CN108568530A - A method of by surfactant-free microemulsion reaction methods Nano silver grain - Google Patents
A method of by surfactant-free microemulsion reaction methods Nano silver grain Download PDFInfo
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- CN108568530A CN108568530A CN201810420515.5A CN201810420515A CN108568530A CN 108568530 A CN108568530 A CN 108568530A CN 201810420515 A CN201810420515 A CN 201810420515A CN 108568530 A CN108568530 A CN 108568530A
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- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 42
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 96
- 239000008346 aqueous phase Substances 0.000 claims abstract description 38
- 239000012071 phase Substances 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 14
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 14
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000005642 Oleic acid Substances 0.000 claims description 14
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 14
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- LVGKNOAMLMIIKO-UHFFFAOYSA-N Elaidinsaeure-aethylester Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC LVGKNOAMLMIIKO-UHFFFAOYSA-N 0.000 claims description 10
- LVGKNOAMLMIIKO-QXMHVHEDSA-N ethyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC LVGKNOAMLMIIKO-QXMHVHEDSA-N 0.000 claims description 10
- 229940093471 ethyl oleate Drugs 0.000 claims description 10
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 claims description 8
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 claims description 8
- 229940073769 methyl oleate Drugs 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 229960002969 oleic acid Drugs 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 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 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract description 4
- 229910052709 silver Inorganic materials 0.000 description 14
- 239000004332 silver Substances 0.000 description 14
- 235000013339 cereals Nutrition 0.000 description 12
- 230000003287 optical effect Effects 0.000 description 8
- 230000000670 limiting effect Effects 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- -1 siloxanes Chemical class 0.000 description 2
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005323 electroforming Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- 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 application belongs to the preparation method of noble metal, and specially a kind of method by surfactant-free microemulsion reaction methods Nano silver grain, preparation process is as follows,（1）Oil phase solvent, aqueous phase solvent A, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to keep mixed liquor transparent microemulsion A, mixing speed are 150 220r/min；（2）Oil phase solvent, aqueous phase solvent B, solvent pairs are uniformly mixed under room temperature, and stirred under room temperature to making mixed liquor clarify to obtain microemulsion B, mixing speed is 150 220r/min；（3）Isometric microemulsion B is slowly dropped to from constant pressure funnel in microemulsion A under stirring, and continues stirring 12h, 50 60 drops of rate of addition/min at 25 DEG C.
Description
Technical field
The application belongs to the preparation method of noble metal, and specially one kind is by surfactant-free microemulsion reaction methods nano grain of silver
The method of son.
Background technology
Nanosecond science and technology and nano material be known as be " 21st century it is most promising science and technology and material it
One ", wherein nano silver due to diameter of particle it is small, and there is large specific surface area, surface-active point is more, catalytic activity height, fusing point are low,
The advantages that sintering character is good, while also retaining the good conductivity of metallic silver, anti-microbial property is good, bright excellent of electroforming silver color
Point so that nano-silver powder has broad application prospects in terms of heat, electricity, light, sound, magnetic and catalysis.Optical research shows Yin Na
The surface plasma body resonant vibration of rice corpuscles can cause the effects such as the strong absorption, scattering and near field enhancing of light, so as to by silver nanoparticle
Particle is applied to the preparation of optical limiting materials.Different according to the property of coating material, nano-noble metal particle can be divided into parent
Aqueous and two class of hydrophobicity, the wherein structure of the preparation of hydrophobicity noble metal nano particles and its orderly self-assembled structures are for grinding
Nano electron device processed has especially important meaning.
The liquid-phase synthesis process of nano-particle have spray-on process, hydrothermal reduction method, replacement method, solution phase chemical reduction,
Microemulsion method etc..Wherein microemulsion method synthetic method has the advantages that equipment simple, mild condition, particle monodisperse and interface characteristics good
It is widely used in the synthesis of nano-particle.Since classical microemulsion contains exhibiting high surface activating agent, using it as template system
Standby nano-material surface usually contains surfactant, needs repeatedly to wash to remove remaining surface in last handling process
Activating agent, this undoubtedly increases production process and cost.Surfactant-free microemulsion（Surfactant-free
Microemulsion, abbreviation SFME）By immiscible oil phase, water phase and solvent pairs（Water can be dissolved in but also be dissolved in the non-of oil
Conventional surface active material）It constitutes, is a kind of novel microemulsion liquid.SFME is more easy to be produced in application process because component is simple
Object recycles and post-processing, has a clear superiority compared with classical microemulsion.
