CN106694900B - A kind of preparation method of more metal nucleocapsid nanometer sheets - Google Patents
A kind of preparation method of more metal nucleocapsid nanometer sheets Download PDFInfo
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of preparation methods of more metal nucleocapsid nanometer sheets, and steps are as follows：Palladium nano sheet, metal-organic precursor body, dispersant and benzyl alcohol are mixed to get precursor solution, under oxygen-free environment, more metal nucleocapsid nanometer sheets are obtained after 160~220 DEG C of reactions.The present invention provides a kind of preparation methods of more metal nucleocapsid nanometer sheets, and method is simple, and repeatability is high, at low cost, and the more metal nucleocapsid nanometer sheets being prepared have two-dimentional nucleocapsid, size uniform, good dispersion, and size can regulate and control with wall thickness.
Description
Technical field
The present invention relates to the preparation fields of nano material, and in particular to a kind of preparation method of more metal nucleocapsid nanometer sheets.
Background technology
Noble metal nano particles show unique chemically and physically characteristic, there is very extensive development prospect.
Every unique physico-chemical property of noble metal nanometer material is all highly dependent with its grain size and pattern.Therefore, preparation method letter
Mild condition, easy to operate, size tunable, uniform, the quick, high yield of pattern etc. single, need are always various nano materials
The target that preparation method is pursued.In recent years, metal two-dimensional material is considered to have bigger serface and is imitated with Two-dimensional electron confinement
It answers, thus has huge catalytic applications potentiality.
Application No. is 201510106358.7 Chinese invention patents to disclose a kind of hollow palladium nano-crystal of two dimension, specific public
It has opened hexagon palladium nano sheet and bromide ion dressing agent and palladium presoma and reducing agent Hybrid Heating in a solvent, has collected washing
After obtain the hollow palladium nano sheet of two dimension.The hollow palladium nano-crystal of two dimension is a kind of ultra-thin cyclic structure, improves material and compares table
Area and atom utilization effectively enhance the catalytic performance of palladium nano-crystal.
Application No. is 201010117232.7 Chinese invention patents to disclose a kind of preparation method of nano sheets of platinum, specifically
It discloses then sodium polyphosphate is added to the organic compound of platinum in sodium hydroxide and potassium hydroxide fused salt mixt system
Solid powder, which is added in above-mentioned mixed molten liquid, to be vigorously stirred until by mixture after abundant reaction standing heat preservation a period of time cooling
It is carried out repeatedly washing the nanometer sheet that the product being centrifugally separating to obtain is platinum with water.This nanometer sheet is mutually interconnected by nano platinum particle
The polycrystalline two-dimensional plane structure of composition is connect, there is prodigious specific surface and surface selective catalysis activity.
Application No. is 201210141091.1 Chinese invention patents to disclose a kind of the expensive of self-supporting, monatomic thickness
Metal nano plate and preparation method thereof specifically discloses precious metal salt being dissolved in alcohols, utilizes the aldehyde radical pair of aldehyde compound
The suction-operated hydro-thermal method of noble metal particular crystal plane restores to obtain the noble metal nano-plate of self-supporting, monatomic thickness.
Although the synthesis that monometallic nanometer sheet may be implemented in some technological means has been developed now, in catalytic applications
In, thinking will be nanocrystalline in monometallic, and more metallic nano crystals embody the catalytic performance being obviously improved since it acts synergistically.Institute
With more Metal two-dimensional nano materials, which are believed, has more excellent catalytic performance and application potential.
Invention content
The present invention provides a kind of preparation methods of more metal nucleocapsid nanometer sheets, and method is simple, and repeatability is high, at low cost,
The more metal nucleocapsid nanometer sheets being prepared have two-dimentional nucleocapsid, size uniform, good dispersion, and size and wall thickness are all
It can regulate and control.
Specific technical solution is as follows：
A kind of preparation method of more metal nucleocapsid nanometer sheets, includes the following steps：
Palladium nano sheet, metal-organic precursor body, dispersant and benzyl alcohol are mixed to get precursor solution, oxygen-free environment
Under, more metal nucleocapsid nanometer sheets are obtained after 160~220 DEG C of reactions.
