CN106001598A - Method for synthesizing piece-shaped gold nanoparticles through hydrotalcite interlamination - Google Patents
Method for synthesizing piece-shaped gold nanoparticles through hydrotalcite interlamination Download PDFInfo
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- CN106001598A CN106001598A CN201610310958.XA CN201610310958A CN106001598A CN 106001598 A CN106001598 A CN 106001598A CN 201610310958 A CN201610310958 A CN 201610310958A CN 106001598 A CN106001598 A CN 106001598A
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- hydrotalcite
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- deionized water
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- 239000010931 gold Substances 0.000 title claims abstract description 33
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 32
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 27
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 21
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 21
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 5
- 238000000034 method Methods 0.000 title claims description 16
- 239000000463 material Substances 0.000 claims abstract description 37
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims abstract description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 14
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 36
- 239000012528 membrane Substances 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 15
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011777 magnesium Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000084 colloidal system Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 9
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 235000013877 carbamide Nutrition 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 5
- 229910052599 brucite Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 235000009566 rice Nutrition 0.000 claims description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 229940059939 kayexalate Drugs 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 240000007594 Oryza sativa Species 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 235000010344 sodium nitrate Nutrition 0.000 claims 1
- 235000011149 sulphuric acid Nutrition 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 238000001514 detection method Methods 0.000 abstract description 10
- 238000006722 reduction reaction Methods 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 229940107698 malachite green Drugs 0.000 abstract description 5
- 238000001069 Raman spectroscopy Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 abstract 1
- -1 malachite green isothiocyanate Chemical class 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 description 16
- 239000010409 thin film Substances 0.000 description 16
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 10
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 9
- 238000002835 absorbance Methods 0.000 description 8
- 229940002712 malachite green oxalate Drugs 0.000 description 7
- 239000011229 interlayer Substances 0.000 description 6
- 239000002082 metal nanoparticle Substances 0.000 description 6
- 239000000575 pesticide Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- UJOHNXQDVUADCG-UHFFFAOYSA-L aluminum;magnesium;carbonate Chemical compound [Mg+2].[Al+3].[O-]C([O-])=O UJOHNXQDVUADCG-UHFFFAOYSA-L 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000002699 waste material Substances 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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- 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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
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- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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Abstract
The invention discloses a preparation method based on hydrotalcite interlamination confinement for synthesizing a piece-shaped gold nanoparticle ultrathin film and belongs to the field of material design. According to the technical scheme of the preparation method, firstly, sodium polystyrene sulfonate and hydrotalcite are assembled alternately, and an ultrathin film material of a reaction precursor is obtained; and then the ultrathin film material is soaked in a chloroauric acid solution and a sodium borohydride solution alternately for reaction, and the piece-shaped gold nanoparticle ultrathin film which is uniform in interlamination dispersion and single in size is obtained. The piece-shaped gold nanoparticle ultrathin film prepared through the preparation method can be repeatedly applied to reduction reaction catalysis of nitrophenol and Raman detection of fishery medicine malachite green isothiocyanate and has good repeatability and stability and wide application prospects.
Description
Technical field
The invention belongs to nano material design field, equal at hydrotalcite layers reduction synthesis particularly to one
The method of even scattered lamellar gold nanoparticulate thin films.
Background technology
Metal nanoparticle (such as gold, silver, platinum etc.) is arranged because of its outermost layer single electron, and has higher
Chemism and special optics, electricity and catalytic property, thus be widely used in sensing, detection,
Catalysis and biomedicine field.But at present research to metal nanoparticle, mostly it is confined to solution state,
Thus limit its range of application, and this nanoparticle cannot be reused, metallic catalyst is difficult to have
Effect separates and causes the waste of substantial amounts of Precious Metals Resources.In order to constantly expand the application of metal nanoparticle,
Some researchs are fixed in substrate based on by the metal nanoparticle of synthesis, but owing to its colloid is prone to assemble, often
Method (such as nanolithographic, electrochemical reduction, vacuum evaporation etc.) complex process cause in the thin film obtained
Pattern and the state of metal nanoparticle are difficult to control to, so that the stability of system and repeatability are poor.