The present invention is using SFME as reaction template one-step synthesis hydrophobicity silver nano-grain, and mild condition, step is simple, and
It is not necessary to separately add coating material.
The hydrophobic Nano silver grain of synthesis is transferred in siloxanes and is solidified into organosilicone film, optical Limiting experiment shows
The Nano silver grain content adulterated in silica gel piece is more, can more show higher plasmon absorption intensity and lower
Optical Limiting threshold value, the influence to optical Limiting are relatively more apparent.
Invention content
A method of by surfactant-free microemulsion reaction methods Nano silver grain, preparation process is as follows,（1）Oil phase is molten
Agent, aqueous phase solvent A, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to keep mixed liquor transparent microemulsion A, stir
It is 150-220r/min to mix speed；（2）Oil phase solvent, aqueous phase solvent B, solvent pairs are uniformly mixed under room temperature, and in room temperature
Lower stirring is to making mixed liquor clarify to obtain microemulsion B, mixing speed 150-220r/min；（3）It will be isometric under stirring
Microemulsion B be slowly dropped in microemulsion A from constant pressure funnel, and continue at 25 DEG C to stir 12h, rate of addition 50-60 drops/
min。
Preferably, the oil phase solvent is one or more of oleic acid, methyl oleate, ethyl oleate.
Preferably, the oil phase solvent is oleic acid.
Preferably, the oil phase solvent is the mixture of oleic acid, methyl oleate, ethyl oleate, the oleic acid, methyl oleate, oil
The mass ratio of acetoacetic ester is 10：3：7.
Preferably, the molar concentration rate of the compatible with water dose of B of aqueous phase solvent A can be 1:1~ 4.
Preferably, the aqueous phase solvent A is silver nitrate solution.
Preferably, the aqueous phase solvent B is hydrazine hydrate solution, and ascorbic acid solution, sodium citrate solution, sodium borohydride is molten
Liquid, one kind in citric acid solution.
Preferably, the aqueous phase solvent A is 0.1 molL-1Silver nitrate solution.
Preferably, the solvent pairs be normal propyl alcohol, isopropanol, ethyl alcohol it is one or more.
Preferably, the step（1）Middle oil phase solvent, aqueous phase solvent A, solvent pairs volume ratio are 5:3:13
Preferably, the step（2）Middle oil phase solvent, aqueous phase solvent B, solvent pairs volume ratio be 5:3:13.
Advantageous effect：The noble silver nano-particle of the application synthesis has hydrophobicity, and dispersibility is preferable, Size Distribution
It is relatively narrow；Hydrophobic Nano silver grain, which is transferred in siloxanes, is solidified into organosilicone film, and optical Limiting experiment shows to adulterate in silica gel piece
Nano silver grain it is more, higher plasmon absorption intensity and lower optical Limiting threshold value can be more shown, to light
The influence of amplitude limit is relatively more apparent.
Attached drawing and description of the drawings
Fig. 1 be silver nano-grain be dispersed in the TEM photos in chloroform, it can be seen that Argent grain is uniformly dispersed, pattern be it is spherical,
Diameter is about 10-20 nm；
Fig. 2 is the X ray diffracting spectrum of silver nano-grain, 2θTo there are five feature diffraction of metallic silver at 30-90 °
Peak, what is shown has arrived pure phase silver simple substance；
Fig. 3 silver nano-grain ultraviolet-visible spectrums, it is seen that prepared silver colloid has surface plasma resonance near 430 nm
It absorbs, peak type is sharp, illustrates that particle diameter distribution is uniform.
