CN105834446A - Synthetic method for ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite - Google Patents
Synthetic method for ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite Download PDFInfo
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- CN105834446A CN105834446A CN201610221985.XA CN201610221985A CN105834446A CN 105834446 A CN105834446 A CN 105834446A CN 201610221985 A CN201610221985 A CN 201610221985A CN 105834446 A CN105834446 A CN 105834446A
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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 invention relates to a synthetic method for an ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite. The method specifically comprises the steps that firstly, an inorganic salt solution of Ni and an inorganic salt solution of Co are added into a collodion film in a conical flask form, and the collodion film is sealed and put into a beaker with a sodium carbonate solution for a precipitation reaction; and secondly, a reducing agent is used for reducing solutions, which are not reacted completely, in the collodion film at the certain temperature, a sample is subjected to centrifugation, washing, drying and roasting after the reaction, and a final product, namely the ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite is obtained. The method is used for preparing the nano composite with the large specific surface area and good magnetism and catalytic activity. The method is simple, easy to operate and control, simple in product processing and suitable for medium scale industrial production.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, particularly relate to a kind of ultra-thin stratiform NiO-CoOxThe synthetic method of nanometer sheet load NiCo nano composition.
Background technology
Electricity, magnetics and optical property excellent under microcosmic can organically be combined by two-dimensional ultrathin nanometer sheet with ultra-thin property, the transparency and the pliability under macroscopic view such that it is able to realize device miniaturization and function maximizes perfect unity.Two-dimension nano materials is different from the electronic structure of respective masses material because the feature of its gauge and two-dimension plane structure often has, it is not only able to affect its intrinsic performance, some new properties can also be produced, it has the highest theoretical specific surface area and electron mobility simultaneously so that it rapidly becomes the study hotspot that material science and chemical field are active.Nanoalloy particle can improve the performance of material further with being combined of dimensional thinlayer oxide, significantly widen the range of application of inorganic metal nanoparticle and metal-oxide.Nanoalloy particle modifies dimensional thinlayer oxide, and this is possible not only to overcome Van der Waals force huge between nanoscale twins, prevents the reunion of nanometer sheet, makes the peculiar property of the ultra-thin layer structure of metal-oxide be retained.Meanwhile, its many performances of the composite obtained are more superior than alloy, have important using value at aspects such as chemically modified electrode, electrochmical power source, caltalyst and gas sensors.By ultra-thin stratiform NiO-CoO in this experimentxNanometer sheet and NiCo nanoparticle are effectively combined, and form two-dimensional nano composite construction, first, ultra-thin stratiform NiO-CoOxNanometer sheet surface has a large amount of undersaturated negative oxygen ion of low coordination can be the Compounds with Hydrazine Hydrate Catalyzed decomposition product hydrogen substantial amounts of basic site of offer thus improves the selectivity of reaction；Secondly, the synergism of NiCo alloy can be greatly improved the activity of catalytic reaction；Again, this two-dimensional film structure has bigger specific surface area, is provided that the avtive spot of more catalytic reaction, improves catalytic efficiency.
Summary of the invention
It is an object of the invention to provide a kind of ultra-thin stratiform NiO-CoOxThe synthetic method of nanometer sheet load NiCo nano composition.
To achieve these goals, technical scheme is as follows:
The synthetic method of a kind of ultra-thin stratiform NiO-CoOx nanometer sheet load NiCo nano composition that the present invention proposes, specifically comprises the following steps that
(1) by Ni, the inorganic salt solution of Co joins in the pyroxylin film of conical flask pattern, puts into equipped with carrying out precipitation in the beaker of sodium carbonate liquor after sealing；The mol ratio of the inorganic salt of Ni, Co is 7:3；The molal quantity summation of described Ni, Co inorganic salt and the mol ratio of sodium carbonate are 1:4；
(2) not precipitating solution completely in reducing agent reduction pyroxylin film at 0～25 DEG C, sample is centrifuged after terminating by reaction, and washing is dried, and calcining obtains final product, loads NiCo nano composition for ultra-thin stratiform NiO-CoOx nanometer sheet.
In the present invention, the solvent that the inorganic salt solution of preparation Ni, Co uses is deionized water.
In the present invention, described in step (1), the inorganic salt of Ni is Nickel dichloride., and the inorganic salt of Co is cobaltous chloride, and its concentration is 0.005～0.02mol/L.
In the present invention, described in step (1), its concentration of sodium carbonate liquor is 0.02～0.08mol/L.
