CN106735295A - A kind of two-dimensional layer Au nanometer sheet materials and preparation method thereof - Google Patents
A kind of two-dimensional layer Au nanometer sheet materials and preparation method thereof Download PDFInfo
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- CN106735295A CN106735295A CN201611140572.5A CN201611140572A CN106735295A CN 106735295 A CN106735295 A CN 106735295A CN 201611140572 A CN201611140572 A CN 201611140572A CN 106735295 A CN106735295 A CN 106735295A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a kind of two-dimensional layer Au nanometer sheet materials and preparation method thereof, comprise the following steps：Silicon chip is immersed in sodium citrate ethanol colloidal sol, the silicon substrate with sodium citrate film is obtained by the method for liquid deposition；The silicon substrate with sodium citrate film and the ethanol solution of gold chloride are reacted, after reaction, silicon substrate and Au nanometer sheets is separated, you can obtained two-dimensional layer Au nanometer sheet materials.The preparation method of two-dimensional layer Au nanometer sheet materials provided herein, by liquid phase deposition, obtain sodium citrate film, and reduce gold chloride in this film surface, prepare Au nanometer sheets, with process is simple, single step reaction complete, reaction temperature is low, reaction condition is simple, low cost many advantages, such as.Prepared two-dimensional layer Au nanometer sheets, active strong, good dispersion, thickness is uniform, easily transfer, the advantages of size and dimension is controllable, its size range can cover nanometer to Centimeter Level.
Description
Technical field
Manufacturing technology field is prepared the present invention relates to nano metal material, is received in particular to a kind of two-dimensional layer Au
Rice sheet material and preparation method thereof.
Background technology
Au is considered as stable chemical nature within a very long time, lacks catalysis activity, and with good anti-oxidant
Property and corrosion resistance, be often used to make various jewellery and artwork Ornament, it is deep to be liked by people.But, when the size of Au reduces
During to Nano grade, many novel physicochemical characteristics that stock size cannot represent can be represented.For example：Nanometer Au particles exist
There is catalysis activity very high under low temperature, surface Raman scattered signals etc. can greatly be strengthened.Therefore Au nano materials are studied
Preparation method, and how size and the pattern of simple and effective its growth of control etc., have important practical significance and answer
With value.
It is one kind side being most frequently with present using reduction of sodium citrate gold chloride in existing Au nano materials preparation technology
Method.The method has flow simple, low cost, the advantages of generation Au granular mass is good.However, directly utilizing reduction of sodium citrate
Gold chloride, the product for obtaining is Au nano particles, rather than Au nanometer sheets.And it is reducing agent to utilize dimethyl sulfoxide (DMSO), although can
To prepare small size Au nanometer sheets, but preparation process needs to add substantial amounts of dispersant and stabilizer, while being prepared into
This also increased compared with reduction of sodium citrate method.The addition of dispersant and stabilizer, certainly will cause that follow-up removal, purification process become
Obtain sufficiently complex, the remnants of these dispersants and stabilizer will also largely effect on catalysis activity, the optics of generation Au nano materials
Performance etc..Sastry et al. (Ambarish Sanyal and Murali Sastry, Gold nanosheets via
reduction of aqueous chloroaurate ions by anthracene anions bound to a
Liquid-liquid interface, Chem.Commun., 11 (2003) 1236) using the chloroform reduction chlorine gold containing anthracene
Acid has prepared a kind of mixture containing Au nanometer sheets, and the method uses 4 hours of ultraviolet light, and preparation efficiency is low and makes
Standby flow is complicated, and the product for obtaining is mixture, and the content of Au nanometer sheets is not high.Ekgasit et al. (Supeera
Nootchanat,Chuchaat Thammacharoen,Boonrat Lohwongwatana and Sanong Ekgasit,
Formation of large H2O2-reduced gold nanosheets via starch-induced two-
Dimensional oriented attachment, RSC Adv., 3 (2013) 3707) using hydrogen peroxide (H2O2) and hydroboration
Sodium (NaBH4) used as reducing agent, starch is stabilizer, gold chloride provides Jin Yuan, has prepared the Au nanometer sheets of large area, but
It is that the method equally has the shortcomings that preparation flow is complicated, preparation efficiency is low, needs to add stabilizer.
