CN105692595A - Preparation method of layered nanoscale material - Google Patents
Preparation method of layered nanoscale material Download PDFInfo
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Abstract
The invention discloses a layered nanoscale material and a preparation method of a composite material thereof. The preparation method comprises the following three steps: firstly, uniformly mixing a layered polymer and a precursor of a layered material to be synthesized, and polymerizing the layered polymer precursor to obtain a layered compound; secondly, using the layered compound as a two-dimensional nanoreactor, and synthesizing the layered nanoscale material and its composite material through a nucleation growth mode under confinement and induction action of the two-dimensional confinement space; and finally, decomposing the layered polymer through high-temperature treatment to obtain the required layered material and its nanocomposite. The method has wide universality. The nanocomposite of the layered material containing graphene, doped graphene and transition metal carbide, nitride, phosphide, sulfide and boride can be prepared. The method is simple and feasible. The prepared layered material has a neat structure and has potential application value in application fields of catalysis, energy storage and the like.
Description
Technical field
The present invention relates to field of nano material preparation, more particularly to the preparation method of a kind of stratified nano materials。
Background technology
Graphene and nano composite material thereof, with the physical and chemical performance that it is superior, cause the extensive concern of academia and industrial circle, show good application prospect in fields such as catalysis, sensing, energy storage。
At present, the preparation method of Graphene mainly includes the chemical vapour deposition technique of " from top to bottom " and the physics of " from bottom to top " or chemical stripping method。The former is that the atmosphere utilizing carbon containing deposits at metallic catalyst surfaces, and Graphene both can have been obtained grapheme material from metal surface stripping by certain method by indigenous graphite olefinic carbon layer。This method is mainly for the preparation of high-quality grapheme material, but prepared by the batch being difficulty with Graphene。Physics stripping method from bottom to top is that graphite flake layer is peeled off by the method utilizing physics, and the high-quality Graphene of the equally possible acquisition of this method, preparation in macroscopic quantity is also highly difficult。The method being presently used for preparing Graphene on a large scale, realizes mainly by chemical stripping method。This method is to utilize chemical oxidization method to overcome the interaction between graphite flake layer, first obtains graphene oxide, is then reduced again and obtain grapheme material。Material preparation process involved by this method is more complicated, and has used the material such as strong acid, strong oxidizer, contaminated environment。
The preparation method that we have developed a kind of stratified nano materials。This method is based on the space confinement effect of Two dimensional layer polymer and prepares the synthetic method of a kind of new stratified nano materials of stratified nano materials。The method utilizes solid state reaction, simple to operate, technological process is short, easily batch amplifies, and this preparation method has universality widely, it is possible to prepare stratified material and include the nano composite material of Graphene, doped graphene and Graphene and transition metal carbide, nitride, phosphide, sulfide, boride。Prepared stratified material compound with regular structure, pattern are uniform, have potential using value in the application such as catalysis, energy storage。
Summary of the invention
The preparation method that the invention discloses a kind of stratified nano materials。This method is based on the space confinement effect of Two dimensional layer polymer and prepares the new method of stratified nano materials and composite thereof。Specifically, this preparation method is divided into three steps: first, by the presoma Homogeneous phase mixing of layered polymer and stratified material to be synthesized, and makes layered polymer presoma aggregate into lamellar compound at the temperature set；Secondly, with lamellar compound for two-dimensional nano reactor, under the confinement and inducing action of its two-dimensional confinement space, stratified nano materials and composite thereof are synthesized by the mode of nucleation and growth process；Finally, by high-temperature process, layered polymer is decomposed, it is thus achieved that required stratified material and nano composite material thereof。
