CN108161021A - A kind of ice is mutually sustained the method for preparing atom level dispersion - Google Patents
A kind of ice is mutually sustained the method for preparing atom level dispersion Download PDFInfo
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- CN108161021A CN108161021A CN201711228353.7A CN201711228353A CN108161021A CN 108161021 A CN108161021 A CN 108161021A CN 201711228353 A CN201711228353 A CN 201711228353A CN 108161021 A CN108161021 A CN 108161021A
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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
- 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 belongs to Materials Science and Engineering technology and chemical fields, and in particular to a kind of ice is mutually sustained the method for preparing atom level dispersion, includes the following steps：(1) reactant solution A is made into presoma and solvent, the presoma is the monoatomic compound of metal；(2) it is made into reactant solution B with reducing agent and solvent；(3) reactant solution A prepared by above-mentioned steps (1) is frozen into ice cube, the ice cube is placed into reactant solution B, or reactant solution B prepared by step (2) is frozen into ice cube, and the ice cube is placed into reactant solution A；The ice cube is allowed slowly to melt and react to each other, obtains atom level dispersed metal material.The present invention have many advantages, such as quick, high density, it is a large amount of, efficient, have a wide range of application, relative to the methods of co-precipitation and infusion process with significant advantage.
Description
Technical field
The invention belongs to Materials Science and Engineering technology and chemical fields, and in particular to ice, which is mutually sustained, prepares atom level dispersion
The method of material,.
Background technology
Solution synthesis be it is a kind of prepare nanocrystalline universal method, wherein it is most crucial the problem of be how to effectively control its into
Core and growth course.100 for many years, and nanocrystalline nucleation and growth course get more and more people's extensive concerning and study.Example
Such as, nearest Mirsaidov etc. observes nanocrystalline forming process in the solution using in situ TEM：1. solution is spontaneously
It is decomposed into high concentration phase and low concentration phase；2. single aggressiveness is mutually nucleated in high concentration, small cluster is formed；3. non-crystal crystallization is receives
Meter Jing.From a large amount of experiment and research, we obtain：Concentration significantly affects nanocrystalline nucleation and growth course.Pass through
The concentration of reactant is reduced, can effectively inhibit the nucleation and growth course of solid product.People have also recognized that how to turn
The concentration, kinetics and thermodynamics of reactions of reaction can be directly affected by moving reactant.The mixed on low speed of reactant solution is one
The method that kind effectively controls its concentration, such as micro-fluidic engineering just can significantly control the rate of release of reactant.Use miniflow
It controls equipment and spreads dimension etc. by creating local low concentration, increasing specific surface area and reduction and then control quality and the biography of heat transfer
Material that is defeated and reducing chemical reaction practice, preparation nanometer or sub-nanometer.But further the concentration of control reactant is so as to more
It is still a huge challenge effectively to control nanocrystalline nucleating growth process.
When the size of material is reduced to nanometer scale, then reduce size from the nanometer scale limit from block, what is obtained will be
Atom one by one.The material of this atom level dispersion can become monatomic material.With conventional blocks material and nano material ratio
Compared with the material of atom level dispersion not only significantly reduces the cost of material, also has more excellent performance.It is for example, monatomic
Catalyst not only has higher catalytic activity, also with higher catalytic selectivity.For metal is monatomic, each of which
Metallic atom can serve as active site so as to fulfill its high catalytic activity.But the material of atom level dispersion, it is contemplated that single
The high surface of atom metal and high unstability, efficiently extensive prepare is still problem.
Invention content
The method for preparing atom level dispersion is mutually sustained the purpose of the present invention is to propose to a kind of ice, to conventional wet chemical method
It is improved, using the method for ice-out slow release reactant, it is diversified effectively simply to prepare a large amount of high quality
Atom level dispersion significantly reduces the cost of noble metal catalyst.
Technical scheme is as follows：
A kind of ice is mutually sustained the method for preparing atom level dispersion, which is characterized in that this method includes the following steps：
(1) reactant solution A is made into presoma and solvent, the presoma is the monoatomic compound of metal；
(2) it is made into reactant solution B with reducing agent and solvent；
(3) reactant solution A prepared by above-mentioned steps (1) is frozen into ice cube, the ice cube is placed into reactant solution B
In or step (2) prepare reactant solution B be frozen into ice cube, the ice cube is placed into reactant solution A；Allow the ice
Block slowly melts and reacts to each other, and obtains atom level dispersed metal material.