Additionally, the preparation process of Au nanometer sheets is required for the hot environment, usual reaction temperature to reach 90 in the prior art
DEG C, or even it is heated to boiling.However, pyroreaction condition is one of the principal element for causing nano-particle to be reunited, it should as far as possible
Avoid.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of preparation method of two-dimensional layer Au nanometer sheet materials, existing to solve
Prepare in the method for nanometer Au materials, preparation flow is complicated, preparation efficiency is low, need addition stabilizer or reaction temperature too high
The shortcomings of, the preparation method of described two-dimensional layer Au nanometer sheet materials, by liquid phase deposition, obtains sodium citrate film,
And two-dimensional layer Au nanometer sheets are prepared in this film surface reduction gold chloride, completed with process is simple, single step reaction, anti-
Answer that temperature is low, reaction condition simple, low cost, easily transfer, many advantages, such as stabilizer and protective agent need not be added.
The second object of the present invention is that a kind of preparation method of described two-dimensional layer Au nanometer sheet materials of offer is made
Standby two-dimensional layer Au nanometer sheet materials, the method two-dimensional layer Au nanometer sheet materials, active strong, good dispersion, thickness
Uniformly, the advantages of size and dimension is controllable, its size range can cover nanometer to the two-dimensional layer Au nanometer sheets of Centimeter Level.
In order to realize above-mentioned purpose of the invention, spy uses following technical scheme：
A kind of preparation method of two-dimensional layer Au nanometer sheet materials, comprises the following steps：
Silicon chip is immersed in sodium citrate ethanol colloidal sol, sodium citrate film is obtained by the method for liquid deposition
Silicon substrate；
There is the silicon substrate of sodium citrate film to be reacted with the ethanol solution of gold chloride by described, after reaction, silicon is served as a contrast
Bottom and Au nanometer sheets are separated, you can obtain two-dimensional layer Au nanometer sheet materials.
The preparation method of two-dimensional layer Au nanometer sheet materials provided herein, using sodium citrate as reducing agent,
Can with simple flow, effectively reduce preparation cost.For other reducing agents, ethanol has relatively low surface tension and pole
Property, while ethanol is relative to water, it is a kind of excellent organic dispersing agent with lower fusing point (- 114 DEG C).Also, use second
Alcohol prepares Au nanometer sheets as solvent, can be in the situation without protective agent and stabilizer, and low temperature environment is prepared to be had
Dispersed high, the two-dimensional layer Au nanometer sheets that activity is strong, size is controllable.Therefore it is precursor liquid using sodium citrate ethanol colloidal sol,
Sodium citrate film is prepared by liquid deposition, gold chloride is reduced in the film surface, it is possible to achieve without any
On the premise of protective agent and stabilizer, low temperature synthesis has the two-dimensional layer Au nanometer sheets that dispersiveness is high, activity is strong.Meanwhile, because
For the size of sodium citrate film can be effectively controlled by adjusting related physical during liquid deposition, chemical parameters,
So the size of the two-dimensional layer Au nanometer sheets for preparing can also effectively be regulated and controled.The method have process is simple,
Single step reaction is completed, reaction temperature is low, reaction condition is simple, low cost, need not to add stabilizer and protective agent etc. many excellent
Point.
Preferably, the preparation method of the sodium citrate ethanol colloidal sol, specifically includes following steps：
To be dissolved in the water under two citric acid monohydrate sodium heating conditions, after stirring, obtain the water-soluble of sodium citrate
Liquid；, during the aqueous solution of sodium citrate is instilled into absolute ethyl alcohol under the rotating speed more than 1000rpm, obtain sodium citrate ethanol molten
Sol solution；Sodium citrate ethanol sol solution is carried out into centrifugal treating, sodium citrate ethanol colloidal sol is obtained after centrifugation；
It is furthermore preferred that the temperature of the heating is 45~60 DEG C；
It is furthermore preferred that the time of the stirring is 15~25 minutes；
It is furthermore preferred that the mass concentration of the aqueous solution of the sodium citrate is 60%~70%, and even more preferably, institute
The volume ratio of the aqueous solution and the absolute ethyl alcohol of stating sodium citrate is 1：(200~500).
