CN105234427A - Platinum alloy nano core-shell cube and preparation method thereof - Google Patents
Platinum alloy nano core-shell cube and preparation method thereof Download PDFInfo
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- CN105234427A CN105234427A CN201510741980.5A CN201510741980A CN105234427A CN 105234427 A CN105234427 A CN 105234427A CN 201510741980 A CN201510741980 A CN 201510741980A CN 105234427 A CN105234427 A CN 105234427A
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Abstract
The invention provides a platinum alloy nano core-shell cube and a preparation method thereof. The preparation method comprises the following steps: 1) under the protection of an inert gas, adding platinum acetylacetone, an acetylacetone metallic compound, alkylamine and an alkyl acid in a reaction vessel simultaneously to be homogenized to obtain a uniformly mixed first mixed solution; 2) quickly transferring the first mixed solution obtained in the step 1) to a high-temperature oil bath, preserving heat for a preset time, then introducing a reducing gas for reaction to obtain a black suspension; and 3) sequentially conducting organic solvent cleaning, magnetic separation and vacuum drying on the obtained black suspension to obtain the platinum alloy nano core-shell cube. The platinum alloy nano core-shell cube is good in dispersity, controllable in components and easy to collect and is magnetic; and in the preparation method, a one-pot oleylamine system is adopted and the used reagents are nontoxic, and the preparation method is simple, and is easy to operate.
Description
Technical field
The invention belongs to the preparing technical field of nano material, be specifically related to platinum alloy nano core-shell cube and preparation method thereof.
Background technology
Noble metal nanometer material, particularly platinum based nano-material, because the physicochemical properties of its uniqueness all have wide practical use in a lot of fields such as catalysis.But the reserves of noble metal are rare and expensive, people transfer to sight in their service efficiency of raising, such as the noble metals such as platinum are combined with base metal and are prepared into bimetal nano catalyst, not only significantly decrease noble metal dosage, and utilize the electro transfer effect between bimetallic to produce cooperative effect.
Along with deepening continuously of nanotechnology research, it is found that and two or more nanostructureds are combined, will excellent physics and chemistry character be embodied.Wherein most typically surely belong to nanometer nuclear shell nano-structure.Interacted shell material after the ordered fabrication of core surface by chemical bond or other, not only the several functions of core and shell can be combined, synergy can also be produced on interface.Therefore, nanometer nuclear shell nano-structure has more abundant and excellent performance than the nano particle of single component, has important application prospect in fields such as medical science, biology, catalysis.
For the nano particle of platinum cobalt binary system, reported that major part is the uniform alloying pellet of component, comprised cube, octahedra, the patterns such as dendritic particle, about the preparation of platinum cobalt nucleocapsid cubic type bimetal nano particles, there is no report both at home and abroad in the past.
Summary of the invention
The object of the invention is to overcome defect of the prior art, a kind of platinum alloy nano core-shell cube and preparation method thereof is provided.The cubical core of platinum alloy nano core-shell is made up of flower-shaped platinum alloy particle, and shell is made up of cobalt, nickel or iron simple substance, good dispersion, and composition is controlled, is magnetic, and is easy to collect; Present invention also offers the cubical preparation method of a kind of platinum alloy nano core-shell, adopt one kettle way oleyl amine system, by regulating and controlling the ratio of metal precursor and reaction time and temperature, obtain the platinum alloy nano core-shell cube that component is different, agents useful for same is nontoxic, and method is simple, is easy to operation.
To achieve these goals and other related objectives, the invention provides a kind of platinum alloy nano core-shell cube, described platinum alloy comprises metal platinum and the second metal, described platinum alloy nano core-shell cube comprises kernel and is coated on the shell of described kernel periphery, described kernel is flower-shaped platinum alloy particle kernel, and described shell is the second metal simple-substance shell.
As the cubical a kind of preferred version of platinum alloy nano core-shell of the present invention, described second metal is cobalt, and described flower-shaped platinum alloy particle kernel is the flower-shaped alloy particle kernel of platinum cobalt, and described shell is cobalt simple substance shell.
