CN109877342A - A kind of amorphous noble metal nano-plate and preparation method thereof - Google Patents
A kind of amorphous noble metal nano-plate and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of amorphous noble metal nano-plate, comprising the following steps: is uniformly mixed the solid powder of inorganic salts and noble metal organic salt, high-temperature calcination, after removing inorganic salts, obtains the amorphous noble metal nano-plate of carbon doping.The present invention is using inorganic salts as template, using noble metal organic salt as presoma, a large amount of amorphous noble metal nano-plate can be made by the method for high temperature pyrolysis, precious metal atom exists in mixed and disorderly unordered form, and is homogeneously dispersed on carbon nanosheet.Preparation method is simple for this, and repetitive rate and yield are higher, has versatility, is also used to prepare other amorphous metal materials, is expected to become one of the effective ways for preparing amorphous noble metal nanometer material.The preparation method of above-mentioned amorphous noble metal nano-plate proposed by the present invention is to be put forward for the first time, and this method provides a kind of completely new strategy to prepare amorphous noble metal nano-plate.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of amorphous noble metal nano-plate and preparation method thereof.
Background technique
Due to the unique physicochemical properties of noble metal, noble metal nanometer material is in necks such as catalysis, energy energy storage and conversions
Domain has a wide range of applications.But due to the Costco Wholesale and scarcity of noble metal valuableness, seriously constrain precious metal catalyst
The large-scale practical application of agent.In order to improve the atom utilization and effective active of noble metal, the crystalline substance of noble metal nanometer material
One of the effective way for such issues that mutually regulation and optimization are solutions, especially amorphous noble metal nanometer material are constructed certain
The catalytic performance of catalyst is greatly improved in degree.
Relative to crystalline material, non-crystalline material has unique atomic arrangement mode, has shortrange order and long-term unordered
Atomic arrangement feature.To which, non-crystalline material shows different from crystalline material and unique chemistry and structural property, as it is each to
The same sex, high concentration unsaturated coordination activity site, can regulate and control extensively constituent the features such as.Because of its unique chemistry and knot
Structure feature, non-crystalline material show to be much better than urging for corresponding crystalline material in fields such as Chemical Manufacture, energy conversion, environmental renovations
Change performance, to receive significant attention.
The synthesis of non-crystalline material at present mainly has the methods of rapid freezing method, electro-deposition method and light degradation synthesis.But
These synthetic methods are cumbersome, without versatility and are difficult to accurately control the pattern and size of amorphous nano material.So tool
The synthesis of the amorphous noble metal nanometer material of standby accurate dimension and Morphological control is still a huge challenge.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of amorphous noble metal nano-plate and its preparation side
Method, simple and easy, repetitive rate and yield are higher, and have versatility.
The present invention provides a kind of preparation methods of amorphous noble metal nano-plate, comprising the following steps:
The solid powder of inorganic salts and noble metal organic salt is uniformly mixed, high-temperature calcination, after removing inorganic salts, obtains carbon
The amorphous noble metal nano-plate of doping.
The present invention is using inorganic salts as template, and using noble metal organic salt as presoma, the method for high temperature pyrolysis, your gold passed through
Belong to atom and non-metal carbon atomic interaction, forms carbon and adulterate amorphous noble metal nano-plate.Precious metal atom is with mixed and disorderly unordered
Form exist, and be homogeneously dispersed on carbon nanosheet.Preparation method is simple for this, has versatility, is also used to make
Other standby amorphous metal materials.
Wherein, the inorganic salts are preferably one of nitrate and haloid or a variety of.
Wherein, the nitrate is preferably NaNO3；The haloid is preferably KBr.
The noble metal organic salt is preferably the acetylacetonate of precious metal atom.The precious metal atom be preferably Rh,
One of Ru and Ir or a variety of.
The i.e. described noble metal organic salt is preferably acetylacetone,2,4-pentanedione rhodium, one of acetylacetone,2,4-pentanedione ruthenium and acetylacetone,2,4-pentanedione iridium or more
Kind.
The mass ratio of the inorganic salts and noble metal organic salt is preferably (1~2): 1.