Further, in above-mentioned method：
(1) the reactant solution A for being made into that quality-volumetric concentration is 0.01-60mg/ml with presoma and solvent, it is described
Presoma is the monoatomic compound of metal, and the compound is inorganic salts, preferably chloride, sulfate or nitrate；It is described
Metal it is monatomic any one of for Fe, Co, Ni, Cu, Ru, Rh, Pd, Ag, Os, Ir, Pt and Au, the solvent is
Any one of water, ethylene glycol, ethyl alcohol, tetraethylene-glycol, dimethylformamide or formaldehyde；
(2) the reactant solution B for being made into that quality-volumetric concentration is 0.01-100mg/ml with reducing agent and solvent, it is described
Reducing agent has NaBH4,KBH4,N2H4,N2H5OH, formaldehyde, formic acid, ascorbic acid, Na2SO3,K2SO3,H2C2O4Deng any one
Kind, the solvent is any one of water, ethylene glycol, ethyl alcohol, tetraethylene-glycol, dimethylformamide or formaldehyde；
(3) reactant solution A (or reactant solution B) prepared by above-mentioned steps (1) is frozen into ice cube, and placed
Into reactant solution B (or reactant solution A), it is allowed slowly to melt and react to each other, just obtain monodispersed metal
Atom solution.Melt temperature and reaction temperature are consistent, ranging from -30-10 DEG C；
Slow release reactant proposed by the present invention and the method for preparing atom level dispersion, advantage are：The present invention
Method can not only effectively control nucleation and growth course in wet chemistry method, and can obtain quick, efficient and applicable model
Wide high quality monodisperse material is enclosed, preparation process is simple, easy to operate.The present invention can prepare the various gold of atom level dispersion
Belong to material, such as Fe, Co, Ni, Cu, Ru, Rh, Pd, Ag, Os, Ir, Pt and Au of atom level dispersion.
Description of the drawings
Fig. 1 is the scanning transmission electron microscope figure of the Ag of atom level dispersion prepared by the method for the present invention.
Specific embodiment
Below in conjunction with the accompanying drawings, the present invention is described in more detail.
Embodiment 1
The preparation of the Fe materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses FeCl2The FeCl of 3mg/ml is made into deionized water2Solution.Use liquid
Reactant solution A is rapidly frozen into ice cube by nitrogen.Then, the reactant solution B of needs is configured, uses NaBH4Match with deionized water
Into the NaBH of 3mg/ml4Solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting, i.e.,
The Fe of atom level dispersion can be obtained.
Embodiment 2
The preparation of the Fe of atom level dispersion.
First, the reactant solution A of needs is configured, with Fe (NO3)2Fe (the NO of 0.1mg/ml are made into ethyl alcohol3)2Solution.
Then, the reactant solution B of needs is configured, uses N2H5OH and deionized water are made into the N of 0.5mg/ml2H5OH solution.It will with liquid nitrogen
Reactant solution B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in -15 DEG C.Treat ice
Block melts, you can obtains the Fe of atom level dispersion
Embodiment 3
The preparation of the Fe of atom level dispersion.
First, the reactant solution A of needs is configured, uses FeSO4The FeSO of 30mg/ml is made into ethyl alcohol4Solution.Then, match
The reactant solution B of needs is put, uses KBH4The KBH of 50mg/ml is made into deionized water4Solution.With liquid nitrogen by reactant solution B
It is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 5 DEG C.It treats ice melting, you can obtain
Obtain the Fe of atom level dispersion
Embodiment 4
The preparation of the Co materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses CoCl2The CoCl of 2mg/ml is made into deionized water2Solution.Use liquid
Reactant solution A is rapidly frozen into ice cube by nitrogen.Then, the reactant solution B of needs is configured, uses NaBH4Match with deionized water
Into the NaBH of 4mg/ml4Solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting, i.e.,
The Co of atom level dispersion can be obtained.