Therefore a kind of effective in-situ reducing preparation gold in substrate is obtained by the selection of material and the improvement of method
The method belonging to nanoparticulate thin films is very important.A kind of effective approach is first to construct confinement in substrate
Space, then by in-situ reducing in confinement space, thus obtains efficient metal nanoparticle, goes forward side by side one
Step explores its application.
Summary of the invention
It is an object of the invention to provide a kind of based on in-situ reducing gold in brucite (LDHs) interlayer confinement space
Nanoparticle, thus obtain chemically active golden nanometer particle Multifunctional ultrathin film homodisperse, high, and will
It is applied in the catalysis of chemical reaction and the detection of pesticide.
The technical scheme is that first to be furnished with kayexalate (PSS) and the delamination of sodium chloride
LDHs LBL self-assembly, on the component film obtained, utilizes the confinement space in-situ reducing chlorine that LDHs provides
Auric acid obtains thin-film material high dispersive, based on golden nanometer particle.The ultrathin membrane material that the present invention prepares,
Due to the confinement effect of LDHs, the horizontal particle diameter of golden nanometer particle of interlayer is at 13nm, and its thickness is 7.6nm,
It it is a kind of class flaky material.Pattern and character that this material is special are expected in catalysis, surface enhanced raman spectroscopy inspection
Survey aspect possesses better performance.
A kind of method of hydrotalcite layers synthesizing flaky golden nanometer particle, its concrete preparation process is as follows:
A. in 100mL Methanamide, the nitrate anion Intercalated 0.06-0.15g of preparation is added, at N2
Stirring 36-60h under protection, 2000 revs/min after centrifugal 5-10 minute, the brucite taking upper strata clear is received
Rice sheet colloid solution;
B. weigh kayexalate powder 0.05-0.2g in 100mL deionized water, be subsequently adding chlorination
Sodium, sodium chloride concentration is 1-2mol/L, standby after ultrasonic dissolution;
C. will the hydrotalcite nano piece colloid solution in a step of the quartz substrate after hydrophilicity-imparting treatment immerse
10-20 minute, with deionized water rinsing and use N after being drawn off2Dry up, piezoid is placed into b step and joins
Immersing 10-20 minute in the polystyrolsulfon acid solution of the sodium chloride-containing of system, taking-up is rinsed well, continuously repeats this
Step 2-10 time, obtains the ultrathin membrane material with confinement space;
D. compound concentration is the sodium borohydride solution of 50-100mmol/L;Compound concentration is 1-10mmol/L's
Chlorauric acid solution also adjusts pH value to be 8-9 with NaOH;By the ultrathin membrane material of step c first in chlorauric acid solution
Soak 5-10 minute, take out to put in sodium borohydride solution after cleaning and fully react 5-10 minute, repeat this step
1-5 time, obtain the ultrathin membrane material of lamellar gold nanoparticle.
The preparation method of described nitrate anion Intercalated: magnesium nitrate, aluminum nitrate and carbamide are dissolved in
Being configured to mixing salt solution in deionized water, wherein magnesium is (2-3) with the mol ratio of aluminum: 1, and magnesium with the total concentration of aluminum is
2-4mmol/L, the concentration of carbamide is 10-30mmol/L, and it is anti-that ultrasonic and stirring pours high pressure into after making its mix homogeneously
Answering to react at 90-120 DEG C 20-30 hour in still and take out, deionized water wash, 60 DEG C of drying obtain carbonate magnesium
Aluminum hydrotalcite;With the NaNO of 0.4-0.6mol after 0.2-0.5g carbonate Intercalated is ground3And 1-3
The dense HNO of mmol3Mixing adds in the deionized water that 200-400mL is boiled, N236-48h is stirred under protection,
Centrifugal, dry, after grinding, obtain the magnesium aluminum-hydrotalcite of nitrate anion.
The method of hydrophilizing of described quartz substrate is: be first the dense of 7:3 by volume ratio by quartz substrate
H2SO4And H2O2Mixed solution soak 20-60 minute, and with deionized water fully clean ultrasonic after, be dried
In case using.