Preferably, the preparation method specifically includes the following steps:
A) ethanol solution of inorganic salt solution and noble metal organic salt is mixed, obtains mixed solution；
B) the mixed solution drying for obtaining step A) is handled, and obtains the hybrid solid of inorganic salts and noble metal organic salt
Powder；
C the hybrid solid powder metallurgy for) obtaining step B) is calcined, using second alcohol and water mixed solution or water into
Row washing, removes inorganic salts, obtains the amorphous noble metal nano-plate of carbon doping.
The ethanol solution of inorganic salt solution and noble metal organic salt is mixed first, obtains mixed solution.
It is currently preferred, inorganic salt solution is added dropwise in the ethanol solution of noble metal organic salt, is stirred.
The present invention is to time of the stirring and is not particularly limited, preferably 3~5h.
Then by the processing of obtained mixed solution drying, the hybrid solid powder of inorganic salts and noble metal organic salt is obtained
End.
The temperature of the drying is preferably 60~90 DEG C.
Then high-temperature calcination is carried out to obtained hybrid solid powder.
The present invention is to the method for the calcining and is not particularly limited, and can be calcining side well known to those skilled in the art
Method.
In some embodiments of the invention, solid powder is placed in porcelain boat, porcelain boat is put into tube furnace, carried out
High-temperature calcination.
The temperature of the high-temperature calcination is preferably 260~300 DEG C；Time is preferably 90~120min.
In the present invention, the high-temperature calcination preferably carries out in air atmosphere.
The heating rate of the high-temperature calcination is preferably 3~8 DEG C/min.Further preferably 5 DEG C/min.
High-temperature calcination and after material natural cooling is cooled to room temperature, is washed using the mixed solution of second alcohol and water,
Or adopt and be washed with deionized, inorganic salts are removed, the amorphous noble metal nano-plate of carbon doping is obtained.
The present invention is to the number of washing and is not particularly limited, preferably 3~4 times.
The present invention also provides a kind of amorphous noble metal nano-plates of carbon doping, are prepared according to method made above.
Preferably, the amorphous noble metal nano-plate of carbon doping with a thickness of 4~10nm, width is 1~2 μm.
The present invention also provides a kind of preparation methods of amorphous precious metal alloys nanometer sheet, comprising the following steps:
The solid powder of inorganic salts, noble metal organic salt and base metal organic salt is uniformly mixed, high-temperature calcination, is removed
After inorganic salts, the amorphous precious metal alloys nanometer sheet of carbon doping is obtained.
Wherein, the inorganic salts, noble metal organic salt are same as above, and details are not described herein.
The base metal organic salt is preferably the acetylacetonate of base metal atom；The base metal atom is preferred
For 3d transition metal, in some embodiments of the invention, the base metal atom is selected from Ni, Fe, one of Co
Or it is a variety of.
The mass ratio of the inorganic salts, noble metal organic salt and base metal organic salt is preferably (1-2): 1:(0.01-
0.1)。
Preferably, the preparation method specifically includes the following steps:
A) by the ethanol solution of the ethanol solution and base metal organic salt of inorganic salt solution and noble metal organic salt
Mixing, obtains mixed solution；
B) the mixed solution drying for obtaining step A) is handled, and obtains inorganic salts, noble metal organic salt and base metal
The hybrid solid powder of organic salt；
C the hybrid solid powder metallurgy for) obtaining step B) is calcined, using second alcohol and water mixed solution or water into
Row washing, removes inorganic salts, obtains the amorphous precious metal alloys nanometer sheet of carbon doping.
It is first that the ethyl alcohol of the ethanol solution and base metal organic salt of inorganic salt solution and noble metal organic salt is molten
Liquid mixing, obtains mixed solution.
It is currently preferred, it is organic that the ethanol solution of inorganic salt solution and base metal organic salt is added dropwise to noble metal
In the ethanol solution of salt, it is stirred.
The present invention is to time of the stirring and is not particularly limited, preferably 3~5h.
Then by the processing of obtained mixed solution drying, it is organic that inorganic salts, noble metal organic salt and base metal are obtained
The hybrid solid powder of salt.
The temperature of the drying is preferably 60~90 DEG C.
Then high-temperature calcination is carried out to obtained hybrid solid powder.
The concrete operations of the high-temperature calcination and condition are same as above, and details are not described herein.