As the cubical a kind of preferred version of platinum alloy nano core-shell of the present invention, described second metal is nickel, and described flower-shaped platinum alloy particle kernel is the flower-shaped alloy particle kernel of platinum nickel, and described shell is nickel simple substance shell.
As the cubical a kind of preferred version of platinum alloy nano core-shell of the present invention, described second metal is iron, and described flower-shaped platinum alloy particle kernel is platinum ornamental work of iron shape alloy particle kernel, and described shell is iron simple substance shell.
As the cubical a kind of preferred version of platinum alloy nano core-shell of the present invention, described platinum alloy nano core-shell is cubical is of a size of 20nm ~ 40nm; The thickness of described shell is 2nm ~ 5nm.
The present invention also provides a kind of platinum alloy nano core-shell cubical preparation method, and the described cubical preparation method of platinum alloy nano core-shell comprises the steps:
1) under the protection of inert gas, acetylacetone,2,4-pentanedione platinum, acetylacetone metallic compound, alkylamine and alkyl acid are added in reaction vessel simultaneously and carries out Homogenization Treatments, obtain the first mixed solution mixed;
2) by step 1) described first mixed liquor that obtains transfers to rapidly in high temperature oil bath, and after the insulation scheduled time, pass into reducing gas and react, obtain black suspension;
3) by step 2) the described black suspension that obtains carries out organic solvent cleaning, Magneto separate and vacuum drying successively, namely obtains platinum alloy nano core-shell cube.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 1) in, described acetylacetone metallic compound is acetylacetone cobalt, nickel acetylacetonate or ferric acetyl acetonade.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 1) in, the temperature of Homogenization Treatments is 100 DEG C ~ 150 DEG C, and the time of Homogenization Treatments is 5min ~ 30min.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 1) in, described alkylamine is one or more in oleyl amine, lauryl amine, cetylamine etc.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 1) in, described alkyl acid is one or more in oleic acid, stearic acid, laurate.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 1) in, the mol ratio of described acetylacetone,2,4-pentanedione platinum and described acetylacetone metallic compound is 1:4 ~ 1:2.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 2) in, the temperature of described high temperature oil bath is 220 DEG C ~ 235 DEG C, and the described scheduled time is 2min ~ 8min.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 2) in, described reducing gas is carbon monoxide, and the flow velocity of described reducing gas is 100mL/min ~ 300mL/min.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 2) in, described in pass into the time that reducing gas carries out reacting be 20min ~ 1h.
As a kind of preferred version of the cubical preparation method of platinum alloy nano core-shell of the present invention, described step 3) in, described organic solvent is one or more in ethanol, chloroform, n-hexane, acetone etc.
Platinum alloy nano core-shell cube of the present invention and preparation method thereof has following beneficial effect: the cubical core of platinum alloy nano core-shell is made up of flower-shaped platinum alloy particle, shell is made up of cobalt, nickel or iron simple substance, good dispersion, and composition is controlled, be magnetic, be easy to collect; Present invention also offers the cubical preparation method of a kind of platinum alloy nano core-shell, adopt one kettle way oleyl amine system, by regulating and controlling the ratio of metal precursor and reaction time and temperature, obtain the platinum alloy nano core-shell cube that component is different, agents useful for same is nontoxic, and method is simple, is easy to operation.
Accompanying drawing explanation
Fig. 1 is shown as the TEM figure of the platinum cobalt nano core-shell cube particle of preparation in the embodiment of the present invention 1.
The high-resolution TEM that Fig. 2 is shown as the platinum cobalt nano core-shell cube particle of preparation in the embodiment of the present invention 1 schemes.
Detailed description of the invention
After now specific embodiments of the invention being described in.Following embodiment only in order to illustrate of the present invention, and does not do any restriction to scope of the present invention, and any person skilled in the art person can realize modifications and variations easily and include within the present invention and claims scope.