The preparation method of a kind of stratified nano materials is based on Two dimensional layer polymer and prepares stratified nano materials。
The preparation method of layered nano material, pre-prepared including three below step, (1) Two dimensional layer polymer and stratified nano materials；(2) with Two dimensional layer polymer for two-dimensional nano reactor, stratified nano materials is synthesized at its interlayer；(3) decomposition of Two dimensional layer polymer。
Particularly as follows: Two dimensional layer polymer precursor and solubility carbon source are mixed by (1) Yu Shuizhong by a certain percentage, stir to mix homogeneously rotary evaporation and dry to obtain precipitate；(2) step (1) gained precipitate it is warmed up to 350-650 DEG C with the heating rate of 1-20 DEG C/min and is incubated 1-24 hour so that the polymerization of Two dimensional layer polymer presoma obtains g-C3N4Lamellar compound, soluble carbon is at this temperature at g-C simultaneously3N4Interlayer two-dimensional space in carbonization, form the Graphene of stratiform and g-C3N4Composite；(3) step (2) products therefrom high-temperature process under an inert atmosphere is obtained stratified nano materials。
Prepared stratified nano materials lamella is likely to be loaded with nano-particle。
The preparation method of the described stratified nano materials being loaded with nano-particle, including three below step, (1) Two dimensional layer polymer, stratified nano materials and nano-particle material pre-prepared；(2) with Two dimensional layer polymer for two-dimensional nano reactor, the stratified nano materials being loaded with nano-particle on nanoscale twins is synthesized at its interlayer；(3) decomposition of Two dimensional layer polymer。
Particularly as follows: Two dimensional layer polymer precursor, solubility carbon source, soluble metallic salt are mixed by (1) Yu Shuizhong by a certain percentage, stir to after being completely dissolved, obtaining mixed solution；In mixed solution, add acid source, stir to mix homogeneously rotary evaporation and dry to obtain precipitate；(2) step (1) gained precipitate it is warmed up to 350-650 DEG C with the heating rate of 1-20 DEG C/min and is incubated 1-24 hour so that the polymerization of Two dimensional layer polymer presoma obtains g-C3N4Lamellar compound, soluble carbon is at this temperature at g-C simultaneously3N4Interlayer two-dimensional space in carbonization, form Graphene and the g-C of the stratiform being loaded with nano-particle on nanoscale twins3N4Composite；(3) make step (2) products therefrom high-temperature process under an inert atmosphere nanoscale twins is loaded with the stratified nano materials of nano-particle。
Described Two dimensional layer polymer is g-C3N4。
Layered nano material is Graphene or doped graphene。
On described nanoscale twins, the nano-particle of load is one or more in transition metal carbide, transition metal nitride, transition metal phosphide, transient metal sulfide, transition metal boride。
The precursor of described Two dimensional layer polymer is one or more in carbamide, tripolycyanamide, nitrile amine。
Described solubility carbon source is one or more in glucose, sucrose, fructose, maltose, lactose, crystal sugar, chitosan, polyvinyl alcohol, Polyethylene Glycol, soluble starch。
Described soluble metallic salt is one or more in iron chloride, ferrous chloride, iron acetate, Ferrous acetate, cobaltous chloride, cobaltous acetate, Nickel dichloride., nickel acetate, manganese chloride, manganese acetate, zinc chloride, zinc acetate, molybdenum chloride, tungsten chloride, vanadium oxychloride, Chlorizate chromium。
Described acid source is one or more in phosphoric acid, phosphorus pentoxide, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, sodium phosphate, dibastic sodium phosphate, sodium dihydrogen phosphate, sulphuric acid, sulfur trioxide, sodium sulfate, potassium sulfate, copper sulfate, zinc sulfate, iron sulfate, boric acid, potassium borate, sodium borate。
