CN108655414A - Simple method for rapidly and massively preparing two-dimensional Ag micro-nano material - Google Patents
Simple method for rapidly and massively preparing two-dimensional Ag micro-nano material Download PDFInfo
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- CN108655414A CN108655414A CN201810619469.1A CN201810619469A CN108655414A CN 108655414 A CN108655414 A CN 108655414A CN 201810619469 A CN201810619469 A CN 201810619469A CN 108655414 A CN108655414 A CN 108655414A
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002063 nanoring Substances 0.000 claims abstract description 7
- 230000009467 reduction Effects 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 5
- 239000002105 nanoparticle Substances 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims description 19
- 239000000654 additive Substances 0.000 claims description 11
- 229910019931 (NH4)2Fe(SO4)2 Inorganic materials 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 101710134784 Agnoprotein Proteins 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract description 2
- 239000002135 nanosheet Substances 0.000 abstract 4
- 239000002127 nanobelt Substances 0.000 abstract 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 239000010970 precious metal Substances 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- -1 at room temperature Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Abstract
A simple method for rapidly and massively preparing a two-dimensional Ag micro-nano material relates to the technical field of preparation and application of precious metal nano materials. The preparation method comprises two processes of rapid mixing and ultrasonic reaction of reaction liquid, and the ultrasonic reaction is adopted to lead Fe to react at room temperature2+Fast reduction of Ag+And obtaining the two-dimensional Ag micro-nano material. The size of the Ag micro-nano belt and sheet is 5-20 mu m, the Ag micro-nano belt and sheet are in a multilayer structure state, and the Ag micro-nano belt and sheet are assembled by a plurality of nano sheets with the thickness of 10-20 nm; the prepared Ag micro-nano ring is assembled by countless Ag nano particles. The Ag micro-nano material obtained by the method has the characteristics of high yield, good dispersibility, good film forming property and the like, and provides a material basis and guarantee for the preparation of the high-performance SERS substrate. The two-dimensional Ag micro-nano material with various forms can be quickly obtained by simply controlling the type and the using amount of the ferrous salt, and the method has the advantages of simple operation, less required raw materials, high yield, excellent performance, low cost and the like.
Description
Technical field
The present invention relates to the preparation and application technical fields of noble metal nanometer material, are specifically related to a kind of quick magnanimity system
The simple and easy method of standby two dimension Ag micro Nano materials.
Background technology
Silver-colored (Ag) nano material has surface enhanced Raman scattering effect (Surface-Enhanced Raman
Scattering, SERS), SERS spectra technology is capable of providing " fingerprint " characteristic peak of sample, has highly sensitive detection and knows
The advantages such as not, thus be concerned in fields such as environmental organic pollutant analyses, it is acknowledged as a kind of very promising ring
Border analysis means.
Ag micro Nano materials have some double gradings of micro-meter scale material and nano structural material：Such as high ratio table
Area, good optical property, high chemistry and mechanical stability, in necks such as electrocondution slurry, optical device, catalysis and medicine
It is widely used in domain.Two-dimentional Ag micro Nano materials have good film forming and photoelectric properties, in terms of the preparation of SERS substrates
It is widely used.With AgNO3During preparing Ag nano materials for raw material, it is widely adopted there are many reducing agent at present.
For example, polyvinylpyrrolidone, sodium citrate, ethylene glycol, sodium borohydride, vitamin C, n,N-Dimethylformamide and various
Biomass extract etc. is that can make to be common reducing agent.With these reducing agents can get it is such as linear, rodlike, cube and
The series As g nano materials such as tripartite.
Invention content
For the shortcoming in the presence of the prior art, the present invention provides a kind of quick magnanimities to prepare two dimension Ag micro-nanos
The simple and easy method of rice material, using Fe2+Quickly reduction Ag+Obtain several two dimension Ag micro Nano materials, the Ag micro Nano materials at
Film property is good, has excellent optical property.
To achieve the goals above, the technical solution adopted in the present invention is：A kind of quick magnanimity preparation two dimension Ag micro-nanos
The simple and easy method of rice material includes quick mixing and two processes of ultrasonic reaction of reaction solution, specifically adopts at ambient temperature
Make Fe with ultrasonic reaction2+Quickly reduction Ag+Obtain two-dimentional Ag micro Nano materials.
As the optimal technical scheme of preparation method of the present invention, specifically by the solid FeSO of 0.05~0.4g4.7H2O or
Solid (NH4)2Fe(SO4)2It rapidly joins to the AgNO of a concentration of 0.01mol/L of 50mL3In solution, at room temperature ultrasonic reaction 2~
10min is to get two-dimentional Ag micro Nano materials.