High-temperature calcination and after material natural cooling is cooled to room temperature, is washed using the mixed solution of second alcohol and water,
Or adopt and be washed with deionized, inorganic salts are removed, the amorphous precious metal alloys nanometer sheet of carbon doping is obtained.
The present invention is to the number of washing and is not particularly limited, preferably 3~4 times.
The present invention also provides a kind of amorphous precious metal alloys nanometer sheets of carbon doping, are prepared into according to above-mentioned preparation method
It arrives.
Preferably, the amorphous precious metal alloys nanometer sheet of carbon doping with a thickness of 4~10nm, width is 1~2 μm.
The present invention provides a kind of preparation methods of amorphous noble metal nano-plate, comprising the following steps: by inorganic salts and expensive
The solid powder of metal organic salt is uniformly mixed, high-temperature calcination, after removing inorganic salts, obtains the amorphous noble metal nano of carbon doping
Piece.The present invention is using inorganic salts as template, using noble metal organic salt as presoma, can be made big by the method for high temperature pyrolysis
The amorphous noble metal nano-plate of amount, precious metal atom exists in mixed and disorderly unordered form, and is homogeneously dispersed on carbon nanosheet.
Preparation method is simple for this, and repetitive rate and yield are higher, has versatility, is also used to prepare other amorphous metal materials,
It is expected to become one of the effective ways for preparing amorphous noble metal nanometer material.
The preparation method of above-mentioned amorphous noble metal nano-plate proposed by the present invention is to be put forward for the first time, and belongs to amorphous noble metal and receives
The universal synthesis method of rice piece, the amorphous noble metal nano-plate of preparation includes the single metal nano plate of amorphous noble metal and amorphous
Precious metal alloys nanometer sheet.
When the noble metal organic salt of addition is a kind of, the single metal nano plate of amorphous noble metal, such as amorphous is prepared
Iridium nanometer sheet, amorphous rhodium nanometer sheet, amorphous ruthenium nanometer sheet.
When the noble metal organic salt of addition is a variety of, amorphous precious metal alloys nanometer sheet, including noble metal-is prepared
Noble metal bimetallic/tri- metal alloy nanometer sheets, such as amorphous iridium ruthenium nanometer sheet, amorphous iridium rhodium nanometer sheet, amorphous rhodium ruthenium nanometer sheet,
Amorphous iridium rhodium ruthenium nanometer sheet etc..
When the raw material of addition includes noble metal organic salt and base metal organic salt, amorphous precious metal alloys are prepared
Nanometer sheet, including noble metal-base metal bimetallic/tri- metal alloy nanometer sheets, such as amorphous rhodium iron nanometer sheet, amorphous rhodium cobalt is received
Rice piece, amorphous rhodium nickel nano film, amorphous ruthenium iron nanometer sheet, amorphous ruthenium nickel nano film, amorphous ruthenium cobalt nanometer sheet, amorphous iridium iron nanometer
Piece, amorphous iridium nickel nano film, amorphous iridium cobalt nanometer sheet etc..
This method provides a kind of completely new strategy to prepare amorphous noble metal nano-plate.
Detailed description of the invention
Fig. 1 is dark for transmission electron microscope image, the high angle annular of amorphous iridium nanometer sheet catalyst prepared by the present invention
Field scan transmission electron microscope image and X ray diffracting spectrum；
Fig. 2 is dark for transmission electron microscope image, the high angle annular of amorphous rhodium nanometer sheet catalyst prepared by the present invention
Field scan transmission electron microscope image and X ray diffracting spectrum；
Fig. 3 is the transmission electron microscope image of amorphous rhodium iron nanometer sheet catalyst prepared by the present invention, high angle annular
Dark field scanning transmission electron microscope image and X ray diffracting spectrum；
Fig. 4 is the transmission electron microscope image of amorphous iridium ruthenium nanometer sheet catalyst prepared by the present invention, high angle annular
Dark field scanning transmission electron microscope image and X ray diffracting spectrum.
Specific embodiment
In order to further illustrate the present invention, ultra-thin two-dimension amorphous noble metal provided by the invention is received below with reference to embodiment
Rice sheet material and its preparation method and application is described in detail.