The preparation of sodium citrate ethanol colloidal sol, is the presoma of the sodium citrate film of silicon substrate, at a high speed, violent stir
Mix down, the aqueous solution of sodium citrate is added drop-wise in absolute ethyl alcohol with dropper.Typically, sodium citrate is configured in a heated state
Into the aqueous solution, 60%~70%, the concentration ensure that in preparation process mass concentration, the stabilization of sodium citrate ethanol colloidal sol
Property.Preferably, in the range of above-mentioned mass concentration, the aqueous solution of sodium citrate is 1 with the volume ratio of absolute ethyl alcohol：(200~
500), in about per 100mL absolute ethyl alcohols, the aqueous solution of 0.2~0.5mL sodium citrates is added dropwise, according to the dropper of 3mL, about 8~
12 drops.The time stirred in preparation process is 15~25 minutes, is conducive to the aqueous solution of sodium citrate uniformly to divide in absolute ethyl alcohol
Dissipate, form the sodium citrate ethanol colloidal sol of stabilization.In addition, because sodium citrate is dissolved in water, the lemon for preparing
During sour sodium ethanol colloidal sol, using absolute ethyl alcohol, market purchase is 95% alcoholic solution, is prepared as using prior art anhydrous
Ethanol.
Preferably, the process of the centrifugation, specifically includes following steps：
The sodium citrate ethanol sol solution is centrifuged 10~14 minutes under 6000~8000rpm rotating speeds, after filtering
Precipitation is dispersed in absolute ethyl alcohol, then is centrifuged 10~14 minutes under 4000~5000rpm rotating speeds, isolated sodium citrate
Ethanol colloidal sol.
The size of the sodium citrate sol particle for preparing can be regulated and controled by the rotating speed for controlling to be centrifuged.It is different twice
After the centrifugal treating of rotating speed, filtering, the unprecipitated sodium citrate ethanol colloidal sol of milky that extraction is obtained.
Preferably, the cleaning method of the silicon chip, specifically includes following steps：
After silicon chip first is used into the concentrated sulfuric acid-hydrogen peroxide system digestion at 100~120 DEG C, then ammonia is used at 30~80 DEG C
Water-hydrogen peroxide system digestion, is finally cleaned by ultrasonic with acetone, the silicon chip after being cleaned；
It is furthermore preferred that twice the time of the digestion be 10~20 minutes.
Silicon chip is sufficiently cleaned, it is uniformly complete to ensure the sodium citrate film that it is formed above, and then ensure
The Au piece properties that obtain are complete, thickness is uniform, good dispersion.The concentrated sulfuric acid-hydrogen peroxide is cleaned to silicon chip, to solve silicon chip table
The organic impurities (mainly being brought by cutting fluid and home roll) of face residual.Ammoniacal liquor be in order to eliminate the impurity of silicon chip and cutting abrasive material,
Hydrogen peroxide is that, in order to the nubbin of cutting fluid is rinsed well, and acetone can help it to volatilize.
Preferably, the time of the immersion is 10~14 hours.
The process of immersion, is using the principle of liquid deposition.Show to form sodium citrate film in silicon chip.Because citric acid
Sodium is dissolved in water, so the sodium citrate film for preparing will avoid being contacted with water, using ethanol as solution, destroys film
Integrality.
Preferably, the mass concentration of the ethanol solution of the gold chloride is 0.20~0.25%.
In the application, reacted in sodium citrate film using gold chloride, and then obtained the Au pieces of given shape.Chlorine gold
The concentration of acid embodies the effective ion quantity that interface participates in reaction, controls the concentration of gold chloride, can effectively control reaction
Speed, obtains the Au nanometer sheets that thickness is uniform, shape is complete.
Preferably, the temperature of the reaction is 20~50 DEG C, and the time of reaction is 4~12 hours；
It is furthermore preferred that the temperature of the reaction is 25~40 DEG C, the time of reaction is 6~8 hours；
It is further preferred that the temperature of the reaction is 25~30 DEG C, the time of reaction is 5~6 hours.
The preparation method of two-dimensional layer Au nanometer sheet materials provided herein, reaction temperature condition requirement is not harsh,
30 DEG C or so can react, and the reaction time is short, be adapted to produce in enormous quantities and extensive use.
Preferably, described separation to silicon substrate and Au nanometer sheets is operated using the method for ultrasonic vibration, more excellent
Choosing, the time of the ultrasonic vibration is 1~5 minute, and the time of the further preferred ultrasonic vibration is 2~3 minutes.