In the quick magnanimity of the present invention prepares the simple and easy method of two dimension Ag micro Nano materials, as solid FeSO4.7H2O's
Ag micro-nano bands are prepared in additive amount when being 0.15~0.35g, be prepared when additive amount is less than 0.15g or more than 0.35g
Micro-nano of random Ag.As solid (NH4)2Fe(SO4)2Additive amount that Ag is prepared is micro-nano when being 0.15~0.35g
Micro-nano of random Ag is prepared when additive amount is less than 0.15g or more than 0.35g in ring.
The size of the micro-nano bands of Ag, micro-nano of Ag that the present invention is prepared is 5~20 μm, is in multilayered structure state,
If being assembled by the nanometer sheet that dry thickness is 10~20nm；The micro-nano rings of Ag being prepared are assembled by countless Ag nano particles
It forms.
The two-dimentional Ag micro Nano materials that the present invention obtains can be prepared into quasi- monocrystalline Ag films, it is specifically that two-dimentional Ag is micro-
Nano material is distributed in absolute alcohol after formation Ag slurries, is dripped on silicon chip or sheet glass, to obtain being orientated consistent quasi- list
Brilliant Ag films.
The present invention is with AgNO3For silver-colored source, Fe2+(FeSO4.7H2O and (NH4)2Fe(SO4)2) it is reducing agent, at room temperature, lead to
It crosses ultrasonic quickly reduction method and is successfully prepared a variety of two dimension Ag micro Nano materials.It is compared with existing preparation method, the present invention also has
It has the advantage that：
1), the method for the present invention realizes the form controllable preparation of two-dimentional Ag micro Nano materials, obtained Ag micro Nano materials
The features such as yield height, dispersibility and good film-forming property, the preparation for high-performance SERS substrates provides material foundation and guarantee, it is expected to
The fields such as preparation and conductive film actual production for SERS substrates.
2), the method for the present invention can be quickly obtained the two-dimentional Ag of variform by simply controlling ferrous salt type and dosage just
Micro Nano material, has that easy to operate, required raw material are few, and yield is high, the advantages that haveing excellent performance and is at low cost.
Description of the drawings
Fig. 1 is the SEM and XRD spectra that each product is obtained in embodiment 1；
Fig. 2 is the SEM figures that each product is obtained in embodiment 2；
Fig. 3 is the SEM figures that each product is obtained in embodiment 3；
Fig. 4 is XRD the and UV-vis spectrograms of each product in embodiment 4.
Specific implementation mode
Prepare the simple and easy method of two dimension Ag micro Nano materials to the quick magnanimity of the present invention with attached drawing with reference to embodiments
It makes and being discussed further.X-ray powder diffraction is respectively adopted in structure, form and the optical property of the method for the present invention products therefrom
(XRD, D3500) and field emission scanning electron microscope (FE-SEM, SU8010) and UV-vis spectroscopy spectrometer (UV-vis,
V-650 it) characterizes and analyzes.
Embodiment 1：The preparation and representation of 3 kinds of two dimension Ag micro Nano materials
To a concentration of 0.01mol/L AgNO of 3 groups of 50mL30.05g FeSO are separately added into aqueous solution4.7H2O solids,
0.15g FeSO4.7H2O solids and 0.3g (NH4)2Fe(SO4)2After solid, at room temperature by ultrasonic fast reaction after, you can obtain
Obtain three kinds of Ag random micro-nano (see Fig. 1 a), the micro-nano bands of Ag (see Fig. 1 b) and the micro-nano rings of Ag (see Fig. 1 c) micro-nano materials
Material.XRD analysis result such as Fig. 1 d (a, b, c distinguish the XRD spectra of counterpiece, band and ring) institute of 3 kinds of two dimension Ag micro Nano materials
Show.
Embodiment 2：FeSO4.7H2Influence of the O solids usage amount to product form
To a concentration of 0.01mol/L AgNO of 4 groups of 50mL3Be separately added into aqueous solution 0.05g, 0.25g, 0.35g and
The FeSO of 0.40g4.7H2O solids, it is as shown in Figure 2 by each product obtained after ultrasonic quickly reduction reaction at room temperature.It can see
Go out, with FeSO4.7H2The shape of the increase of O solid usage amounts, product will be changed from random micro-nano to micro-nano band
(see Fig. 2 a, Fig. 2 b and Fig. 2 c), works as FeSO4.7H2O usage amounts are more than after 0.35g reaches 0.40g, and product will become random again
Micro-nano (see Fig. 2 d).
It follows that solid FeSO4.7H2The micro-nano bands of Ag are prepared when being 0.15~0.35g in the additive amount of O, add
Micro-nano of random Ag is prepared when amount is less than 0.15g or more than 0.35g.