Embodiment 1
The preparation of amorphous iridium nanometer sheet:
(1) 10mg acetylacetone,2,4-pentanedione iridium is dissolved in ethanol solution, it is mixed that 1mL sodium nitrate aqueous solution (16mg/mL) is added dropwise
It closes solution to stir 4 hours, obtains uniform solution；
(2) obtained mixed solution is placed in 65 DEG C of baking oven, dry out solvent, obtain metal iridium acetylacetonate and
The hybrid solid powder of sodium nitrate；
(3) solid powder obtained above is placed in porcelain boat, then porcelain boat is put into tube furnace.In air atmosphere with 5
DEG C/min is warming up to 300 DEG C, 90min is calcined, then natural cooling cools to room temperature.3- is washed with the mixed solution of second alcohol and water
4 times to get arrive amorphous iridium nanometer sheet.
The pattern of the amorphous iridium nanometer sheet of preparation is characterized, as a result as shown in Figure 1, Fig. 1 is prepared by the present invention non-
The transmission electron microscope image (a) of brilliant iridium nanometer sheet catalyst, high angle annular dark field scanning transmission electron microscope image
(b) and X ray diffracting spectrum (c).
As seen from Figure 1: obtained nanometer sheet be size be 1.0 μm or so and atomic disorder disordered arrangements
Amorphous iridium nanometer sheet.
Embodiment 2
The preparation of amorphous rhodium nanometer sheet:
Difference from Example 1 are as follows: 8mg acetylacetone,2,4-pentanedione rhodium is dissolved in ethanol solution, 1mL potassium bromide water is added dropwise
Solution (16mg/mL).Mixed solution is dried after stirring 4 hours, and then obtained sample is put into tube furnace in air atmosphere
Lower 280 DEG C of calcinings 90min, obtains amorphous rhodium nanometer sheet.
The pattern of the amorphous rhodium nanometer sheet of preparation is characterized, as a result as shown in Fig. 2, Fig. 2 is prepared by the present invention non-
The transmission electron microscope image (a) of brilliant rhodium nanometer sheet catalyst, high angle annular dark field scanning transmission electron microscope image
(b) and X ray diffracting spectrum (c).
As seen from Figure 2: obtained nanometer sheet be size be 1.0 μm or so and atomic disorder disordered arrangements
Amorphous rhodium nanometer sheet.
Embodiment 3
Difference from Example 1 are as follows: 8mg acetylacetone,2,4-pentanedione ruthenium is dissolved in ethanol solution, 1mL potassium bromide water is added dropwise
Solution (16mg/mL).Mixed solution is dried after stirring 4 hours, and then obtained sample is put into tube furnace in air atmosphere
Lower 280 DEG C of calcinings 90min, obtains amorphous ruthenium nanometer sheet.
Embodiment 4
Amorphous noble metal-base metal bimetallic/tri-metal nano piece preparation:
By taking amorphous rhodium iron nanometer sheet as an example:
Difference from Example 1 are as follows: 8mg acetylacetone,2,4-pentanedione rhodium is dissolved in ethanol solution, 0.25mL acetyl is added dropwise
Acetone iron ethanol solution (1.4mg/mL) and 1mL kbr aqueous solution (16mg/mL).Mixed solution is dried after stirring 4 hours, so
Obtained sample is put into tube furnace 270 DEG C of calcining 90min in air atmosphere afterwards, obtains amorphous rhodium iron nanometer sheet.
The pattern of the amorphous rhodium iron nanometer sheet of preparation is characterized, as a result as shown in figure 3, Fig. 3 is prepared by the present invention
Transmission electron microscope image (a), the high angle annular dark field scanning transmission electron microscope of amorphous rhodium iron nanometer sheet catalyst
Image (b) and X ray diffracting spectrum (c).
As seen from Figure 3: obtained nanometer sheet be size be 1.0 μm or so and atomic disorder disordered arrangements
Amorphous rhodium iron nanometer sheet.
By changing the type of corresponding salt, other kinds of noble metal-base metal bimetallic/tri- metals are prepared and receive
Rice piece, such as amorphous rhodium cobalt nanometer sheet, amorphous rhodium nickel nano film, amorphous ruthenium iron nanometer sheet, amorphous ruthenium nickel nano film, amorphous ruthenium cobalt received
Rice piece, amorphous iridium iron nanometer sheet, amorphous iridium nickel nano film, amorphous iridium cobalt nanometer sheet etc..