In the present invention, the precipitation time described in step (1) is 20 minutes.
In the present invention, the reducing agent described in step (2) is potassium borohydride aqueous solution, and its concentration is 0.02～0.08mol/L.
In the present invention, the reduction reaction time described in step (2) is 30 minutes.
In the present invention, the washing described in step (2) is all to use deionized water and dehydrated alcohol alternately to wash.
In the present invention, the centrifugation rotating speed described in step (2) is 6000 revs/min, and the time is 5 minutes.
In the present invention, dry described in step (2) is to be dried 10h at 60 DEG C of vacuum drying oven.
In the present invention, the calcining described in step (2) is that 1 DEG C/min is warming up to 400 DEG C of insulation 1h in argon gas atmosphere.
Owing to using such scheme, the method have the advantages that
1, present invention achieves to utilize and achieve the presoma utilizing common Nickel dichloride., cobaltous chloride to be reaction, by co-precipitation-reducing process, synthesized ultra-thin stratiform NiO-CoO firstxThe composite of nanometer sheet load NiCo nanoparticle.
2, the method for the present invention has the highest control to the pattern of product.
3, the present invention uses simple inorganic salt as reactant, has the strongest versatility.
4, product prepared by the present invention has the performance of good Compounds with Hydrazine Hydrate Catalyzed decomposition product hydrogen, can have more vast potential for future development and application space as high performance catalyst.
5, the technique of the present invention is simple, and preparation condition is general, and product morphology is stable, purity is high, and product processes convenient succinct, is suitable for medium-scale commercial production.
6, the method for the present invention has mild condition, efficient energy-saving, the feature such as easily controllable.
Accompanying drawing explanation
Fig. 1 is the SEM photograph of the intermediate product obtained under the multiple of 500nm in embodiment 1.
Fig. 2 is the SEM photograph of the product obtained under the multiple of 200nm in embodiment 1.
Fig. 3 is the TEM photo of the intermediate product obtained under the multiple of 20nm in embodiment 1.
Fig. 4 is the TEM photo of the product obtained under the multiple of 50nm in embodiment 1.
Fig. 5 is the XRD figure spectrum of embodiment 1 products therefrom and intermediate product.
Fig. 6 is the EDS collection of illustrative plates of embodiment 1 products therefrom and intermediate product.
Fig. 7 is the SEM photograph of the intermediate product obtained under the multiple of 500nm in embodiment 2.
Fig. 8 is the SEM photograph of the intermediate product obtained under the multiple of 500nm in embodiment 3.
Fig. 9 is the SEM photograph of the product obtained under the multiple of 500nm in embodiment 4.
Detailed description of the invention
The present invention is further detailed explanation for illustrated embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The first step, accurately weighs 0.1185gNiCl2·6H2O, is configured to 100ml solution with deionized water, and concentration is 5mmol/L, accurately weighs 0.1189gCoCl2·2H2O, is configured to 100ml solution with deionized water, and concentration is 5mmol/L, Ni2+: Co2+Mixing according to 7:3 mol ratio, cumulative volume is 100ml, is subsequently placed in the pyroxylin film of conical flask pattern, is placed in 250ml beaker after sealing.
Second step, accurately weighs the sodium carbonate of 0.166g, is configured to 100ml solution with deionized water, and concentration is 20mmol/L, is then poured in the beaker of the first step and is sealed by beaker mouth with preservative film and reacts.
3rd step, after reacting 20 minutes, collects the solution in pyroxylin film and precipitation is poured in 250 ml beakers, adds magneton stirring and is placed in mixture of ice and water reaching 0 DEG C.
4th step, accurately weighs the potassium borohydride of 0.1079g, is configured to 100ml solution with deionized water, and concentration is 20mmol/L, and puts it into and treat in refrigerator that it reaches 0 DEG C, is then added drop-wise to it slowly in beaker of the 3rd step react.
5th step, reacts 30 minutes, takes out magneton, centrifugal and with dehydrated alcohol and deionized water wash for several times, is placed in vacuum drying oven dry.
6th step, the powder sample that will obtain after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to 400 DEG C and is incubated 1h, obtains final ultra-thin stratiform NiO-CoOxThe composite of nanometer sheet load NiCo nanoparticle.
