The first step, accurately weigh 0.4740gNiCl2·6H2O, 100ml solution is configured to deionized water, concentration is
20mmol/L, accurately weigh 0.4756gCoCl2·2H2O, 100ml solution is configured to deionized water, concentration 20mmol/L,
Ni2+：Co2+According to 7:3 mol ratios are mixed, and cumulative volume 100ml, are subsequently placed in the pyroxylin film of conical flask pattern,
It is placed on after sealing in 250ml beakers.
Second step, 0.664g sodium carbonate is accurately weighed, 100ml solution, concentration 80mmol/ are configured to deionized water
L, then it is poured into the beaker of the first step and is sealed beaker mouth with preservative film and reacted.
3rd step, after reacting 20 minutes, collect the solution in pyroxylin film and precipitation is poured into 250 ml beakers, add
Enter magneton stirring to be placed in reaching 0 DEG C in mixture of ice and water.
4th step, 0.4316g potassium borohydride is accurately weighed, be configured to 100ml solution with deionized water, concentration is
80mmol/L, and put it into refrigerator and treat that it reaches 0 DEG C, then it is slowly added drop-wise in the beaker of the 3rd step and carried out instead
Should.
5th step, react 30 minutes, take out magneton, centrifuge and washed for several times with absolute ethyl alcohol and deionized water, be placed in true
Dried in empty drying box.
6th step, the powder sample that will be obtained after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to
400 DEG C and 1h is incubated, obtains final ultra-thin stratiform NiO-CoOxNanometer sheet loads the composite of NiCo nano-particles.
Fig. 8 is the intermediate product NiO-CoO obtained in embodiment 3 under 500nm multiplexThe SEM photograph of nanometer sheet.By
It is not it is obvious that be more likely to multi-level flower-like structure that picture, which can be seen that the laminate structure formed on this condition, illustrates reaction
After thing concentration improves, the speed of growth is accelerated to be difficult to generate dimensional thinlayer structure.
Embodiment 4
The first step, accurately weigh 0.1185gNiCl2·6H2O, 100ml solution is configured to deionized water, concentration is
5mmol/L, accurately weigh 0.1189gCoCl2·2H2O, 100ml solution is configured to deionized water, concentration 5mmol/L,
Ni2+：Co2+According to 7:3 mol ratios are mixed, and cumulative volume 100ml, are subsequently placed in the pyroxylin film of conical flask pattern,
It is placed on after sealing in 250ml beakers.
Second step, 0.166g sodium carbonate is accurately weighed, 100ml solution, concentration 20mmol/ are configured to deionized water
L, then it is poured into the beaker of the first step and is sealed beaker mouth with preservative film and reacted.
3rd step, after reacting 20 minutes, collect the solution in pyroxylin film and precipitation is poured into 250 ml beakers, add
Enter magneton stirring to be placed in reaching steady temperature in 25 DEG C of water-bath.
4th step, 0.1079g potassium borohydride is accurately weighed, be configured to 100ml solution with deionized water, concentration is
20mmol/L, and put it into refrigerator and treat that it reaches 0 DEG C, then it is slowly added drop-wise in the beaker of the 3rd step and carried out instead
Should.
5th step, react 30 minutes, take out magneton, centrifuge and washed for several times with absolute ethyl alcohol and deionized water, be placed in true
Dried in empty drying box.
6th step, the powder sample that will be obtained after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to
400 DEG C and 1h is incubated, obtains final ultra-thin stratiform NiO-CoOxNanometer sheet loads the composite of NiCo nano-particles.
Fig. 9 is the SEM photograph for obtaining product in embodiment 4 under 500nm multiple.The NiO- it can be seen from picture
CoOxThe dimensional thinlayer structure of nanometer sheet can still be formed, but the particle diameter of NiCo nano-particles is bigger, be reunited more severe,
When illustrating that reduction temperature is higher, the increase of particle growth speed, it is easy to reunite.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using this hair
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to implementation here
Example, in the modification made without departing from the scope of the invention all within protection scope of the present invention.
Claims (10)
- A kind of 1. ultra-thin stratiform NiO-CoOxNanometer sheet loads the synthetic method of NiCo nano compositions, it is characterised in that Comprise the following steps that：（1）By Ni, Co inorganic salt solution is added in the pyroxylin film of conical flask pattern, is put into after sealing molten equipped with sodium carbonate Precipitation reaction is carried out in the beaker of liquid；The mol ratio of Ni, Co inorganic salts is 7:3；The molal quantity summation of the Ni, Co inorganic salts Mol ratio with sodium carbonate is 1:4；（2）With complete solution is not precipitated in reducing agent reduction pyroxylin film at 0~25 DEG C, reaction is carried out sample after terminating Centrifugation, wash, dry, calcining obtains final product, is ultra-thin stratiform NiO-CoOxNanometer sheet load NiCo nano-particles are answered Condensation material；Calcining is that 1 DEG C/min is warming up to 400 DEG C of insulation 1h in argon gas atmosphere.
- A kind of 2. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Ni is prepared, the solvent that Co inorganic salt solution uses is deionized water.
- A kind of 3. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（1）Described in Ni inorganic salts be nickel chloride, Co inorganic salts are cobalt chloride, its concentration It is 0.005~0.02mol/L.
- A kind of 4. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（1）Described in sodium carbonate liquor its concentration be 0.02~0.08mol/L.
- A kind of 5. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（1）Described in the precipitation reaction time be 20 minutes.
- A kind of 6. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（2）Described in reducing agent be the potassium borohydride aqueous solution, its concentration is 0.02~ 0.08mol/L。
- A kind of 7. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（2）Described in the reduction reaction time be 30 minutes.
- A kind of 8. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（2）Described in washing be using deionized water and absolute ethyl alcohol carry out alternately washing.
- A kind of 9. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（2）Described in centrifugation rotating speed be 6000 revs/min, the time be 5 minutes.
- A kind of 10. ultra-thin stratiform NiO-CoO according to claim 1xNanometer sheet load NiCo nano compositions Synthetic method, it is characterised in that：Step（2）Described in drying be that 10h is dried at 60 DEG C of vacuum drying chamber.
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| CN106925282A (en) * | 2017-03-02 | 2017-07-07 | 同济大学 | NiFe/CeO is obtained by topology reducing process in situ2The method of nano composite material |
| CN107398564B (en) * | 2017-07-25 | 2019-06-25 | 陕西师范大学 | A kind of preparation method of ultra-thin CoNi alloy nano piece |
| CN107597141B (en) * | 2017-08-22 | 2019-12-03 | 安徽师范大学 | Pd nano particle loads nanocomposite of layered double-hydroxide and preparation method thereof and ammonia borine catalytic decomposing method |
| CN112023931A (en) * | 2020-09-01 | 2020-12-04 | 上海应用技术大学 | Synthesis method of nickel-cobalt nano alloy particles with stable two-dimensional silicon dioxide nanobelt |
| CN114944492A (en) * | 2022-01-28 | 2022-08-26 | 上海应用技术大学 | Preparation method of two-dimensional ultrathin nano composite material |
| CN115155596B (en) * | 2022-07-25 | 2023-11-10 | 同济大学 | Preparation method and application of three-dimensional cluster structure re-CuFeNi-MMOs nanocomposite |
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| CN101736332B (en) * | 2009-12-09 | 2011-09-14 | 同济大学 | Method for synthesizing amorphous nickel-cobalt alloy nano-film loaded with platinum particles |
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