Embodiment 5
The preparation of amorphous noble metal bimetallic/tri-metal nano piece:
By taking amorphous iridium ruthenium nanometer sheet as an example:
Difference from Example 1 are as follows: 10mg acetylacetone,2,4-pentanedione iridium is dissolved in ethanol solution, 0.25mL acetyl is added dropwise
Acetone ruthenium ethanol solution (0.8mg/mL) and 1mL sodium nitrate aqueous solution (16mg/mL).Mixed solution is dried after stirring 4 hours, so
Obtained sample is put into tube furnace 280 DEG C of calcining 90min in air atmosphere afterwards, obtains amorphous iridium ruthenium nanometer sheet.
The pattern of the amorphous iridium ruthenium nanometer sheet of preparation is characterized, as a result as shown in figure 4, Fig. 4 is prepared by the present invention
Transmission electron microscope image (a), the high angle annular dark field scanning transmission electron microscope of amorphous iridium ruthenium nanometer sheet catalyst
Image (b) and X ray diffracting spectrum (c).
As seen from Figure 4: obtained nanometer sheet be size be 1.0 μm or so and atomic disorder disordered arrangements
Amorphous iridium ruthenium nanometer sheet.
By the type of the corresponding salt of change, other kinds of noble metal bimetallic/tri- metal alloy nanometer sheets are prepared,
Such as amorphous iridium rhodium nanometer sheet, amorphous rhodium ruthenium nanometer sheet and amorphous iridium rhodium ruthenium nanometer sheet etc..
As can be seen from the above embodiments, the present invention uses simple method, and amorphous noble metal nano-plate has been prepared.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
Claims (10)
1. a kind of preparation method of amorphous noble metal nano-plate, which comprises the following steps:
The solid powder of inorganic salts and noble metal organic salt is uniformly mixed, high-temperature calcination, after removing inorganic salts, obtains carbon doping
Amorphous noble metal nano-plate.
2. preparation method according to claim 1, which is characterized in that specifically:
A) ethanol solution of inorganic salt solution and noble metal organic salt is mixed, obtains mixed solution；
B) the mixed solution drying for obtaining step A) is handled, and obtains the hybrid solid powder of inorganic salts and noble metal organic salt
End；
C) the hybrid solid powder metallurgy for obtaining step B) is calcined, and is washed using the mixed solution or water of second alcohol and water
It washs, removes inorganic salts, obtain the amorphous noble metal nano-plate of carbon doping.
3. preparation method according to claim 1, which is characterized in that the mass ratio of the inorganic salts and noble metal organic salt
For (1~2): 1.
4. a kind of preparation method of amorphous precious metal alloys nanometer sheet, which comprises the following steps:
The solid powder of inorganic salts, noble metal organic salt and base metal organic salt is uniformly mixed, high-temperature calcination, is removed inorganic
After salt, the amorphous precious metal alloys nanometer sheet of carbon doping is obtained.
5. the preparation method according to claim 4, which is characterized in that the base metal organic salt is base metal atom
Acetylacetonate；The base metal atom is one of 3d transition metal or a variety of；One in preferably Ni, Fe, Co
Kind is a variety of.
6. preparation method according to claim 1 or 4, which is characterized in that the inorganic salts are in nitrate and haloid
It is one or more；The noble metal organic salt is the acetylacetonate of precious metal atom；The precious metal atom be Rh, Ru and
One of Ir or a variety of；
The temperature of the high-temperature calcination is 260~300 DEG C；Time is 90~120min.
7. preparation method according to claim 6, which is characterized in that the nitrate is sodium nitrate；The haloid is
Potassium bromide.
8. a kind of amorphous noble metal nano-plate of carbon doping, which is characterized in that according to described in claims 1 to 3,6~7 any one
Preparation method be prepared.
9. the amorphous noble metal nano-plate of carbon doping according to claim 8, which is characterized in that wide with a thickness of 4~10nm
Degree is 1~2 μm.
10. a kind of amorphous precious metal alloys nanometer sheet of carbon doping, which is characterized in that according to described in any one of claim 4~7
Preparation method be prepared.
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