The process of described high-temperature process is be warming up to 750-1100 DEG C with the heating rate of 1-20 DEG C/min to be incubated 1-24 hour。
Described inert atmosphere is one or more in nitrogen, argon or helium。
Carbon in described solubility carbon source is 1:10-1:100 with the mol ratio of nitrogen element in Two dimensional layer polymer precursor。
In described soluble metallic salt, metallic element is 1:1-1:50 with the mol ratio of carbon in Two dimensional layer polymer precursor；In described soluble metallic salt, metallic element is 1:0.1-1:10 with the mol ratio of the sulfonate groups in acid source。
In solubility carbon source in described mixed solution, the molar concentration of carbon is 0.01molL-1-2molL-1。
The present invention has universality widely, it is possible to prepares stratified material and includes the nano composite material of Graphene, doped graphene and Graphene and transition metal carbide, nitride, phosphide, sulfide, boride。The method is simple, it is easy to amplify。Prepared stratified material compound with regular structure, pattern are uniform, have potential using value in the application such as catalysis, energy storage。
Accompanying drawing explanation
Fig. 1: the electromicroscopic photograph of CoP/ grapheme material prepared by the method for employing embodiment 1；
Fig. 2: the electromicroscopic photograph of FeP/ grapheme material prepared by the method for employing embodiment 1；
Fig. 3: the electromicroscopic photograph of NiP/ grapheme material prepared by the method for employing embodiment 1；
Fig. 4: the electromicroscopic photograph of MnP/ grapheme material prepared by the method for employing embodiment 1；
Fig. 5: the electromicroscopic photograph of CrP/ grapheme material prepared by the method for employing embodiment 1；
Fig. 6: the electromicroscopic photograph of TiP/ grapheme material prepared by the method for employing embodiment 1。
Detailed description of the invention
Embodiment 1:
The preparation method of a kind of CoP/ grapheme material, comprises the following steps:
A () adds mol ratio in 95 DEG C of deionized waters is the nitrile amine of 40:1:0.001, crystal sugar and cobaltic chloride, stirs and obtains mixed solution after being completely dissolved；
B () adds the mol ratio of phosphoric acid, phosphate radical and nitrile amine in the described mixed solution of step (a) is 1:1, stirs to mix homogeneously rotary evaporation and dries；
C (), in tube furnace, under nitrogen protection, is warming up to 600 DEG C with 5 DEG C/min, be incubated 2 hours, be then warming up to 900 DEG C with 5 DEG C/min again, is incubated 2 hours, takes out to obtain CoP/ graphene composite material after cooling。
Prepared material, as it is shown in figure 1, material is macroscopically in block structure, is peeled off between lamella, and above load and lamella。
Embodiment 2:
The preparation method of a kind of MoP/ grapheme material, comprises the following steps,
A () adds mol ratio in 95 DEG C of deionized waters is the carbamide of 30:1:0.05, glucose and molybdenum pentachloride, stirs and obtains mixed solution after being completely dissolved；
B () adds the mol ratio of phosphoric acid, phosphate radical and carbamide in the described mixed solution of step (a) is 1:0.5, stirs to mix homogeneously rotary evaporation and dries；
C (), in tube furnace, under nitrogen protection, is warming up to 600 DEG C with 5 DEG C/min, be incubated 2 hours, be then warming up to 900 DEG C with 5 DEG C/min again, is incubated 2 hours, takes out to obtain MnP/ graphene composite material after cooling。
Prepared material, as in figure 2 it is shown, material presents the stripping film Rotating fields of proper alignment on the whole, has uniformly tiny nano-particle load herein above。
Embodiment 3:
The preparation method of a kind of NiP/ graphene composite material, comprises the following steps,
A () adds mol ratio in 95 DEG C of deionized waters is the carbamide of 30:1:0.05, glucose and Nickel Chloride, stirs and obtains mixed solution after being completely dissolved；
B () adds the mol ratio of phosphoric acid, phosphate radical and carbamide in the described mixed solution of step (a) is 1:0.5, stirs to mix homogeneously rotary evaporation and dries；
C (), in tube furnace, under nitrogen protection, is warming up to 600 DEG C with 5 DEG C/min, be incubated 2 hours, be then warming up to 900 DEG C with 5 DEG C/min again, is incubated 2 hours, takes out to obtain NiP/ graphene composite material after cooling。