Embodiment 3：(NH4)2Fe(SO4)2Morphology influence of the solid dosage to product
To a concentration of 0.01mol/L AgNO of 4 groups of 50mL3Be separately added into aqueous solution 0.05g, 0.25g, 0.35g and
(the NH of 0.40g4)2Fe(SO4)2It is as shown in Figure 3 by each product obtained after ultrasonic quickly reduction reaction at room temperature when solid.
As can be seen that with (NH4)2Fe(SO4)2The increase of solid usage amount, the shape of product also will be from random micro-nano to micro-
Nano-rings change (see Fig. 3 a, Fig. 3 b and Fig. 3 c), as (NH4)2Fe(SO4)2Usage amount is more than product after 0.35g reaches 0.40g
Also will become random micro-nano (see Fig. 3 d).Ag0Forming process and embodiment 2 are identical (see reaction equation (1)).
It follows that solid (NH4)2Fe(SO4)2Additive amount be 0.15~0.35g when the micro-nano rings of Ag are prepared,
Micro-nano of random Ag is prepared when additive amount is less than 0.15g or more than 0.35g.
Integrated embodiment 2 and 3 as a result, being found through experiments that, ultrasound can accelerate rate of reduction.At room temperature, Fe2+It can be quickly
Restore Ag+, to obtain simple substance Ag0.The above process can be indicated with formula (1).
Embodiment 4：The structure of micro-nano film of Ag and optical property research
The sheet Ag micro-nano powders material that embodiment 1 obtains is obtained into aggregation by tabletting respectively and film (will
Two-dimentional Ag micro Nano materials are distributed in absolute alcohol after formation Ag slurries, are dripped on silicon chip or sheet glass) form Ag films, the two
XRD test results are as shown in fig. 4 a.The XRD spectra difference of tabletting and film is very big it can be seen from Fig. 4 a, and after film, Ag is micro-
Nanometer sheet or the orientation of band are consistent ([111] crystal orientation), and so as to obtain the Ag films of quasi- monocrystalline, this is the SERS substrates of high activity
Preparation provide guarantee.
Fig. 4 b are the visible absorption spectrum figure for 3 kinds of two dimension Ag micro Nano materials that embodiment 1 obtains, and comparing figure can see
Go out, sheet (a), the main absorption peak position of band-like (b) and ring-type (c) Ag micro Nano materials are~321nm, illustrate three and be by
Ag nano structured units assemble.In addition, band-like and cyclic annular Ag micro Nano materials~490nm (see figure (b)) and~
There is certain absorption at 612nm (see figure (c)), this may be larger relevant with the size and structure of the two.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or substitutes by a similar method, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (6)
1. a kind of quick magnanimity prepares the simple and easy method of two dimension Ag micro Nano materials, which is characterized in that including the quick of reaction solution
Mixing and two processes of ultrasonic reaction, specifically use ultrasonic reaction to make Fe at ambient temperature2+Quickly reduction Ag+Obtain two dimension
Ag micro Nano materials.
2. preparation method as described in claim 1, which is characterized in that by the solid FeSO of 0.05~0.4g4.7H2O or solid
(NH4)2Fe(SO4)2It rapidly joins to the AgNO of a concentration of 0.01mol/L of 50mL3In solution, at room temperature ultrasonic reaction 2~
10min is to get two-dimentional Ag micro Nano materials.
3. preparation method as claimed in claim 2, which is characterized in that solid FeSO4.7H2The additive amount of O is 0.15~0.35g
When be prepared the micro-nano bands of Ag, additive amount is less than 0.15g or micro-nano of random Ag is prepared in more than 0.35g when.
4. preparation method as claimed in claim 2, which is characterized in that solid (NH4)2Fe(SO4)2Additive amount be 0.15~
Ag micro-nano rings are prepared when 0.35g, it is micro-nano that random Ag is prepared when additive amount is less than 0.15g or more than 0.35g
Piece.
5. preparation method as described in claim 3 or 4, which is characterized in that micro-nano of the micro-nano bands of Ag, Ag being prepared
Size be 5~20 μm, be in multilayered structure state, if by dry thickness be 10~20nm nanometer sheet assemble；It is prepared
The micro-nano rings of Ag assembled by countless Ag nano particles.
6. a kind of thin using any one of such as Claims 1 to 5 the method acquisition two dimension Ag micro Nano materials preparation quasi- monocrystalline Ag
The method of film, which is characterized in that two-dimentional Ag micro Nano materials are distributed in absolute alcohol after forming Ag slurries, drip to silicon chip or glass
Glass on piece, to obtain being orientated consistent quasi- monocrystalline Ag films.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111515383A (en) * | 2020-04-03 | 2020-08-11 | 江苏师范大学 | Silver nano triangular protection method based on ferrous ions |
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