Embodiment 1
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.
Accompanying drawing 1 is the TEM figure of the platinum cobalt nano core-shell cube particle of preparation, accompanying drawing 2 is that the high-resolution TEM of the platinum cobalt nano core-shell cube particle of preparation schemes, from Fig. 1 and Fig. 2, the described platinum cobalt nano core-shell cube particle diameter size obtained is at 20 ~ 40nm, and wherein, the thickness of the shell be made up of simple substance cobalt is 2 ~ 5nm, described platinum cobalt nano core-shell cube good dispersion, composition is controlled, is magnetic, and is easy to collect.
Embodiment 2
Take 0.02mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 220 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum cobalt nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 3
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add octadecylamine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 140 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 230 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 40min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum cobalt nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 4
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 150 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum cobalt nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 5
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 15min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum cobalt nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 6
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 235 DEG C, after temperature stabilization 3min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum cobalt nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 7
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 8min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum cobalt nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 8
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol acetylacetone cobalt puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 1h, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum cobalt nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum cobalt nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 9
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 10
Take 0.02mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 220 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 11
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add octadecylamine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 140 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 230 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 40min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 12
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 150 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 13
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 15min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 14
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 235 DEG C, after temperature stabilization 3min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 15
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 8min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 16
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol nickel acetylacetonate puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 1h, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum nickel nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum nickel nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 17
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 18
Take 0.02mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 220 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 19
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add octadecylamine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 140 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 230 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 40min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 20
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 150 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 21
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 15min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 22
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 235 DEG C, after temperature stabilization 3min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 23
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 8min, pass into reaction of carbon monoxide 30min, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
Embodiment 24
Take 0.017mmol acetylacetone,2,4-pentanedione platinum and 0.05mmol ferric acetyl acetonade puts into there-necked flask, add oleyl amine and the 2mL oleic acid of 8ml, under argon shield, be uniformly mixed 5min in 130 DEG C of heating, obtain the first mixed solution A.First mixed solution A is transferred to rapidly in the oil bath pan of 225 DEG C, after temperature stabilization 5min, pass into reaction of carbon monoxide 1h, obtain black suspension B.Clean three times with chloroform after cool to room temperature, dried in vacuo overnight at 60 DEG C, obtain platinum iron nano core-shell cube.The described platinum cobalt nano core-shell cube that the described platinum iron nano core-shell cube and the embodiment 1 that obtain in the present embodiment obtain has similar structural form and characteristic.
In sum, the invention provides a kind of platinum alloy nano core-shell cube and preparation method thereof, the described cubical preparation method of platinum alloy nano core-shell comprises the steps: 1) under the protection of inert gas, acetylacetone,2,4-pentanedione platinum, acetylacetone metallic compound, alkylamine and alkyl acid are added in reaction vessel simultaneously and carries out Homogenization Treatments, obtain the first mixed solution mixed; 2) by step 1) described first mixed liquor that obtains transfers to rapidly in high temperature oil bath, and after the insulation scheduled time, pass into reducing gas and react, obtain black suspension; 3) by step 2) the described black suspension that obtains carries out organic solvent cleaning, Magneto separate and vacuum drying successively, namely obtains platinum alloy nano core-shell cube.Platinum alloy nano core-shell cube of the present invention and preparation method thereof has following beneficial effect: the cubical core of platinum alloy nano core-shell is made up of flower-shaped platinum alloy particle, shell is made up of cobalt, nickel or iron simple substance, good dispersion, and composition is controlled, be magnetic, be easy to collect; Present invention also offers the cubical preparation method of a kind of platinum alloy nano core-shell, adopt one kettle way oleyl amine system, by regulating and controlling the ratio of metal precursor and reaction time and temperature, obtain the platinum alloy nano core-shell cube that component is different, agents useful for same is nontoxic, and method is simple, is easy to operation.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (15)
1. a platinum alloy nano core-shell cube, it is characterized in that, described platinum alloy comprises metal platinum and the second metal, described platinum alloy nano core-shell cube comprises kernel and is coated on the shell of described kernel periphery, described kernel is flower-shaped platinum alloy particle kernel, and described shell is the second metal simple-substance shell.