Embodiment 5
The preparation of the Co materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses C4H6CoO4It is made into 0.5mg/ml's with tetraethylene-glycol
C4H6CoO4Solution.Then, the reactant solution B of needs is configured, uses N2H5OH and deionized water are made into the N of 0.5mg/ml2H5OH
Solution.Reactant solution B is rapidly frozen into ice cube with liquid nitrogen.Ice cube is placed into reactant solution A, it is allowed in -10 DEG C
Slowly melt.It treats ice melting, you can obtain the Co of atom level dispersion.
Embodiment 6
The preparation of the Co materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses CoSO4The CoSO of 20mg/ml is made into ethylene glycol4Solution.Then,
The reactant solution B needed is configured, uses KBH4The KBH of 40mg/ml is made into deionized water4Solution.With liquid nitrogen by reactant solution
B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 5 DEG C.It treats ice melting, you can obtain
Obtain the Co of atom level dispersion.
Embodiment 7
The preparation of the Ni materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses NiCl2The NiCl of 2mg/ml is made into deionized water2Solution.Use liquid
Reactant solution A is rapidly frozen into ice cube by nitrogen.Then, the reactant solution B of needs is configured, uses NaBH4Match with deionized water
Into the NaBH of 4mg/ml4Solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting, i.e.,
The Ni of atom level dispersion can be obtained.
Embodiment 8
The preparation of the Ni materials of atom level dispersion.
First, the reactant solution A of needs is configured, with Ni (NO3)2The Ni of 0.5mg/ml is made into dimethylformamide
(NO3)2Solution.Then, the reactant solution B of needs is configured, uses N2H5OH and deionized water are made into the N of 0.5mg/ml2H5OH is molten
Liquid.Reactant solution B is rapidly frozen into ice cube with liquid nitrogen.Ice cube is placed into reactant solution A, allows it slow in -10 DEG C
It is slow to melt.It treats ice melting, you can obtain the Ni of atom level dispersion.
Embodiment 9
The preparation of the Ni materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses NiSO4The NiSO of 20mg/ml is made into ultra-pure water4Solution.Then,
The reactant solution B needed is configured, uses KBH4The KBH of 40mg/ml is made into deionized water4Solution.With liquid nitrogen by reactant solution
B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 5 DEG C.It treats ice melting, you can obtain
Obtain the Ni of atom level dispersion.
Embodiment 10
The preparation of the Cu materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses CuCl2The CuCl of 2mg/ml is made into deionized water2Solution.Use liquid
Reactant solution A is rapidly frozen into ice cube by nitrogen.Then, the reactant solution B of needs is configured, uses NaBH4Match with deionized water
Into the NaBH of 4mg/ml4Solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting, i.e.,
The Cu of atom level dispersion can be obtained.
Embodiment 11
The preparation of the Cu materials of atom level dispersion.
First, the reactant solution A of needs is configured, with Cu (NO3)2Cu (the NO of 0.5mg/ml are made into ethyl alcohol3)2Solution.
Then, the reactant solution B of needs is configured, uses KBH4The KaBH of 0.5mg/ml is made into deionized water4Solution.It will be anti-with liquid nitrogen
Object solution B is answered to be rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in -10 DEG C.Treat ice cube
Melt, you can obtain the Cu of atom level dispersion.
Embodiment 12
The preparation of the Cu materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses CuSO4The CuSO of 20mg/ml is made into formaldehyde4Solution.Then, match
The reactant solution B of needs is put, uses N2H5OH and deionized water are made into the N of 40mg/ml2H5OH solution.It is with liquid nitrogen that reactant is molten
Liquid B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 5 DEG C.It treats ice melting, you can
Obtain the Cu of atom level dispersion.
Embodiment 13
The preparation of the Ru materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses C6H9O6Ru and deionized water are made into the C of 2mg/ml6H9O6Ru is molten
Liquid.Reactant solution A is rapidly frozen into ice cube with liquid nitrogen.Then, the reactant solution B of needs is configured, uses NaBH4With go from
Sub- water is made into the NaBH of 4mg/ml4Solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat ice cube
Melt, you can obtain the Ru of atom level dispersion.
Embodiment 14
The preparation of the Ru materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses RuCl3The RuCl of 0.5mg/ml is made into ethyl alcohol3Solution.Then,
The reactant solution B needed is configured, uses N2H5OH and deionized water are made into the N of 0.5mg/ml2H5OH solution.It will be reacted with liquid nitrogen
Object solution B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in -10 DEG C.Treat that ice cube melts
Change, you can obtain the Ru of atom level dispersion.