Ultrathin membrane material by the lamellar gold nanoparticle of above-mentioned preparation:
(1) by the test of UV-Vis uv-vis spectra, determine and obtain when different gold chloride reaction densities
To the amount of golden nanometer particle and go out peak position, thus find most suitable reaction in-situ concentration;
(2) test of UV-Vis uv-vis spectra is carried out, to determine increasing along with reaction times, thin film
The amount of middle golden nanometer particle constantly rises;
(3) the film surface form containing golden nanometer particle obtained is carried out transmission electron microscope and atomic force microscopy
The sign of mirror, to check the particle diameter of the golden nanometer particle of fabricated in situ, dispersion and thickness;
(4) nanostructured thin film before and after reacting with gold chloride carries out the test of little angle XRD, to determine former
The situation of change of interlamellar spacing in thin-film material in the reduction process of position, and with this, thickness of the golden nanometer particle obtained is described
Degree and interlayer distribution situation;
(5) ultrathin membrane based on golden nanometer particle obtained is carried out explorative research,
It is an advantage of the current invention that: the present invention provides a kind of in-situ reducing lamellar in brucite confinement interlayer environment
The preparation method of golden nanometer particle, and can be applicable to catalysis and in the detection of pesticide.Brucite is lamellar gold
Nanoparticle provides the environment of a kind of reaction in-situ, effectively achieves interlayer homodisperse lamellar gold nanometer
The preparation of particle.The ultrathin membrane material based on golden nanometer particle of preparation has height-oriented property, can repeatedly answer
Catalyst for reduction reaction and the detection for pesticide molecule.
Accompanying drawing explanation
Fig. 1 is the ultra-thin of the lamellar gold nanoparticle that in the embodiment of the present invention 1, different gold chloride concentration reduction obtain
The uv absorption explanatory diagram of membrane material.Wherein abscissa is the gold chloride concentration for reaction, unit: mM
Every liter;Left side vertical coordinate is absworption peak position, unit: nanometer;Right side vertical coordinate is absorbance.Initial point in figure
Represent and be respectively 1 in gold chloride concentration, when 2.5,5,7.5,10 mMs every liter, react the lamellar Jenner obtained
The absworption peak position of the ultrathin membrane material of rice corpuscles, diamond indicia represents the absorbance of this thin film.This figure explanation
The amount of the golden nanometer particle that different gold chloride concentration-responses obtain and the difference of particle diameter.
Fig. 2 is reacting not in the gold chloride of 7.5 mMs every liter and sodium borohydride of obtaining of the embodiment of the present invention 1
The uv absorption figure of the ultrathin membrane material of the lamellar gold nanoparticle obtained with number of times.Wherein abscissa is wavelength,
Unit: nanometer, vertical coordinate is absorbance.The explanation of this figure is along with the increase of reaction times, the Jenner that reaction obtains
The amount of rice corpuscles is continuously increased.
Fig. 3 is the high power transmission electron microscope picture of the ultrathin membrane material of the lamellar gold nanoparticle that reaction in-situ obtains, its
Middle scale is 50 nanometers.
Fig. 4 A is the atomic force microscope figure of the ultrathin membrane material of the lamellar gold nanoparticle that reaction in-situ obtains, figure
Sheet overall range is 2 microns, and in figure, small white spots represents homodisperse golden nanometer particle.Fig. 4 B is atomic force
Microscope height map, by the Elevation Analysis of nanoparticle in figure A, characterizing the gold nano that reaction obtains
The height of particle.
Fig. 5 is that (PSS/LDH) ultrathin membrane material of the assembling that obtains of the embodiment of the present invention 1 10 times is in gold chloride
XRD analysis figure before and after reaction, wherein abscissa is angle, unit: degree, vertical coordinate is relative intensity.Figure
Middle a, b are respectively after reacting and the XRD analysis of original thin film.