Ultrasonic vibration makes Au nanometer sheets be sunk to the bottom with silicon to separate, the integrality of Au nanometer sheets is not destroyed.
Two-dimensional layer Au nanometer sheet materials prepared by the preparation method of two-dimensional layer Au nanometer sheet materials as described above.
Preferably, the two-dimensional layer Au nanometer sheets material is N sides shape, wherein, N >=3.
Prepared two-dimensional layer Au nanometer sheet materials, with good dispersion, thickness is uniform, size and dimension is controllable etc.
Advantage, its size range covers nanometer to micron-sized two-dimensional layer Au nanometer sheets.Often it is made as triangle, hexagon etc. many
Side shape, controlled shape, size is controllable.
Compared with prior art, beneficial effects of the present invention are：
(1) preparation method of two-dimensional layer Au nanometer sheet materials provided herein, by liquid phase deposition, obtains lemon
Lemon acid sodium film, and two-dimensional layer Au nanometer sheets are prepared in this film surface reduction gold chloride, with process is simple, a step
Reaction complete, reaction temperature is low, reaction condition is simple, low cost many advantages, such as.
(2) preparation method of two-dimensional layer Au nanometer sheet materials provided herein, using sodium citrate as reduction
Agent, can simplify preparation technology, effectively reduce preparation cost, without protective agent and stabilizer.
(3) two-dimensional layer Au nanometers prepared by the preparation method of two-dimensional layer Au nanometer sheet materials provided herein
Sheet material, the advantages of active strong, good dispersion, thickness are uniform, size and dimension is controllable, its size range covers nanometer
To the two-dimensional layer Au nanometer sheets of Centimeter Level.
Brief description of the drawings
In order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art, below will be to specific
The accompanying drawing to be used needed for implementation method or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
The method flow diagram for preparing two-dimensional layer Au nanometer sheets that Fig. 1 is provided for the embodiment of the present application；
The polygon Au nanometer sheet TEM photos that Fig. 2 is provided by the embodiment of the present application 1；
The polygon Au nanometer sheet TEM photos that Fig. 3 is provided by the embodiment of the present application 2；
The hexagon Au nanometer sheet TEM photos that Fig. 4 is provided by the embodiment of the present application 3；
The triangle Au nanometer sheet TEM photos that Fig. 5 is provided by the embodiment of the present application 4；
The TEM diffractional lattices of the triangle Au nanometer sheet monocrystalline that Fig. 6 is provided by the embodiment of the present application.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with the drawings and specific embodiments, but
It is it will be understood to those of skill in the art that following described embodiment is a part of embodiment of the invention, rather than whole
Embodiment, is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained under the premise of creative work is not made, belongs to guarantor of the present invention
The scope of shield.Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same
Or the unreceipted production firm person of instrument, it is the conventional products that can be obtained by commercially available purchase.
The two-dimensional layer Au nanometers of flow chart of piece preparation method that Fig. 1 is provided by the embodiment of the present application 1-4, specific implementation
Example method is as shown in embodiment 1-4.
Embodiment 1
The method for preparing polygonal Au nanometer sheets provided herein, specifically includes following steps：
(1) sodium citrate colloidal sol, is prepared
(a), under the conditions of 50 DEG C, by 40g (Na3C6H5O7·2H2O (mass percent is in) being dissolved in the 20mL aqueous solution
66.7%) after, being sufficiently stirred for 20 minutes, sodium citrate aqueous solution is obtained, it is standby；
(b), 100mL absolute ethyl alcohols are prepared with beaker, be stirred vigorously with magnetic stirring apparatus, low whipping speed is more than
Under the conditions of 1000rpm, instill about 8 drop (0.2ml) the step of (a) in sodium citrate aqueous solution, prepare sodium citrate second
Alcosol solution, is repeated 2 times, and obtains amounting to 200ml sodium citrate ethanol sol solutions；
(c), by the 200ml sodium citrate ethanol sol solutions in step (b) by centrifugal treating, first turn in 6000rpm
, be dispersed in precipitation in absolute ethyl alcohol after filtering by the lower centrifugation of speed 12 minutes, then is centrifuged 12 minutes under 4000rpm rotating speeds, filtering,
Obtain milky sodium citrate ethanol colloidal sol.