Fig. 1 is the intermediate product NiO-CoO obtained under the multiple of 200nm in embodiment 1xThe SEM picture of nanometer sheet；Fig. 2 is the SEM picture of the product obtained under the multiple of 500nm in embodiment 1；Fig. 3 is embodiment 1 gained intermediate product NiO-CoOxThe TEM picture of nanometer sheet；Fig. 4 is the TEM picture of embodiment 1 products therefrom；Fig. 5 is the XRD figure spectrum of embodiment 1 products therefrom (a) and intermediate product (b), it was demonstrated that NiO-CoOxNanometer sheet and NiCo nanoparticle compound；Fig. 6 is that in embodiment 1, the EDS collection of illustrative plates of product (a) and intermediate product (b) indicates wherein Ni, the existence of Co, O element, and in product, the atomic ratio of oxygen, less than intermediate product, has proved the synthesis of composite further simultaneously.
Embodiment 2
The first step, accurately weighs 0.2370gNiCl2·6H2O, is configured to 100ml solution with deionized water, and concentration is 10mmol/L, accurately weighs 0.2378gCoCl2·2H2O, is configured to 100ml solution with deionized water, and concentration is 10mmol/L, Ni2+: Co2+Mixing according to 7:3 mol ratio, cumulative volume is 100ml, is subsequently placed in the pyroxylin film of conical flask pattern, is placed in 250ml beaker after sealing.
Second step, accurately weighs the sodium carbonate of 0.332g, is configured to 100ml solution with deionized water, and concentration is 40mmol/L, is then poured in the beaker of the first step and is sealed by beaker mouth with preservative film and reacts.
3rd step, after reacting 20 minutes, collects the solution in pyroxylin film and precipitation is poured in 250 ml beakers, adds magneton stirring and is placed in mixture of ice and water reaching 0 DEG C.
4th step, accurately weighs the potassium borohydride of 0.2158g, is configured to 100ml solution with deionized water, and concentration is 40mmol/L, and puts it into and treat in refrigerator that it reaches 0 DEG C, is then added drop-wise to it slowly in beaker of the 3rd step react.
5th step, reacts 30 minutes, takes out magneton, centrifugal and with dehydrated alcohol and deionized water wash for several times, is placed in vacuum drying oven dry.
6th step, the powder sample that will obtain after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to 400 DEG C and is incubated 1h, obtains final ultra-thin stratiform NiO-CoOxThe composite of nanometer sheet load NiCo nanoparticle.
Fig. 7 is the intermediate product NiO-CoO obtained under the multiple of 500nm in embodiment 2xThe SEM photograph of nanometer sheet.By picture it can be seen that the most still can form dimensional thinlayer structure, simply the amount of crimp of thin film is relatively big, and the surface area that compares is less.
Embodiment 3
The first step, accurately weighs 0.4740gNiCl2·6H2O, is configured to 100ml solution with deionized water, and concentration is 20mmol/L, accurately weighs 0.4756gCoCl2·2H2O, is configured to 100ml solution with deionized water, and concentration is 20mmol/L, Ni2+: Co2+Mixing according to 7:3 mol ratio, cumulative volume is 100ml, is subsequently placed in the pyroxylin film of conical flask pattern, is placed in 250ml beaker after sealing.
Second step, accurately weighs the sodium carbonate of 0.664g, is configured to 100ml solution with deionized water, and concentration is 80mmol/L, is then poured in the beaker of the first step and is sealed by beaker mouth with preservative film and reacts.
3rd step, after reacting 20 minutes, collects the solution in pyroxylin film and precipitation is poured in 250 ml beakers, adds magneton stirring and is placed in mixture of ice and water reaching 0 DEG C.
4th step, accurately weighs the potassium borohydride of 0.4316g, is configured to 100ml solution with deionized water, and concentration is 80mmol/L, and puts it into and treat in refrigerator that it reaches 0 DEG C, is then added drop-wise to it slowly in beaker of the 3rd step react.
5th step, reacts 30 minutes, takes out magneton, centrifugal and with dehydrated alcohol and deionized water wash for several times, is placed in vacuum drying oven dry.
6th step, the powder sample that will obtain after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to 400 DEG C and is incubated 1h, obtains final ultra-thin stratiform NiO-CoOxThe composite of nanometer sheet load NiCo nanoparticle.
Fig. 8 is the intermediate product NiO-CoO obtained under the multiple of 500nm in embodiment 3xThe SEM photograph of nanometer sheet.By picture it can be seen that the laminate structure formed with this understanding is not it is obvious that be more likely to multi-level flower-like structure, after illustrating that reactant concentration improves, the speed of growth is accelerated to be difficult to generate dimensional thinlayer structure.