Embodiment 15
The preparation of the Ru materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses RuCl3The RuCl of 20mg/ml is made into ethylene glycol3Solution.Then,
The reactant solution B needed is configured, uses KBH4The KBH of 40mg/ml is made into ultra-pure water4Solution.With liquid nitrogen by reactant solution B
It is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.It treats ice melting, you can obtain
Obtain the Ru of atom level dispersion.
Embodiment 16
The preparation of the Rh materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses C6H9O6Rh and deionized water are made into the C of 3mg/ml6H9O6Rh is molten
Liquid.Reactant solution A is rapidly frozen into ice cube with liquid nitrogen.Then, the reactant solution B of needs is configured, uses NaBH4With go from
Sub- water is made into the NaBH of 3mg/ml4Solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat ice cube
Melt, you can obtain the Rh of atom level dispersion.
Embodiment 17
The preparation of the Rh materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses RhCl3The RhCl of 0.5mg/ml is made into ethyl alcohol3Solution.Use liquid nitrogen
Reactant solution A is rapidly frozen into ice cube.Then, the reactant solution B of needs is configured, uses N2H5OH and ethyl alcohol are made into
The N of 0.5mg/ml2H5OH solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in -10 DEG C.Treat it is ice melting,
The Rh of atom level dispersion can be obtained.
Embodiment 18
The preparation of the Rh materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses RhCl3The RhCl of 20mg/ml is made into ethylene glycol3Solution.Then,
The reactant solution B needed is configured, uses KBH4The KBH4 solution of 40mg/ml is made into ultra-pure water.With liquid nitrogen by reactant solution B
It is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.It treats ice melting, you can obtain
Obtain the Rh of atom level dispersion.
Embodiment 19
The preparation of the Pd materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses H2PdCl4The H of 3mg/ml is made into deionized water2PdCl4Solution.
Reactant solution A is rapidly frozen into ice cube with liquid nitrogen.Then, the reactant solution B of needs is configured, with NaBH4 and deionization
Water is made into the NaBH4 solution of 3mg/ml.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat that ice cube melts
Change, you can obtain the Pd of atom level dispersion.
Embodiment 20
The preparation of the Pd materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses K2PdCl4The K of 0.5mg/ml is made into ethyl alcohol2PdCl4Solution.With
Reactant solution A is rapidly frozen into ice cube by liquid nitrogen.Then, the reactant solution B of needs is configured, uses N2H5OH and ethyl alcohol are made into
The N of 0.5mg/ml2H5OH solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in -10 DEG C.Treat it is ice melting,
The Pd of atom level dispersion can be obtained.
Embodiment 21
The preparation of the Pd materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses Na2PdCl4The Na of 20mg/ml is made into ethylene glycol2PdCl4It is molten
Liquid.Then, the reactant solution B of needs is configured, uses KBH4The KBH of 40mg/ml is made into ultra-pure water4Solution.It will be reacted with liquid nitrogen
Object solution B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.Treat it is ice melting,
The Pd of atom level dispersion can be obtained.
Embodiment 22
The preparation of the Ag materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses AgNO3The AgNO of 3mg/ml is made into deionized water3Solution.Use liquid
Reactant solution A is rapidly frozen into ice cube by nitrogen.Then, the reactant solution B of needs is configured, is matched with NaBH4 and deionized water
Into the NaBH4 solution of 3mg/ml.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting, i.e.,
The Ag of atom level dispersion can be obtained.
Embodiment 23
The preparation of the Ag materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses AgNO3The AgNO of 0.5mg/ml is made into ethyl alcohol3Solution.Use liquid nitrogen
Reactant solution A is rapidly frozen into ice cube.Then, the reactant solution B of needs is configured, 0.5mg/ml is made into formaldehyde and water
Formalin.Ice cube is placed into reactant solution B, it is allowed slowly to melt in -10 DEG C.It treats ice melting, you can obtain
The Ag of atom level dispersion.