In the present invention, using palladium nano sheet as catalyst, catalysis solvent benzol Methanol Decomposition goes out under higher reaction temperatures
The products such as benzaldehyde, toluene, benzene and carbon monoxide, in the middle a small amount of carbon monoxide by one or two kinds of metal organic salts altogether also
Originally it was atom, and in the epitaxial growth of palladium nano sheet surface；Ultimately form the more metal nucleocapsid nanometer sheet structures of two dimension.This reaction needs
It is carried out in the environment of starvation, forms excessive carbon monoxide to avoid the excessive oxidation of benzyl alcohol, this can cause an oxygen
Change carbon hinders the strong adsorption on palladium nano sheet surface the deposition growing to other metallic atoms.
Preferably, the palladium nano sheet is hexagon palladium nano sheet, the length of side is 12~60nm.Hexagon palladium nano sheet
Upper and lower crystal face is (1,1,1), and side is (1,0,0) and (1,1,0), and palladium nano sheet is good masterplate material, can be used as and close
It is used at the seed of more metal nucleocapsid nanometer sheets.
The preparation method of palladium nano sheet is with reference to (Size-Controlled Synthesis of Pd such as Zhang Hui, Li Yi
Nanosheets for Tunable Plasmonic Properties, CrystEngComm, 2015,17,1833-1838) report
The preparation method of the palladium nano sheet in road, but this method has also been done and has further been improved.
Specifically preparation method is：
Palladium salt, cetyl trimethylammonium bromide, tungsten carbonyl, oxalic acid and polyvinylpyrrolidone are added to N, N diformazans
It is reacted in base formamide, the palladium nano sheet is prepared.
The citric acid used in original text chapter is replaced with oxalic acid, this improvement is to be based on a large number of experiments analysis result, through examination
It issues after examination and approval existing, is the hexagon palladium nano sheet that is prepared of raw material as catalyst using citric acid, the more metal nucleocapsids being prepared are received
There are more impurity (Fig. 6) in rice piece, and after being replaced with oxalic acid, impurity in the more metal nucleocapsid nanometer sheets being prepared
Content substantially reduces.
Further preferably, the substance withdrawl syndrome of palladium nano sheet is 1.0 × 10 in the precursor solution-3~3.0 × 10-3mol/L。
Preferably, the metal-organic precursor body be selected from acetylacetone,2,4-pentanedione platinum, nickel acetylacetonate, acetylacetone cobalt,
One or both of acetylacetone,2,4-pentanedione rhodium, acetylacetone,2,4-pentanedione ruthenium.It may finally obtain with different monometallics or alloy surface
Two-dimentional nucleocapsid nanometer sheet.The concentration of metal organic salt directly determines the thickness of the upper epitaxial layer of palladium nano sheet.Further preferably,
A concentration of the 1.0 × 10 of metal-organic precursor body in the precursor solution-4~5.0 × 10-4mol/L。
Preferably, the dispersant is polyvinylpyrrolidone, molecular weight is 10000~40000.Dispersant can
Promote the dispersion of palladium nano sheet in a solvent, prevents the reunion of palladium nano sheet, influence the formation of more metal nucleocapsid nanometer sheets.Into one
Step is preferred, a concentration of the 4.0 × 10 of dispersant in the precursor solution-4~1.2 × 10-3mol/L.Dispersant is in the concentration
Under so that the dispersion effect of palladium nano sheet is further promoted.
Preferably, reaction carries out under nitrogen or inert atmosphere；Further preferred nitrogen or argon gas.
Preferably, the reaction temperature is 160~200 DEG C, the time is 6~20h.Pd is to benzene in this temperature range
The catalyticing decomposition action of methanol is significantly and the metallic atom of reduction is deposited on diffusion rate with appropriate.
Compared with prior art, beneficial effects of the present invention are embodied in：
(1) other organic modifiers in addition to PVP are not introduced in the present invention, it is easy to operate, cost is relatively low, repeatability
It is high；
(2) more metal nucleocapsid nanometer sheet patterns produced by the present invention, size uniformity, and the component of more metal nucleocapsid nanometer sheets
And size and wall thickness can be regulated and controled；
(3) present invention is easily prepared and preserves, and final product is scattered in alcohol preservation.