2. platinum alloy nano core-shell cube according to claim 1, is characterized in that: described second metal is cobalt, and described flower-shaped platinum alloy particle kernel is the flower-shaped alloy particle kernel of platinum cobalt, and described shell is cobalt simple substance shell.
3. platinum alloy nano core-shell cube according to claim 1, is characterized in that: described second metal is nickel, and described flower-shaped platinum alloy particle kernel is the flower-shaped alloy particle kernel of platinum nickel, and described shell is nickel simple substance shell.
4. platinum alloy nano core-shell cube according to claim 1, is characterized in that: described second metal is iron, and described flower-shaped platinum alloy particle kernel is platinum ornamental work of iron shape alloy particle kernel, and described shell is iron simple substance shell.
5. platinum alloy nano core-shell cube according to claim 1, is characterized in that: described platinum alloy nano core-shell is cubical is of a size of 20nm ~ 40nm; The thickness of described shell is 2nm ~ 5nm.
6. the cubical preparation method of platinum alloy nano core-shell, is characterized in that, comprise the following steps:
1) under the protection of inert gas, acetylacetone,2,4-pentanedione platinum, acetylacetone metallic compound, alkylamine and alkyl acid are added in reaction vessel simultaneously and carries out Homogenization Treatments, obtain the first mixed solution mixed;
2) by step 1) described first mixed liquor that obtains transfers to rapidly in high temperature oil bath, and after the insulation scheduled time, pass into reducing gas and react, obtain black suspension;
3) by step 2) the described black suspension that obtains carries out organic solvent cleaning, Magneto separate and vacuum drying successively, namely obtains platinum alloy nano core-shell cube.
7. the cubical preparation method of platinum alloy nano core-shell according to claim 6, is characterized in that: described step 1) in, described acetylacetone metallic compound is acetylacetone cobalt, nickel acetylacetonate or ferric acetyl acetonade.
8. the cubical preparation method of platinum alloy nano core-shell according to claim 6, is characterized in that: described step 1) in, the temperature of Homogenization Treatments is 100 DEG C ~ 150 DEG C, and the time of Homogenization Treatments is 5min ~ 30min.
9. the cubical preparation method of platinum alloy nano core-shell according to claim 6, is characterized in that: described step 1) in, described alkylamine is one or more in oleyl amine, lauryl amine, cetylamine etc.
10. the cubical preparation method of platinum alloy nano core-shell according to claim 6, is characterized in that: described step 1) in, described alkyl acid is one or more in oleic acid, stearic acid, laurate.
The cubical preparation method of 11. platinum alloy nano core-shell according to claim 6, is characterized in that: described step 1) in, the mol ratio of described acetylacetone,2,4-pentanedione platinum and described acetylacetone metallic compound is 1:4 ~ 1:2.
The cubical preparation method of 12. platinum alloy nano core-shell according to claim 6, is characterized in that: described step 2) in, the temperature of described high temperature oil bath is 220 DEG C ~ 235 DEG C, and the described scheduled time is 2min ~ 8min.
The cubical preparation method of 13. platinum alloy nano core-shell according to claim 6, is characterized in that: described step 2) in, described reducing gas is carbon monoxide, and the flow velocity of described reducing gas is 100mL/min ~ 300mL/min.
The cubical preparation method of 14. platinum alloy nano core-shell according to claim 6, is characterized in that: described step 2) in, described in pass into the time that reducing gas carries out reacting be 20min ~ 1h.
The cubical preparation method of 15. platinum alloy nano core-shell according to claim 6, is characterized in that: described step 3) in, described organic solvent is one or more in ethanol, chloroform, n-hexane, acetone etc.
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