(2) sodium citrate film, is prepared
(d), polygon silicon chip is taken, after silicon chip first is used into the concentrated sulfuric acid-hydrogen peroxide system digestion 15 minutes at 120 DEG C, then
Ammoniacal liquor-hydrogen peroxide system digestion 15 minutes is used at 30 DEG C, is finally cleaned by ultrasonic with acetone, the silicon after being cleaned
Piece；
(e), by the silicon chip after cleaning in step (d), it is immersed in the sodium citrate ethanol colloidal sol obtained in step (1),
It is standing and soak for 12 hours, obtains the silicon substrate with sodium citrate film.
(3) Au nanometer sheets, are prepared
(f), by HAuCl4·4H2O is dissolved in absolute ethyl alcohol, prepares the chlorauric acid solution that mass percent is 0.21%：
(g), the gold chloride that the silicon substrate with sodium citrate film obtained in step (2) is placed in step (f) preparation
Reacted 6 hours at 30 DEG C in solution, after reaction terminates, silicon is sunk to the bottom as in ethanol solution, ultrasonic vibration 1 minute exists
Polygon Au nanometer sheet materials are obtained in ethanol solution.
Embodiment 2
The method for preparing polygonal Au nanometer sheets provided herein, specifically includes following steps：
(1) sodium citrate colloidal sol, is prepared
(a), under the conditions of 45 DEG C, by Na3C6H5O7·2H2O is dissolved in the 20mL aqueous solution, after being sufficiently stirred for 15 minutes,
The sodium citrate aqueous solution that mass percent is 60% is prepared, it is standby；
(b), 100mL absolute ethyl alcohols are prepared with beaker, be stirred vigorously with magnetic stirring apparatus, low whipping speed is more than
Under the conditions of 1000rpm, instill about 12 drop (0.5ml) the step of (a) in sodium citrate aqueous solution, prepare sodium citrate second
Alcosol solution, is repeated 2 times, and obtains amounting to 200ml sodium citrate ethanol sol solutions；
(c), by the 200ml sodium citrate ethanol sol solutions in step (b) by centrifugal treating, first turn in 8000rpm
, be dispersed in precipitation in absolute ethyl alcohol after filtering by the lower centrifugation of speed 10 minutes, then is centrifuged 10 minutes under 5000rpm rotating speeds, filtering,
Obtain milky sodium citrate ethanol colloidal sol.
(2) sodium citrate film, is prepared
(d), polygon silicon chip is taken, after silicon chip first is used into the concentrated sulfuric acid-hydrogen peroxide system digestion 20 minutes at 100 DEG C, then
Ammoniacal liquor-hydrogen peroxide system digestion 10 minutes is used at 80 DEG C, is finally cleaned by ultrasonic with acetone, the silicon after being cleaned
Piece；
(e), by the silicon chip after cleaning in step (d), it is immersed in the sodium citrate ethanol colloidal sol obtained in step (1),
It is standing and soak for 14 hours, obtains the silicon substrate with sodium citrate film.
(3) Au nanometer sheets, are prepared
(f), by HAuCl4·4H2O is dissolved in absolute ethyl alcohol, prepares the chlorauric acid solution that mass percent is 0.20%：
(g), the gold chloride that the silicon substrate with sodium citrate film obtained in step (2) is placed in step (f) preparation
Reacted 12 hours at 20 DEG C in solution, after reaction terminates, silicon is sunk to the bottom as in ethanol solution, ultrasonic vibration 3 minutes exists
Polygon Au nanometer sheet materials are obtained in ethanol solution.
Embodiment 3
The method of the Au nanometer sheets for preparing hexagon provided herein, specifically includes following steps：
(1) sodium citrate colloidal sol, is prepared
(a), under the conditions of 60 DEG C, by Na3C6H5O7·2H2O is dissolved in the 20mL aqueous solution, after being sufficiently stirred for 25 minutes,
The sodium citrate aqueous solution that mass percent is 70% is prepared, it is standby；
(b), 100mL absolute ethyl alcohols are prepared with beaker, be stirred vigorously with magnetic stirring apparatus, low whipping speed is more than
Under the conditions of 1000rpm, instill about 10 drop (0.3ml) the step of (a) in sodium citrate aqueous solution, prepare sodium citrate second
Alcosol solution, is repeated 2 times, and obtains amounting to 200ml sodium citrate ethanol sol solutions；
(c), by the 200ml sodium citrate ethanol sol solutions in step (b) by centrifugal treating, first turn in 6000rpm
, be dispersed in precipitation in absolute ethyl alcohol after filtering by the lower centrifugation of speed 10 minutes, then is centrifuged 10 minutes under 4000rpm rotating speeds, filtering,
Obtain milky sodium citrate ethanol colloidal sol.