Prepared material, as it is shown on figure 3, material presents the stripping film Rotating fields of proper alignment on the whole, has uniformly tiny nano-particle load herein above。
Embodiment 4:
The preparation method of a kind of MnS/ graphene composite material, comprises the following steps,
A () adds mol ratio in 95 DEG C of deionized waters is the carbamide of 30:1:0.05, glucose and manganese acetate, stirs and obtains mixed solution after being completely dissolved；
B () adds the mol ratio of sulphuric acid, phosphate radical and carbamide in the described mixed solution of step (a) is 1:0.5, stirs to mix homogeneously rotary evaporation and dries；
C (), in tube furnace, under nitrogen protection, is warming up to 600 DEG C with 5 DEG C/min, be incubated 2 hours, be then warming up to 900 DEG C with 5 DEG C/min again, is incubated 2 hours, takes out to obtain MnS/ graphene composite material after cooling。
As shown in Figure 4, material presents the stripping film Rotating fields of proper alignment to prepared material on the whole。
Embodiment 5:
The preparation method of a kind of CrN/ graphene composite material, comprises the following steps,
A () adds mol ratio in 95 DEG C of deionized waters is the carbamide of 30:1:0.05, glucose and manganese acetate, stirs and obtains mixed solution after being completely dissolved, and then rotary evaporation dries；
B (), in tube furnace, under nitrogen protection, is warming up to 600 DEG C with 5 DEG C/min, be incubated 2 hours, be then warming up to 900 DEG C with 5 DEG C/min again, is incubated 2 hours, takes out to obtain CrN/ graphene composite material after cooling。
Prepared material is as it is shown in figure 5, material presents the stripping film Rotating fields of proper alignment and the sandwich material of CrN on the whole。
Embodiment 6:
The preparation method of a kind of TiP/ graphene composite material, comprises the following steps,
A () adds mol ratio in 95 DEG C of deionized waters is the tripolycyanamide of 30:1:0.05, glucose and four chlorination bodies, stirs and obtains mixed solution after being completely dissolved；
B () adds the mol ratio of phosphoric acid, phosphate radical and carbamide in the described mixed solution of step (a) is 1:1, stirs to mix homogeneously rotary evaporation and dries；
C (), in tube furnace, under nitrogen protection, is warming up to 600 DEG C with 5 DEG C/min, be incubated 2 hours, be then warming up to 900 DEG C with 5 DEG C/min again, is incubated 2 hours, takes out to obtain TiP/ graphene composite material after cooling。
As shown in Figure 6, material presents the stripping film Rotating fields of proper alignment and the sandwich of TiP to prepared material on the whole。
Claims (14)
1. the preparation method of a stratified nano materials, it is characterised in that: the stratified nano materials being loaded with nano-particle on stratified nano materials or stratified nano materials lamella is prepared based on Two dimensional layer polymer；
The preparation of stratified nano materials includes three below step, (1) Two dimensional layer polymer and stratified nano materials pre-prepared；(2) with Two dimensional layer polymer for two-dimensional nano reactor, stratified nano materials is synthesized at its interlayer；(3) decomposition of Two dimensional layer polymer；
The preparation being loaded with the stratified nano materials of nano-particle on stratified nano materials lamella includes three below step, (1) Two dimensional layer polymer, stratified nano materials and nano-particle material pre-prepared；(2) with Two dimensional layer polymer for two-dimensional nano reactor, the stratified nano materials being loaded with nano-particle on nanoscale twins is synthesized at its interlayer；(3) decomposition of Two dimensional layer polymer。
2. the preparation method of as claimed in claim 1 stratified nano materials, it is characterised in that: three steps of layered preparation method of nano material specifically,
(1) Two dimensional layer polymer precursor and solubility carbon source are mixed by Yu Shuizhong, stir to mix homogeneously evaporation drying and obtain precipitate；
(2) step (1) gained precipitate it is warmed up to 350-650 DEG C and is incubated 1-24 hour, obtaining Two dimensional layer polymer and the stratified nano materials of Two dimensional layer polymer interlayer；
(3) step (2) products therefrom high-temperature process under an inert atmosphere is obtained stratified nano materials。