Fig. 6 is that the ultrathin membrane material of the lamellar gold nanoparticle of the fabricated in situ that the embodiment of the present invention 1 obtains is being urged
Change the application in reaction.When the right figure of left figure is respectively the ultrathin membrane material not adding and adding lamellar gold nanoparticle
The mixed solution of paranitrophenol and the sodium borohydride uv absorption variation diagram when the differential responses time.This figure is said
This ultrathin membrane material bright may be used for the reduction catalysts reaction of paranitrophenol.In figure, abscissa is wavelength, unit:
Nanometer;Vertical coordinate is absorbance.
Fig. 7 is that the ultrathin membrane material of the lamellar gold nanoparticle of the fabricated in situ that the embodiment of the present invention 1 obtains is in agriculture
Application in medicine malachite green oxalate, in figure, a, b, c, d, e are respectively concentration is 10-6, 10-7, 10-8, 10-9,
10-10The Raman spectrum detection of the malachite green oxalate of mole every liter.In figure, abscissa is Raman shift, unit: every li
Rice;Vertical coordinate is relative intensity.The ultrathin membrane material of the lamellar gold nanoparticle that this figure obtains can be applied
In the detection to pesticide molecule.
Detailed description of the invention
Embodiment 1
The preparation of step A. hydrotalcite nano piece colloid solution: nitrate anion Intercalated 0.1g is added
In 100ml Methanamide, at N2Stir 48h under protection, be then centrifuged for, discard precipitate, obtain clear
Hydrotalcite nano piece colloid solution;
The preparation of step B.PSS solution: compound concentration is the PSS solution 50ml of 1g/L, wherein containing 2mol/L
Sodium chloride;
Quartz substrate after hydrophilicity-imparting treatment is immersed in the hydrotalcite nano piece glue of gained in step A by step C.
In liquid solution 10 minutes, with deionized water rinsing after being drawn off, N2Place into prepared by step B after drying up
Soaking 10 minutes in PSS and sodium chloride blend solution, taking-up is rinsed well;
The fabricated in situ of step D. golden nanometer particle: configuration concentration be 100mmol/L sodium borohydride solution and
Concentration is the chlorauric acid solution of 7.5mmol/L and adjusts pH value to be 9 with NaOH.By what step C obtained
(PSS/LDH) ultrathin membrane soaks 5 minutes in chlorauric acid solution, takes out and puts into newly configured sodium borohydride after cleaning
Solution fully reacts 5 minutes, repeats this step 5 time,
Gold nanometer particle grain size in the ultrathin membrane material of the lamellar gold nanoparticle that step D obtains is 13nm.
The preparation method of described nitrate anion Intercalated: weigh 2.10g Mg (NO3)2·6H2O、1.50g
Al(NO3)3·9H2O (Mg/Al=2) and 2.90g carbamide are dissolved in 300ml deionized water, and ultrasonic and stirring makes
Pour into after its mix homogeneously in autoclave and take out in 110 DEG C of reaction 24h, deionized water wash, dry
To carbonate Intercalated;With 1.0mol's after 0.6g carbonate Intercalated is ground
NaNO3HNO dense with 3.0mmol3Mixing adds in the deionized water that 600ml is boiled, at N2The lower stirring of protection
48h, spends CO2Deionized water centrifuge washing 3 times, dry, obtain after grinding.
The method of hydrophilizing of described quartz substrate is: be first the dense of 7:3 by volume ratio by quartz substrate
H2SO4And H2O2Mixed solution soak 30 minutes, and with deionized water fully clean ultrasonic after, be dried in case
Use.
The above-mentioned application based on lamellar gold nanoparticle ultrathin membrane prepared: (1) reduction reaction is catalyzed: join
Standby sodium borohydride and paranitrophenol mixed solution, the ultrathin membrane material of the lamellar gold nanoparticle that step D is obtained
Material is statically placed in this mixed solution, the conversion of paranitrophenol when investigating the differential responses time.(2) to pesticide
Detection: the malachite green oxalate of preparation variable concentrations, adds variable concentrations by the ultrathin membrane material of lamellar gold nanoparticle
Malachite green solution, by the malachite green oxalate that Raman spectrum test is adsorbed.