Description of the drawings
Fig. 1 is the transmission electron microscope of palladium nano sheet prepared by embodiment 1 and the product that Examples 1 to 3 is prepared respectively
(TEM) figure；
Fig. 2 is the side for the product that Examples 1 to 3 is prepared respectively and positive spectral distribution phenogram；
Fig. 3 is transmission electron microscope (TEM) figure for the product that embodiment 4~7 is prepared respectively；
Fig. 4 is transmission electron microscope (TEM) figure for the product that embodiment 8~9 is prepared respectively；
Fig. 5 is transmission electron microscope (TEM) figure of product prepared by embodiment 10；
Fig. 6 is transmission electron microscope (TEM) figure of product prepared by comparative example 1.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention will be described in detail, but the present invention is not limited to this.
Embodiment 1：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 6mg acetylacetone,2,4-pentanediones platinum and 3.85mg acetylacetone,2,4-pentanediones
Nickel and 120mg polyvinylpyrrolidones (Mw=29000) be added in 10mL benzyl alcohol solutions, stirring make metal organic salt and
Polyvinylpyrrolidone fully dissolves, and reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, in argon gas
Middle sealing.Water heating kettle after encapsulation is put into convection oven and reacts 12h at 200 DEG C.After the completion of reaction, takes and react molten on a small quantity
Liquid centrifuges, and obtains palladium platinum nickel core-shell nano piece, TEM samples is prepared, by its pattern of transmission electron microscope observation, such as Fig. 1 (b) institutes
Show, the length of side of palladium platinum nickel core-shell nano piece is 18nm, thickness 2.6nm.(a) figure and (b) are respectively prepared by the present embodiment in Fig. 2
Palladium platinum nickel core-shell nano piece side and positive spectral distribution phenogram, be as can be seen from the figure successfully prepared with platinum nickel
The palladium platinum nickel core-shell nano chip architecture of alloy shell.
Embodiment 2：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 6mg acetylacetone,2,4-pentanediones platinum and 6mg acetylacetone,2,4-pentanediones rhodium with
And 120mg polyvinylpyrrolidones (Mw=29000) it is added in 10mL benzyl alcohol solutions, stirring makes metal organic salt and poly- second
Alkene pyrrolidone fully dissolves, and reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, close in argon gas
Envelope.Water heating kettle after encapsulation is put into convection oven and reacts 12h at 200 DEG C.After the completion of reaction, take a small amount of reaction solution from
The heart obtains palladium platinum rhodium core-shell nano piece, prepares TEM samples, by its pattern of transmission electron microscope observation, as shown in Fig. 1 (c),
The length of side of palladium platinum rhodium core-shell nano piece is 20nm, thickness 2.5nm.Fig. 2 (c) figures and (d) figure are respectively that the present embodiment prepares palladium
Platinum rhodium core-shell nano piece side and positive spectral distribution phenogram, are as can be seen from the figure successfully prepared with platinum-rhodium alloy
The palladium platinum rhodium core-shell nano chip architecture of shell.
Embodiment 3：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 6mg acetylacetone,2,4-pentanediones platinum and 6mg acetylacetone,2,4-pentanediones ruthenium with
And 120mg polyvinylpyrrolidones (Mw=29000) it is added in 10mL benzyl alcohol solutions, stirring makes metal organic salt and poly- second
Alkene pyrrolidone fully dissolves, and reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, close in argon gas
Envelope.Water heating kettle after encapsulation is put into convection oven and reacts 8h at 160 DEG C.After the completion of reaction, take a small amount of reaction solution from
The heart obtains palladium platinum ruthenium core-shell nano piece, prepares TEM samples, by its pattern of transmission electron microscope observation, as shown in Fig. 1 (d),
The length of side of palladium platinum ruthenium core-shell nano piece is 18nm, thickness 2.6nm.Fig. 2 (e) figures and (f) figure are respectively that the present embodiment prepares palladium
Platinum ruthenium core-shell nano piece side and positive spectral distribution phenogram, are as can be seen from the figure successfully prepared with platinum-ruthenium alloys
The palladium platinum ruthenium core-shell nano chip architecture of shell.
Embodiment 4：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 6mg acetylacetone,2,4-pentanediones platinum and 120mg polyethylene pyrroles
Pyrrolidone (Mw=29000) it is added in 10mL benzyl alcohol solutions, stirring keeps metal organic salt and polyvinylpyrrolidone abundant
Dissolving, reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, is sealed in argon gas.By the water after encapsulation
Hot kettle is put into convection oven reacts 12h at 200 DEG C.After the completion of reaction, takes a small amount of reaction solution to centrifuge, obtain palladium platinum nucleocapsid
Nanometer sheet prepares TEM samples, by its pattern of transmission electron microscope observation, as shown in Fig. 3 (a), and the side of palladium platinum core-shell nano piece
A length of 19nm, thickness 2.0nm are as can be seen from the figure successfully prepared palladium platinum core-shell nano chip architecture.