(2) sodium citrate film, is prepared
(d), hexagon silicon chip is taken, after silicon chip first is used into the concentrated sulfuric acid-hydrogen peroxide system digestion 10 minutes at 120 DEG C, then
Ammoniacal liquor-hydrogen peroxide system digestion 20 minutes is used at 50 DEG C, is finally cleaned by ultrasonic with acetone, the silicon after being cleaned
Piece；
(e), by the silicon chip after cleaning in step (d), it is immersed in the sodium citrate ethanol colloidal sol obtained in step (1),
It is standing and soak for 10 hours, obtains the silicon substrate with sodium citrate film.
(3) Au nanometer sheets, are prepared
(f), by HAuCl4·4H2O is dissolved in absolute ethyl alcohol, prepares the chlorauric acid solution that mass percent is 0.25%：
(g), the gold chloride that the silicon substrate with sodium citrate film obtained in step (2) is placed in step (f) preparation
Reacted 4 hours at 50 DEG C in solution, after reaction terminates, silicon is sunk to the bottom as in ethanol solution, ultrasonic vibration 5 minutes exists
Six shape Au nanometer sheet materials are obtained in ethanol solution.
Embodiment 4
The method of the Au nanometer sheets for preparing triangle provided herein, specifically includes following steps：
(1) sodium citrate colloidal sol, is prepared
(a), under the conditions of 55 DEG C, by Na3C6H5O7·2H2O is dissolved in the 20mL aqueous solution, after being sufficiently stirred for 20 minutes,
The sodium citrate aqueous solution that mass percent is 65% is prepared, it is standby；
(b), with the step (b) in embodiment 1；
(c), with the step (c) in embodiment 1.
(2) sodium citrate film, is prepared
(d), with the step (d) in embodiment 1；
(e), with the step (e) in embodiment 1.
(3) Au nanometer sheets, are prepared
(f), by HAuCl4·4H2O is dissolved in absolute ethyl alcohol, prepares the chlorauric acid solution that mass percent is 0.22%：
(g), the gold chloride that the silicon substrate with sodium citrate film obtained in step (2) is placed in step (f) preparation
Reacted 6 hours at 40 DEG C in solution, after reaction terminates, silicon is sunk to the bottom as in ethanol solution, ultrasonic vibration 2 minutes exists
Triangle Au nanometer sheet materials are obtained in ethanol solution.
Experimental example electron lens (TEM) is tested
The Au nanometer sheets material provided the embodiment of the present application 1-4 carries out TEM tests, and test result is as shown in Figure 2-5.
Test result indicate that, the preparation method of two-dimensional layer Au nanometer sheet materials provided herein is prepared to obtain
Au nanometer sheets good dispersion, thickness is uniform, size and dimension is controllable.Fig. 6 is the TEM diffractional lattices of Au nanometer sheet monocrystalline,
Result shows that the two-dimensional layer Au nanometer sheets of synthesis are monocrystalline, and diffraction spot has good symmetry explanation synthesis Au nanometer sheets
Defect seldom, diffraction spot completely illustrates face-centered cubic (fcc) lattice structure of Au.
In sum, the preparation method of two-dimensional layer Au nanometer sheet materials provided herein, by liquid phase deposition,
Sodium citrate film is obtained, and two-dimensional layer Au nanometer sheets are prepared in this film surface reduction gold chloride, with technique letter
Single, single step reaction is completed, reaction temperature is low, reaction condition is simple, low cost many advantages, such as.Prepared two-dimensional layer Au receives
Rice sheet material, active strong, good dispersion, the advantages of thickness is uniform, size and dimension is controllable, its size range covers nanometer
To micron-sized two-dimensional layer Au nanometer sheets.