Embodiment 24
The preparation of the Ag materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses AgNO3The AgNO of 20mg/ml is made into ethylene glycol3Solution.Then,
The reactant solution B needed is configured, uses KBH4The KBH of 40mg/ml is made into ultra-pure water4Solution.With liquid nitrogen by reactant solution B
It is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.It treats ice melting, you can obtain
Obtain the Ag of atom level dispersion.
Embodiment 25
The preparation of the Os materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses OsCl3The OsCl of 3mg/ml is made into deionized water3Solution.Use liquid
Reactant solution A is rapidly frozen into ice cube by nitrogen.Then, the reactant solution B of needs is configured, is matched with NaBH4 and deionized water
Into the NaBH4 solution of 3mg/ml.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting, i.e.,
The Os of atom level dispersion can be obtained.
Embodiment 26
The preparation of the Os materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses OsCl3The OsCl of 0.5mg/ml is made into ethyl alcohol3Solution.Use liquid nitrogen
Reactant solution A is rapidly frozen into ice cube.Then, the reactant solution B of needs is configured, uses N2H5OH and ethyl alcohol are made into
The N of 0.5mg/ml2H5OH solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in -10 DEG C.Treat it is ice melting,
The Os of atom level dispersion can be obtained.
Embodiment 27
The preparation of the Os materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses OsCl3The OsCl of 20mg/ml is made into ethylene glycol3Solution.Then,
The reactant solution B needed is configured, uses KBH4The KBH of 40mg/ml is made into ultra-pure water4Solution.With liquid nitrogen by reactant solution B
It is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.It treats ice melting, you can obtain
Obtain the Os of atom level dispersion.
Embodiment 28
The preparation of the Ir materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses HIrCl6The HIrCl of 3mg/ml is made into deionized water6Solution.With
Reactant solution A is rapidly frozen into ice cube by liquid nitrogen.Then, the reactant solution B of needs is configured, with NaBH4 and deionized water
It is made into the NaBH4 solution of 3mg/ml.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting,
The Ir of atom level dispersion can be obtained.
Embodiment 29
The preparation of the Ir materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses KIrCl6The KIrCl of 0.5mg/ml is made into ethyl alcohol6Solution.Use liquid
Reactant solution A is rapidly frozen into ice cube by nitrogen.Then, the reactant solution B of needs is configured, uses N2H5OH and ethyl alcohol are made into
The N of 0.5mg/ml2H5OH solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in -10 DEG C.Treat it is ice melting,
The Ir of atom level dispersion can be obtained.
Embodiment 30
The preparation of the Ir materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses NaIrCl6The NaIrCl of 20mg/ml is made into ethylene glycol6Solution.
Then, the reactant solution B of needs is configured, uses KBH4The KBH of 40mg/ml is made into ultra-pure water4Solution.With liquid nitrogen by reactant
Solution B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.Treat it is ice melting, i.e.,
The Ir of atom level dispersion can be obtained.
Embodiment 31
The preparation of the Pt materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses H2PtCl6The H of 3mg/ml is made into deionized water2PtCl6Solution.
Reactant solution A is rapidly frozen into ice cube with liquid nitrogen.Then, the reactant solution B of needs is configured, with NaBH4 and deionization
Water is made into the NaBH4 solution of 3mg/ml.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat that ice cube melts
Change, you can obtain the Pt of atom level dispersion.
Embodiment 32
The preparation of the Pt materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses Na2PtCl6The Na of 20mg/ml is made into ethyl alcohol2PtCl6Solution.
Reactant solution A is rapidly frozen into ice cube with liquid nitrogen.Then, the reactant solution B of needs is configured, uses N2H5OH and ethyl alcohol are matched
Into the N of 20mg/ml2H5OH solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in -10 DEG C.Treat that ice cube melts
Change, you can obtain the Pt of atom level dispersion.
Embodiment 33
The preparation of the Pt materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses K2PtCl6The K of 0.5mg/ml is made into ethylene glycol2PtCl6Solution.
Then, the reactant solution B of needs is configured, uses KBH4The KBH of 0.5mg/ml is made into ultra-pure water4Solution.With liquid nitrogen by reactant
Solution B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.Treat it is ice melting, i.e.,
The Pt of atom level dispersion can be obtained.