Embodiment 5：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 3.85mg nickel acetylacetonates and the poly- second of 120mg
Alkene pyrrolidone (Mw=29000) it is added in 10mL benzyl alcohol solutions, stirring makes metal organic salt and polyvinylpyrrolidone
Fully dissolving, reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, is sealed in argon gas.After encapsulating
Water heating kettle be put into convection oven and react 12h at 200 DEG C.After the completion of reaction, takes a small amount of reaction solution to centrifuge, obtain palladium nickel
Core-shell nano piece prepares TEM samples, by its pattern of transmission electron microscope observation, as shown in Fig. 3 (b), and palladium nickel core-shell nano piece
The length of side be 18nm, be as can be seen from the figure successfully prepared palladium nickel core-shell nano chip architecture.
Embodiment 6：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 6mg acetylacetone,2,4-pentanediones rhodium and 120mg polyethylene pyrroles
Pyrrolidone (Mw=29000) it is added in 10mL benzyl alcohol solutions, stirring keeps metal organic salt and polyvinylpyrrolidone abundant
Dissolving, reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, is sealed in argon gas.By the water after encapsulation
Hot kettle is put into convection oven reacts 8h at 180 DEG C.After the completion of reaction, takes a small amount of reaction solution to centrifuge, obtain palladium rhodium nucleocapsid
Nanometer sheet prepares TEM samples, by its pattern of transmission electron microscope observation, as shown in Fig. 3 (c), and the side of palladium rhodium core-shell nano piece
A length of 18nm is as can be seen from the figure successfully prepared palladium rhodium core-shell nano chip architecture.
Embodiment 7：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 6mg acetylacetone,2,4-pentanediones ruthenium and 120mg polyethylene pyrroles
Pyrrolidone (Mw=29000) it is added in 10mL benzyl alcohol solutions, stirring keeps metal organic salt and polyvinylpyrrolidone abundant
Dissolving, reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, is sealed in argon gas.By the water after encapsulation
Hot kettle is put into convection oven reacts 12h at 200 DEG C.After the completion of reaction, takes a small amount of reaction solution to centrifuge, obtain palladium ruthenium nucleocapsid
Nanometer sheet prepares TEM samples, by its pattern of transmission electron microscope observation, as shown in Fig. 3 (d), and the side of palladium ruthenium core-shell nano piece
A length of 18nm is as can be seen from the figure successfully prepared palladium ruthenium core-shell nano chip architecture.
Embodiment 8：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 3mg acetylacetone,2,4-pentanediones platinum and 1.98mg acetylacetone,2,4-pentanediones
Nickel and 120mg polyvinylpyrrolidones (Mw=29000) be added in 10mL benzyl alcohol solutions, stirring make metal organic salt and
Polyvinylpyrrolidone fully dissolves, and reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, in argon gas
Middle sealing.Water heating kettle after encapsulation is put into convection oven and reacts 12h at 200 DEG C.After the completion of reaction, takes and react molten on a small quantity
Liquid centrifuges, and obtains palladium platinum nickel core-shell nano piece, prepares TEM samples, by its pattern of transmission electron microscope observation, as a result such as Fig. 4
(a) similar to Example 1 shown in, but thickness is 2.4nm.
Embodiment 9：
Step 1：By 16mg palladium acetylacetonates, 60mg cetyl trimethylammonium bromides, 100mg tungsten carbonyls, 60mg oxalic acid
It is dissolved in 10mL n,N dimethylformamide with 30mg polyvinylpyrrolidones, stirring 1h makes each substance fully dissolve, will
Reaction solution is transferred in 25mL round-bottomed flasks, reacts 3h under the conditions of 60 DEG C.After the completion of reaction, reaction solution is centrifuged, obtains six
Side shape palladium nano sheet.Shown in palladium nano sheet pattern such as Fig. 1 (a), the average side length of hexagon palladium nano sheet is 18nm.