Specific implementation mode
Embodiment 1
A method of by surfactant-free microemulsion reaction methods Nano silver grain, preparation process is as follows,（1）By oil phase solvent,
Aqueous phase solvent A, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to keep mixed liquor transparent microemulsion A, stirring speed
Degree is 150r/min；（2）Oil phase solvent, aqueous phase solvent B, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to
Mixed liquor is set to clarify to obtain microemulsion B, mixing speed 150r/min；（3）It is under stirring that isometric microemulsion B is certainly permanent
Pressure funnel is slowly dropped in microemulsion A, and continues stirring 12h, 60 drops of rate of addition/min at 25 DEG C.
Preferably, the oil phase solvent is oleic acid.
Preferably, the aqueous phase solvent A is 0.1 molL-1Silver nitrate solution.
Preferably, the aqueous phase solvent B is 0.1-0.3 molL-1Hydrazine hydrate solution.
Preferably, the solvent pairs is isopropanol.
Preferably, the step（1）Middle oil phase solvent, aqueous phase solvent A, solvent pairs volume ratio are 5:3:13.
Preferably, the step（1）Middle oil phase solvent, aqueous phase solvent B, solvent pairs volume ratio be 5:3:13.
Embodiment 2
A method of by surfactant-free microemulsion reaction methods Nano silver grain, preparation process is as follows,（1）By oil phase solvent,
Aqueous phase solvent A, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to keep mixed liquor transparent microemulsion A, stirring speed
Degree is 220r/min；（2）Oil phase solvent, aqueous phase solvent B, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to
Mixed liquor is set to clarify to obtain microemulsion B, mixing speed 220r/min；（3）It is under stirring that isometric microemulsion B is certainly permanent
Pressure funnel is slowly dropped in microemulsion A, and continues stirring 12h, 50 drops of rate of addition/min at 25 DEG C.
Preferably, the oil phase solvent be oleic acid, methyl oleate, one or more of ethyl oleate.
Preferably, the oil phase solvent be oleic acid, ethyl oleate mixture, the oleic acid, ethyl oleate volume ratio
It is 5：1.
Preferably, the aqueous phase solvent A is 0.1 molL-1Silver nitrate solution.
Preferably, the aqueous phase solvent B is 0.4 molL-1Sodium citrate solution solution
Preferably, the solvent pairs is the mixture of isopropanol, ethyl alcohol, and the volume ratio of the isopropanol and ethyl alcohol is 1:2.
Preferably, the step（1）Middle oil phase solvent, aqueous phase solvent A, solvent pairs volume ratio are 1:1:3.
Preferably, the step（1）Middle oil phase solvent, aqueous phase solvent B, solvent pairs volume ratio be 1:1:3.
Embodiment 3
A method of by surfactant-free microemulsion reaction methods Nano silver grain, preparation process is as follows,（1）By oil phase solvent,
Aqueous phase solvent A, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to keep mixed liquor transparent microemulsion A, stirring speed
Degree is 200r/min；（2）Oil phase solvent, aqueous phase solvent B, solvent pairs are uniformly mixed under room temperature, and stir under room temperature to
Mixed liquor is set to clarify to obtain microemulsion B, mixing speed 200r/min；（3）It is under stirring that isometric microemulsion B is certainly permanent
Pressure funnel is slowly dropped in microemulsion A, and continues stirring 12h, 70 drops of rate of addition/min at 25 DEG C.
Preferably, the oil phase solvent is the mixture in oleic acid, methyl oleate, ethyl oleate, the oleic acid, oleic acid first
Volume ratio in ester, ethyl oleate is 5:4:1.
Preferably, the concentration ratio of the compatible with water dose of B of aqueous phase solvent A can be 1:1~ 4.
Preferably, the aqueous phase solvent B is hydrazine hydrate solution, ascorbic acid solution, sodium citrate solution, citric acid solution
In mixture；The concentration of the hydrazine hydrate solution, ascorbic acid solution, sodium citrate solution, citric acid solution is 0.2
mol·L-1, the volume ratio of the hydrazine hydrate solution, ascorbic acid solution, sodium citrate, citric acid solution is 1:7:1:3.