The spectrophotometry figure of Fig. 1 illustrates the different gold chloride reaction density golden nanometer particle to synthesis
Impact, when wherein concentration is 7.5 mMs every liter, golden nanometer particle has higher absorbance, and absorption value exists
520 ran, illustrate that it has preferable dispersion and synthetic quantity.Fig. 2 is suction during the different number of times of reaction
Luminosity characterizes, and the figure shows increasing along with reaction times, the golden nanometer particle content obtained in ultrathin membrane material
Increase.The golden nanometer particle that the high power transmission electron microscope of Fig. 3 obtains is dispersed, and particle diameter is left in 13 nanometers
Right.The atomic force microscope of Fig. 4 illustrates that the golden nanometer particle of synthesis is dispersed, and it is at the height of interlayer
Degree is 7.53 nanometers, in the form of sheets structure.The XRD figure of Fig. 5 illustrates in this thin film in-situ reactive synthesis gold nano
The change of interlamellar spacing before and after particle, after the skew explanation reaction of its angle, interlamellar spacing increases from 5.96 original nanometers
Greatly 7.81 nanometers.Fig. 6 shows that sodium borohydride and paranitrophenol mix when with or without Au nanoparticle catalyst
Close solution absorbance in time and be worth change.When Fig. 6 A explanation does not has golden nanometer particle thin film, this reaction is not sent out
Raw, absorbance is not changed in;And paranitrophenol is received 400 after Fig. 6 B explanation adds golden nanometer particle thin film
At meter absorbance constantly decline, illustrate the catalytic performance that golden nanometer particle thin film is higher.Fig. 7 gives
Drawing of golden nanometer particle ultrathin membrane material aperture after passeris montani saturati malachite green molecule is soaked in the malachite green solution of variable concentrations
Graceful vibration detection, illustrates that it can detect 10-10Mole every liter, to its most extensively application provide can
Energy.
Embodiment 2
The preparation of step A. hydrotalcite nano piece colloid solution: nitrate anion intercalation magnalium neatly 0.08g will be obtained and add
Enter in 100ml Methanamide, at N2Stir 48h under protection, be then centrifuged for, discard precipitate, obtain clarification thoroughly
Bright hydrotalcite nano piece colloid solution;
The preparation of step B.PSS solution: compound concentration is the PSS solution 50ml of 1.5g/L, wherein containing 1mol/L
Sodium chloride;
Quartz substrate after hydrophilicity-imparting treatment is immersed in the hydrotalcite nano piece glue of gained in step A by step C.
In liquid solution 15 minutes, with deionized water rinsing after being drawn off, N2Place into prepared by step B after drying up
Soaking 15 minutes in PSS and sodium chloride blend solution, taking-up is rinsed well;
The fabricated in situ of step D. golden nanometer particle: configuration concentration is the sodium borohydride solution of 50mmol/L and dense
Degree is the chlorauric acid solution of 5mmol/L and adjusts pH value to be 8 with NaOH.(PSS/LDH) that will obtain in step C
Ultrathin membrane soaks 8 minutes in chlorauric acid solution, takes out to put in newly configured sodium borohydride solution after cleaning and fills
Divide reaction 8 minutes, repeat this step 5 time,
The gold nanometer particle grain size in ultrathin membrane described in step D is 13-15nm.
The preparation method of described nitrate anion Intercalated: weigh 1.10g Mg (NO3)2·6H2O、0.80g
Al(NO3)3·9H2O (Mg/Al=2) and 1.50g carbamide are dissolved in 160ml deionized water, and ultrasonic and stirring makes
Pour into after its mix homogeneously in autoclave and take out in 100 DEG C of reaction 28h, deionized water wash, dry
To carbonate Intercalated;With 0.8mol's after 0.5g carbonate Intercalated is ground
NaNO3HNO dense with 2.5mmol3Mixing adds in the deionized water that 500ml is boiled, at N2The lower stirring of protection
48h, spends CO2Deionized water centrifuge washing 3 times, dry, obtain after grinding.
The method of hydrophilizing of described quartz substrate is: be first the dense of 7:3 by volume ratio by quartz substrate
H2SO4And H2O2Mixed solution soak 30 minutes, and with deionized water fully clean ultrasonic after, be dried in case
Use.