Step 2：By the 2.23mg palladium nano sheets obtained in step 1 and 9mg acetylacetone,2,4-pentanediones platinum and 5.78mg acetylacetone,2,4-pentanediones
Nickel and 120mg polyvinylpyrrolidones (Mw=29000) be added in 10mL benzyl alcohol solutions, stirring make metal organic salt and
Polyvinylpyrrolidone fully dissolves, and reaction solution, which is transferred to 15mL, to be had in the stainless steel water heating kettle of Teflon liner, in argon gas
Middle sealing.Water heating kettle after encapsulation is put into convection oven and reacts 12h at 200 DEG C.After the completion of reaction, takes and react molten on a small quantity
Liquid centrifuges, and obtains palladium platinum nickel core-shell nano piece, prepares TEM samples, by its pattern of transmission electron microscope observation, as a result such as Fig. 4
(b) similar to Example 1 shown in, but thickness is 2.8nm.
Embodiment 10
Preparation method is identical with embodiment 1, differs only in step 2, and 220 DEG C will be transferred in reaction temperature.System
Standby obtained product TEM as shown in figure 5, it can be seen from the figure that metallic atom be mainly deposited on the extension of palladium nano sheet and
Fail homoepitaxial in entire on piece.
Comparative example 1
Preparation method is identical with embodiment 1, differs only in step 1, and oxalic acid is replaced with citric acid.It is prepared into
The TEM of the product arrived schemes as shown in fig. 6, as can be seen from the figure of low quality due to palladium nano sheet so that has small a large amount of
Grain occurs.
Claims (10)
1. a kind of preparation method of more metal nucleocapsid nanometer sheets, which is characterized in that include the following steps：
Palladium nano sheet, metal-organic precursor body, dispersant and benzyl alcohol are mixed to get precursor solution, under oxygen-free environment,
More metal nucleocapsid nanometer sheets are obtained after 160~220 DEG C of reactions.
2. the preparation method of more metal nucleocapsid nanometer sheets according to claim 1, which is characterized in that the palladium nano sheet
For hexagon palladium nano sheet, the length of side is 12~60nm.
3. the preparation method of more metal nucleocapsid nanometer sheets according to claim 2, which is characterized in that the palladium nano sheet
Preparation method is：
Palladium salt, cetyl trimethylammonium bromide, tungsten carbonyl, oxalic acid and polyvinylpyrrolidone are added to N, N dimethyl first
It is reacted in amide, the palladium nano sheet is prepared.
4. the preparation method of more metal nucleocapsid nanometer sheets according to claim 3, which is characterized in that the precursor solution
The substance withdrawl syndrome of middle palladium nano sheet is 1.0 × 10-3~3.0 × 10-3mol/L。
5. the preparation method of more metal nucleocapsid nanometer sheets according to claim 1, which is characterized in that the metal is organic
One kind in acetylacetone,2,4-pentanedione platinum, nickel acetylacetonate, acetylacetone cobalt, acetylacetone,2,4-pentanedione rhodium, acetylacetone,2,4-pentanedione ruthenium of salt precursor body or
Two kinds.
6. the preparation method of more metal nucleocapsid nanometer sheets according to claim 5, which is characterized in that the precursor solution
A concentration of the 1.0 × 10 of middle metal-organic precursor body-4~5.0 × 10-4mol/L。
7. the preparation method of more metal nucleocapsid nanometer sheets according to claim 1, which is characterized in that the dispersant is
Polyvinylpyrrolidone, molecular weight are 10000~40000.
8. the preparation method of more metal nucleocapsid nanometer sheets according to claim 7, which is characterized in that the precursor solution
A concentration of the 4.0 × 10 of middle dispersant-4~1.2 × 10-3mol/L。
9. the preparation method of more metal nucleocapsid nanometer sheets according to claim 1~8 any claim, feature exist
In reaction carries out under nitrogen or inert atmosphere.
10. the preparation method of more metal nucleocapsid nanometer sheets according to claim 9, which is characterized in that through 160~200 DEG C
React 6~20h.
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| CN109759081A (en) * | 2019-02-20 | 2019-05-17 | 华侨大学 | A kind of preparation method and applications of two dimension multi-element metal nano material |
| CN111659899A (en) * | 2020-04-21 | 2020-09-15 | 华南师范大学 | Flower-like palladium oxide-gold nano composite material and preparation method and application thereof |
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| CN112643045B (en) * | 2020-12-18 | 2023-04-18 | 华侨大学 | Palladium-ruthenium ultrathin nanosheet, preparation method thereof and application of palladium-ruthenium ultrathin nanosheet as electrocatalyst |
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