3. the preparation method of as claimed in claim 1 stratified nano materials, it is characterised in that: layered nano material lamella is loaded with three steps of the preparation method of the stratified nano materials of nano-particle specifically,
(1) Yu Shuizhong is by Two dimensional layer polymer precursor, solubility carbon source, soluble metallic salt mixing, stirs to after being completely dissolved, obtaining mixed solution；In mixed solution, add acid source, stir to mix homogeneously evaporation drying and obtain precipitate；
(2) step (1) gained precipitate it is warmed up to 350-650 DEG C and is incubated 1-24 hour, obtaining the stratified nano materials being loaded with nano-particle on the nanoscale twins of Two dimensional layer polymer and Two dimensional layer polymer interlayer；
(3) step (2) products therefrom high-temperature process under an inert atmosphere is obtained the stratified nano materials being loaded with nano-particle on nanoscale twins。
4. the preparation method of the arbitrary layered nano material of claim 1-3, it is characterised in that: described Two dimensional layer polymer is g-C3N4。
5. the preparation method of layered nano material as arbitrary in claim 1-3, it is characterised in that: layered nano material is Graphene or doped graphene。
6. the preparation method of nano material as layered in claim 1 or 3, it is characterised in that: on described nanoscale twins, the nano-particle of load is one or more in transition metal carbide, transition metal nitride, transition metal phosphide, transient metal sulfide, transition metal boride。
7. the preparation method of nano material as layered in Claims 2 or 3, it is characterised in that: the precursor of Two dimensional layer polymer described in step (1) is one or more in carbamide, tripolycyanamide, nitrile amine；Solubility carbon source described in step (1) is one or more in glucose, sucrose, fructose, maltose, lactose, crystal sugar, chitosan, polyvinyl alcohol, Polyethylene Glycol, soluble starch。
8. the preparation method of stratified nano materials as claimed in claim 3, it is characterised in that: soluble metallic salt described in step (1) is one or more in iron chloride, ferrous chloride, iron acetate, Ferrous acetate, cobaltous chloride, cobaltous acetate, Nickel dichloride., nickel acetate, manganese chloride, manganese acetate, zinc chloride, zinc acetate, molybdenum chloride, tungsten chloride, vanadium oxychloride, Chlorizate chromium；
Acid source described in step (1) is one or more in phosphoric acid, phosphorus pentoxide, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, sodium phosphate, dibastic sodium phosphate, sodium dihydrogen phosphate, sulphuric acid, sulfur trioxide, sodium sulfate, potassium sulfate, copper sulfate, zinc sulfate, iron sulfate, boric acid, potassium borate, sodium borate。
9. the preparation method of nano material as layered in Claims 2 or 3, it is characterised in that: in described step (2), the heating rate from room temperature is 1-20 DEG C/min。
10. the preparation method of nano material as layered in Claims 2 or 3, it is characterised in that: the process of high-temperature process described in step (3) is be warming up to 750-1100 DEG C with the heating rate of 1-20 DEG C/min from room temperature to be incubated 1-24 hour。
11. the preparation method of nano material as layered in Claims 2 or 3, it is characterised in that: inert atmosphere described in step (3) is one or more in nitrogen, argon or helium。
12. the preparation method of nano material as layered in Claims 2 or 3, it is characterised in that: the carbon in solubility carbon source described in step (1) is 1:10-1:100 with the mol ratio of nitrogen element in Two dimensional layer polymer precursor。
13. the preparation method of stratified nano materials as claimed in claim 3, it is characterised in that: in soluble metallic salt described in step (1), metallic element is 1:1-1:50 with the mol ratio of carbon in Two dimensional layer polymer precursor；In described soluble metallic salt, metallic element is 1:0.1-1:10 with the mol ratio of the sulfonate groups in acid source。
14. the preparation method of nano material as layered in Claims 2 or 3, it is characterised in that: in the solubility carbon source in mixed solution described in step (1), the molar concentration of carbon is 0.01molL-1-2molL-1。
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