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that various embodiments above is only used
To illustrate technical scheme, rather than its limitations；It will be understood by those within the art that：Without departing substantially from this hair
In the case of bright spirit and scope, the technical scheme described in foregoing embodiments can be modified, or to wherein
Some or all of technical characteristic carries out equivalent；And these modifications or replacement, do not make the essence of appropriate technical solution
Depart from the scope of various embodiments of the present invention technical scheme；It is, therefore, intended that including belonging to the present invention in the following claims
In the range of all these substitutions and modifications.
Claims (10)
1. a kind of preparation method of two-dimensional layer Au nanometer sheet materials, it is characterised in that comprise the following steps：
Silicon chip is immersed in sodium citrate ethanol colloidal sol, the silicon with sodium citrate film is obtained by the method for liquid deposition
Substrate；
The silicon substrate with sodium citrate film and the ethanol solution of gold chloride are reacted, after reaction, to silicon substrate
Separated with Au nanometer sheets, you can obtain two-dimensional layer Au nanometer sheet materials.
2. the preparation method of two-dimensional layer Au nanometer sheet materials according to claim 1, it is characterised in that the citric acid
The preparation method of sodium ethanol colloidal sol, specifically includes following steps：
To be dissolved in the water under sodium citrate heating condition, after stirring, obtain the aqueous solution of sodium citrate；By sodium citrate
The aqueous solution instill absolute ethyl alcohol under the rotating speed more than 1000rpm, obtain sodium citrate ethanol sol solution；By citric acid
Sodium ethanol sol solution carries out centrifugal treating, and sodium citrate ethanol colloidal sol is obtained after centrifugation；
Preferably, the temperature of the heating is 45~60 DEG C；
Preferably, the time of the stirring is 15~25 minutes；
Preferably, the mass concentration of the aqueous solution of the sodium citrate is 60%~70%, it is furthermore preferred that the sodium citrate
The aqueous solution is 1 with the volume ratio of the absolute ethyl alcohol：(200~500).
3. the preparation method of two-dimensional layer Au nanometer sheet materials according to claim 2, it is characterised in that the centrifugation
Process, specifically includes following steps：
The sodium citrate ethanol sol solution is centrifuged 10~14 minutes under 6000~8000rpm rotating speeds, will be heavy after filtering
Shallow lake is dispersed in absolute ethyl alcohol, then is centrifuged 10~14 minutes under 4000~5000rpm rotating speeds, isolated sodium citrate ethanol
Colloidal sol.
4. the preparation method of two-dimensional layer Au nanometer sheet materials according to claim 1, it is characterised in that the silicon chip
Cleaning method, specifically includes following steps：
By silicon chip at 100~120 DEG C first with after the concentrated sulfuric acid-hydrogen peroxide system digestion, then using ammoniacal liquor-bis- at 30~80 DEG C
Oxygen aqueous systems digestion, is finally cleaned by ultrasonic with acetone, the silicon chip after being cleaned；
Preferably, the time of the digestion is 10~20 minutes twice.
5. the preparation method of two-dimensional layer Au nanometer sheet materials according to claim 1, it is characterised in that the immersion
Time is 10~14 hours.
6. the preparation method of two-dimensional layer Au nanometer sheet materials according to claim 1, it is characterised in that the gold chloride
Ethanol solution mass concentration be 0.20~0.25%.
7. the preparation method of two-dimensional layer Au nanometer sheet materials according to claim 1, it is characterised in that the reaction
Temperature is 20~50 DEG C, and the time of reaction is 4~12 hours；
Preferably, the temperature of the reaction is 25~40 DEG C, and the time of reaction is 6~8 hours；
It is furthermore preferred that the temperature of the reaction is 25~30 DEG C, the time of reaction is 5~6 hours.
8. the preparation method of two-dimensional layer Au nanometer sheet materials according to claim 1, it is characterised in that described to be served as a contrast to silicon
Bottom and Au nanometer sheets are separated to be operated using the method for ultrasonic vibration, and the time of the ultrasonic vibration is 1~5 minute,
The time of the preferred ultrasonic vibration is 2~3 minutes.
9. the two-dimensional layer prepared by the preparation method of the two-dimensional layer Au nanometer sheet materials according to claim any one of 1-8
Shape Au nanometer sheet materials.
10. two-dimensional layer Au nanometer sheet materials according to claim 9, it is characterised in that described two-dimensional layer Au nanometers
Sheet material is N sides shape, wherein, N >=3.
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