Preferably, the aqueous phase solvent A is 0.1 molL-1Silver nitrate solution.
Preferably, the solvent pairs is the mixture of normal propyl alcohol, isopropanol, ethyl alcohol, the normal propyl alcohol, isopropanol, ethyl alcohol
Volume ratio be 3:1:2.
Preferably, the step（1）Middle oil phase solvent, aqueous phase solvent A, solvent pairs volume ratio are 8:7:1.
Preferably, the step（1）Middle oil phase solvent, aqueous phase solvent B, solvent pairs volume ratio be 8:7:1.
Embodiment 4
The aqueous phase solvent B is 0.2 molL-1Ascorbic acid solution, it is other same as Example 3.
The preparation process of the application silica gel piece is as follows：130 μ L are taken to be dispersed in the Nano silver grain in chloroform small in 10 mL
In beaker, 1 g PDMS are weighed（Dimethyl silicone polymer）In upper small beaker, 100 μ L crosslinking agents are stirring evenly and then adding into, are stirred
Exclusion bubble is repeatedly vacuumized after even, temperature programming cures made silica gel piece, surveys optical Limiting property.
The mixture containing silver nano-grain prepared can be obtained silver nano-grain through centrifugation, washing, drying steps,
These are conventional steps, nor present invention point, the application do not do excessive elaboration.
Claims (10)
1. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain, which is characterized in that preparation process is as follows,
（1）Oil phase solvent, aqueous phase solvent A, solvent pairs be uniformly mixed under room temperature, and is stirred under room temperature to keeping mixed liquor transparent
Microemulsion A, mixing speed 150-220r/min；（2）Oil phase solvent, aqueous phase solvent B, solvent pairs are mixed under room temperature
It is even, and stir under room temperature to making mixed liquor clarify to obtain microemulsion B, mixing speed 150-220r/min；（3）In stirring
It is lower to be slowly dropped to isometric microemulsion B in microemulsion A from constant pressure funnel, and continue stirring 12h at 25 DEG C, speed is added dropwise
Degree is 50-60 drops/min.
2. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In the oil phase solvent is one or more of oleic acid, methyl oleate, ethyl oleate.
3. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In the mixture that, the oil phase solvent is oleic acid, methyl oleate, ethyl oleate, the oleic acid, methyl oleate, ethyl oleate
Volume ratio is 10：3：7.
4. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In the molar concentration rate of the compatible with water dose of B of aqueous phase solvent A can be 1:1~ 4.
5. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In the aqueous phase solvent A is silver nitrate solution.
6. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
It is hydrazine hydrate solution in, the aqueous phase solvent B, ascorbic acid solution, sodium citrate solution, sodium borohydride solution, citric acid is molten
One kind in liquid.
7. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In the aqueous phase solvent A is 0.1 molL-1Silver nitrate solution.
8. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In, the solvent pairs be normal propyl alcohol, isopropanol, ethyl alcohol it is one or more.
9. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In the step（1）Middle oil phase solvent, aqueous phase solvent A, solvent pairs volume ratio are 5:3:13.
10. a kind of method by surfactant-free microemulsion reaction methods Nano silver grain as described in claim 1, feature exist
In the step（2）Middle oil phase solvent, aqueous phase solvent B, solvent pairs volume ratio be 5:3:13.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761278A (en) * | 2019-02-15 | 2019-05-17 | 山东师范大学 | Using surfactant-free microemulsion as the method for templated synthesis barium chromate nano material |
| CN111364095A (en) * | 2020-03-18 | 2020-07-03 | 青岛大学 | Method for synthesizing small-size metal nanocrystalline |
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| JP2009102716A (en) * | 2007-10-25 | 2009-05-14 | Dowa Electronics Materials Co Ltd | Method for producing silver nanoparticle |
| CN102248175A (en) * | 2011-05-30 | 2011-11-23 | 东华大学 | Method for preparing homodisperse silver nanoparticles by water-in-oil type microemulsion |
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