Embodiment 34
The preparation of the Au materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses HAuCl4The HAuCl of 3mg/ml is made into deionized water4Solution.With
Reactant solution A is rapidly frozen into ice cube by liquid nitrogen.Then, the reactant solution B of needs is configured, with NaBH4 and deionized water
It is made into the NaBH4 solution of 3mg/ml.Ice cube is placed into reactant solution B, it is allowed slowly to melt in 0 DEG C.Treat it is ice melting,
The Au of atom level dispersion can be obtained.
Embodiment 35
The preparation of the Au materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses NaAuCl4The NaAuCl of 20mg/ml is made into ethyl alcohol4Solution.With
Reactant solution A is rapidly frozen into ice cube by liquid nitrogen.Then, the reactant solution B of needs is configured, uses N2H5OH and ethyl alcohol are made into
The N of 20mg/ml2H5OH solution.Ice cube is placed into reactant solution B, it is allowed slowly to melt in -10 DEG C.Treat it is ice melting,
The Au of atom level dispersion can be obtained.
Embodiment 36
The preparation of the Au materials of atom level dispersion.
First, the reactant solution A of needs is configured, uses KAuCl4The KAuCl of 0.5mg/ml is made into ethylene glycol4Solution.It connects
It, the reactant solution B of needs is configured, uses KBH4The KBH of 0.5mg/ml is made into ultra-pure water4Solution.It is with liquid nitrogen that reactant is molten
Liquid B is rapidly frozen into ice cube.Ice cube is placed into reactant solution A, it is allowed slowly to melt in 1 DEG C.It treats ice melting, you can
Obtain the Au of atom level dispersion.
As shown in Figure 1, Ag nano particles are prepared different from conventional solution method in the present invention, simply can easily prepare
The Ag materials of the atom level dispersion of high quality.
By above-described embodiment result it is found that can efficiently prepare diversified atom fraction rapidly using the method for the present invention
Scattered solution and the material of atom level dispersion.The quality of materials of atom level dispersion prepared according to the methods of the invention is high, uniformity
Good, the material of preparation has extensive and excellent application in fields such as catalysis.
Technical scheme of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited it is retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of ice is mutually sustained the method for preparing atom level dispersion, which is characterized in that this method includes the following steps：
(1) reactant solution A is made into presoma and solvent, the presoma is the monoatomic compound of metal；
(2) it is made into reactant solution B with reducing agent and solvent；
(3) reactant solution A prepared by above-mentioned steps (1) is frozen into ice cube, then the ice cube is placed into reactant solution B
In or by above-mentioned steps (2) prepare reactant solution B be frozen into ice cube, then the ice cube is placed into reactant solution A；
The ice cube is allowed slowly to melt and react to each other, obtains atom level dispersed metal material.
2. according to the method described in claim 1, it is characterized in that, quality-volume of reactant solution A described in step (1)
A concentration of 0.01-60mg/ml.
3. according to the method described in claim 1, it is characterized in that, metal described in step (1) it is monatomic for Fe, Co, Ni,
Any one of Cu, Ru, Rh, Pd, Ag, Os, Ir, Pt and Au.
4. according to the method described in claim 1, it is characterized in that, solvent described in step (1) be water, ethylene glycol, ethyl alcohol,
Any one of tetraethylene-glycol, dimethylformamide or formaldehyde.
5. according to the method described in claim 1, it is characterized in that, quality-volume of reactant solution B described in step (2)
A concentration of 0.01-100mg/ml.
6. according to the method described in claim 1, it is characterized in that, the reducing agent described in step (2) is NaBH4,KBH4,
N2H4,N2H5OH, formaldehyde, formic acid, ascorbic acid, Na2SO3,K2SO3,H2C2O4Any one of.
7. according to the method described in claim 1, it is characterized in that, solvent described in step (2) be water, ethylene glycol, ethyl alcohol,
Any one of tetraethylene-glycol, dimethylformamide or formaldehyde.
8. according to the method described in claim 1, it is characterized in that, melt temperature and reaction temperature described in step (3) are one
It causes, ranging from -30-10 DEG C.
9. according to the method described in claim 1, it is characterized in that, compound described in step (1) is inorganic salts.
10. according to the method described in claim 1, it is characterized in that, compound described in step (1) is chloride, sulfate
Or nitrate.
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