Embodiment 4
The first step, accurately weighs 0.1185gNiCl2·6H2O, is configured to 100ml solution with deionized water, and concentration is 5mmol/L, accurately weighs 0.1189gCoCl2·2H2O, is configured to 100ml solution with deionized water, and concentration is 5mmol/L, Ni2+: Co2+Mixing according to 7:3 mol ratio, cumulative volume is 100ml, is subsequently placed in the pyroxylin film of conical flask pattern, is placed in 250ml beaker after sealing.
Second step, accurately weighs the sodium carbonate of 0.166g, is configured to 100ml solution with deionized water, and concentration is 20mmol/L, is then poured in the beaker of the first step and is sealed by beaker mouth with preservative film and reacts.
3rd step, after reacting 20 minutes, collects the solution in pyroxylin film and precipitation is poured in 250 ml beakers, adds magneton stirring and is placed in the water-bath of 25 DEG C reaching steady temperature.
4th step, accurately weighs the potassium borohydride of 0.1079g, is configured to 100ml solution with deionized water, and concentration is 20mmol/L, and puts it into and treat in refrigerator that it reaches 0 DEG C, is then added drop-wise to it slowly in beaker of the 3rd step react.
5th step, reacts 30 minutes, takes out magneton, centrifugal and with dehydrated alcohol and deionized water wash for several times, is placed in vacuum drying oven dry.
6th step, the powder sample that will obtain after drying, it is placed in tube furnace in argon gas atmosphere, 1 DEG C/min is warming up to 400 DEG C and is incubated 1h, obtains final ultra-thin stratiform NiO-CoOxThe composite of nanometer sheet load NiCo nanoparticle.
Fig. 9 is the SEM photograph obtaining product in embodiment 4 under the multiple of 500nm.By picture it can be seen that NiO-CoOxThe dimensional thinlayer structure of nanometer sheet still can be formed, but the particle diameter of NiCo nanoparticle is bigger, reunites more severe, illustrates when reduction temperature is higher, and particle growth speed increases, it is easy to reunites.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply the present invention.These embodiments obviously easily can be made various amendment by person skilled in the art, and General Principle described herein is applied in other embodiments without through performing creative labour.Therefore, the invention is not restricted to embodiment here, in the amendment made without departing from the scope of the invention all within protection scope of the present invention.
Claims (11)
1. ultra-thin stratiform NiO-CoOxThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that specifically comprise the following steps that
(1) by Ni, the inorganic salt solution of Co joins in the pyroxylin film of conical flask pattern, puts into equipped with carrying out precipitation in the beaker of sodium carbonate liquor after sealing；The mol ratio of the inorganic salt of Ni, Co is 7:3；The molal quantity summation of described Ni, Co inorganic salt and the mol ratio of sodium carbonate are 1:4；
(2) not precipitating solution completely in reducing agent reduction pyroxylin film at 0～25 DEG C, sample is centrifuged after terminating by reaction, and washing is dried, and calcining obtains final product, for ultra-thin stratiform NiO-CoOxNanometer sheet load NiCo nano composition.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: the solvent that the inorganic salt solution of preparation Ni, Co uses is deionized water.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: described in step (1), the inorganic salt of Ni is Nickel dichloride., and the inorganic salt of Co is cobaltous chloride, and its concentration is 0.005～0.02mol/L.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: described in step (1), its concentration of sodium carbonate liquor is 0.02～0.08mol/L.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: the precipitation time described in step (1) is 20 minutes.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: the reducing agent described in step (2) is potassium borohydride aqueous solution, and its concentration is 0.02～0.08mol/L.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: the reduction reaction time described in step (2) is 30 minutes.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: the washing described in step (2) is all to use deionized water and dehydrated alcohol alternately to wash.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: the centrifugation rotating speed described in step (2) is 6000 revs/min, and the time is 5 minutes.
Ultra-thin stratiform NiO-CoO of one the most according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: dry described in step (2) is to be dried 10h at 60 DEG C of vacuum drying oven.
11. ultra-thin stratiforms NiO-CoO of one according to claim 1xThe synthetic method of nanometer sheet load NiCo nano composition, it is characterised in that: the calcining described in step (2) is that 1 DEG C/min is warming up to 400 DEG C of insulation 1h in argon gas atmosphere.
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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 |
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| CN107597141A (en) * | 2017-08-22 | 2018-01-19 | 安徽师范大学 | Nano composite material of Pd nano particle load 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 |
| CN115155596A (en) * | 2022-07-25 | 2022-10-11 | 同济大学 | Preparation method and application of three-dimensional cluster-structured re-CuFeNi-MMOs nano composite material |
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