The above-mentioned application based on lamellar gold nanoparticle ultrathin membrane prepared: (1) catalysis paranitrophenol is also
Former reaction: with sodium borohydride and paranitrophenol mixed solution, golden nanometer particle step D obtained is ultra-thin
Film is statically placed in this mixed solution, the reduction situation of paranitrophenol when investigating the differential responses time.(2) to agriculture
The detection of medicine: the malachite green oxalate of preparation variable concentrations, by molten for golden nanometer particle ultrathin membrane variable concentrations malachite green oxalate
Liquid, by the malachite green oxalate that Raman spectrum test is adsorbed.
Through characterizing: the above-mentioned ultrathin membrane material obtaining lamellar gold nanoparticle have employed and closes in situ in hydrotalcite layers
The method become, is uniformly dispersed, lamellar gold nanoparticle that size is single.This thin-film material may be used for
The catalysis of the reduction reaction of paranitrophenol, has effect significantly.It addition, this thin-film material can be with adsorption hole
Passeris montani saturati malachite green pesticide molecule, and effectively detected by Raman reinforced effects, there is application widely.
Claims (3)
1. the method for a hydrotalcite layers synthesizing flaky golden nanometer particle, it is characterised in that it specifically prepares step
Rapid as follows:
A. in 100mL Methanamide, the nitrate anion Intercalated 0.06-0.15g of preparation is added, at N2
Stirring 36-60h under protection, 2000 revs/min after centrifugal 5-10 minute, the brucite taking upper strata clear is received
Rice sheet colloid solution;
B. weigh kayexalate powder 0.05-0.2g in 100mL deionized water, be subsequently adding chlorination
Sodium, sodium chloride concentration is 1-2mol/L, standby after ultrasonic dissolution;
C. will the hydrotalcite nano piece colloid solution in a step of the quartz substrate after hydrophilicity-imparting treatment immerse
10-20 minute, with deionized water rinsing and use N after being drawn off2Dry up, piezoid is placed into b step and joins
Immersing 10-20 minute in the polystyrolsulfon acid solution of the sodium chloride-containing of system, taking-up is rinsed well, continuously repeats this
Step 2-10 time, obtains the ultrathin membrane material with confinement space;
D. compound concentration is the sodium borohydride solution of 50-100mmol/L;Compound concentration is 1-10mmol/L's
Chlorauric acid solution also adjusts pH value to be 8-9 with NaOH;By the ultrathin membrane material of step c first in chlorauric acid solution
Soak 5-10 minute, take out to put in sodium borohydride solution after cleaning and fully react 5-10 minute, repeat this step
1-5 time, obtain the ultrathin membrane material of lamellar gold nanoparticle.
Method the most according to claim 1, it is characterised in that described nitrate anion Intercalated
Preparation method: magnesium nitrate, aluminum nitrate and carbamide are dissolved in deionized water and are configured to mixing salt solution, its
Middle magnesium is (2-3) with the mol ratio of aluminum: 1, and magnesium is 2-4mmol/L with the total concentration of aluminum, and the concentration of carbamide is 10-30
Mmol/L, ultrasonic and stirring is poured into after making its mix homogeneously in autoclave and is reacted 20-30 at 90-120 DEG C
Hour take out, deionized water wash, 60 DEG C of drying obtain carbonate magnesium aluminum-hydrotalcite;0.2-0.5g carbonate is inserted
After layer magnesium aluminum-hydrotalcite grinds, HNO3 dense with NaNO3 and 1-3mmol of 0.4-0.6mol mixes addition
In the deionized water that 200-400mL is boiled, under N2 protection, stir 36-48h, centrifugal, dry, obtain after grinding
The magnesium aluminum-hydrotalcite of nitrate anion.
Method the most according to claim 1, it is characterised in that the hydrophilicity-imparting treatment of described quartz substrate
Method is: first with the mixed solution of dense H2SO4 and H2O2 that volume ratio is 7:3, quartz substrate is soaked 20-60
Minute, and with deionized water fully clean ultrasonic after, be dried in case use.
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