CN104259482A - Macro preparation method for monodisperse silver nanosheets - Google Patents

Macro preparation method for monodisperse silver nanosheets Download PDF

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CN104259482A
CN104259482A CN201410584162.4A CN201410584162A CN104259482A CN 104259482 A CN104259482 A CN 104259482A CN 201410584162 A CN201410584162 A CN 201410584162A CN 104259482 A CN104259482 A CN 104259482A
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nano silver
silver piece
mol ratio
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CN104259482B (en
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陈代荣
赵新富
焦秀玲
陈波
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Shandong University
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Shandong University
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Abstract

The invention relates to a macro preparation method for monodisperse silver nanosheets. The preparation method comprises the steps: (1) adding PVP and citric acid into silver nanosheet seed crystal suspending liquid under a water bath condition to form uniform solution; (2) carrying out reaction between salt of PVP, NH4SCN and the like, which can form insoluble substance with silver, and AgNO3 aqueous solution for preparation of AgCNS insoluble substance suspending liquid; (3) adding the suspending liquid prepared in the step (2) or salt of NH4SCN and the like which can form insoluble substance with silver in the solution prepared in the step (1), then adding hydrazine hydrate for reaction; adding AgNO3 for reaction over again; conducting centrifugal washing on the solid product to obtain the monodisperse silver nanosheets. The method is easy to control technological conditions, and suitable for mass production; the silver nanosheets yield reaches to 99.0%; the obtained silver nanosheets are high in purity, and controllable in size, and can be used for aspects of optical sensors, optical lens technology, biology labels, conductive silver paste, and the like.

Description

The preparation in macroscopic quantity method of single dispersing Nano silver piece
Technical field
The present invention relates to the preparation in macroscopic quantity method of single dispersing Nano silver piece, belong to field of inorganic chemical engineering.
Background technology
Argent stable in properties, matter are soft, ductility good, heat conduction and conductance is high, acid-alkali-corrosive-resisting etc., and in noble metal relative low price, be widely used in the fields such as photosensitive material, contact material, ornament materials, slurry, in industry and daily life, occupy very important status.The silver of nanoscale has diverse special nature, such as small-size effect with block materials, quantum effect etc.; The character of the Nano Silver of different-grain diameter and pattern is also not quite similar, current people have prepared the one dimension of various sizes and pattern, two-dimentional silver nano material, wherein two-dimensional nano ag material is because specific area is comparatively large, surface energy is lower, is the main raw material(s) of effective catalyst, optics, electronic devices and components and biological detection etc.; In two-dimensional nano ag material, the absorption spectrum of Nano silver piece can cover whole visible region and near-infrared region with the sharp keen degree change of aspect ratio and wedge angle, thus has good application prospect in fields such as chemistry and bio-sensings.
The optical property of Nano silver piece and its design feature closely related, the method therefore designing and research and develop the preparation length of side and the controlled Nano silver piece of thickness is particularly important.The preparation method of Nano silver piece mainly contains photochemical reduction, polyol process, reversed micelle method, electrochemical process and hydro-thermal method etc.Such as, the silver-colored crystal seed such as Mirkin, silver nitrate (AgNO 3) as presoma, irradiated by 150w Halogen lamp LED, and regulate the pH value of reaction solution, prepare the silver-colored triangular plate of the different length of side (see Angew.Chem.Int.Ed.2007,46,2036), although Nano silver piece purity prepared by photochemical reduction is high, but need to irradiate with the light of CF in course of reaction, the change of irradiating light frequency is relied on to regulate Nano silver piece size, the method is higher to equipment requirement, and cost is higher, is difficult to use in the preparation in macroscopic quantity of Nano silver piece; Xia etc. are coating material and reducing agent with polyvinylpyrrolidone (PVP), to have prepared silver-colored triangular plate (see Adv.Mater.2003,15,695) under 60 DEG C of conditions; Zhang etc. also utilize PVP as reducing agent, prepared under 60-100 DEG C of condition monodispersed Nano silver piece (see: CN1935422A); The spent glycols such as Ding and dimethyl formamide are as mixed solvent, adjuvant is made by introducing halogen-containing slaine, under boiling reflux condition obtained single dispersing Nano silver piece (see: CN102632246A), polyol process is by regulating and controlling the reproducibility of alcohols weak reductant to the adjustment of temperature, high to temperature requirement, and the nanometer sheet purity of preparation is low, is unfavorable for preparation in macroscopic quantity; Yan etc. are with AgNO 3with sodium borohydride (NaBH 4) be raw material, at the methyl methacrylate (C of different carboxylic acids 5h 8o 2) prepared in reversed micelle solution different crimpness Nano silver piece (see: CN101811193A); Li etc. prepare Nano silver piece array by the copper-Yin galvanic cell of assembling steaming on the electro-conductive glass after gold, this seminar is the Nano silver piece package assembly array (see CN102560581A, CN103820826A) of obtained morphology controllable in silver electrolyte also.Reversed micelle method to raw material require higher, introduce macromolecular material, be difficult to remove, and electrochemical process to experimental facilities require higher, these two kinds of methods all in various degree add cost, improve the difficulty of preparation in macroscopic quantity; Hydro-thermal method prepares Nano silver piece at present to apply maximum methods, as with silver-colored ammonia ([Ag (NH 3) 2] OH) solution is presoma, Sensor Chip CM 5 is reducing agent or utilize silver mirror reaction, with glucose (C 6h 12o 6) prepare Nano silver piece (see CN103350236A, CN103521777A) for reducing agent; Gao etc., by introducing crystal seed, adopt containing acetonitrile (C 2h 3n) hydrothermal system prepared the Nano silver piece of different size and thickness (see: Nanoscale 2014,6,4513), also by introduce crystal seed, with natrium citricum (C 6h 5na 3o 7) make auxiliary agent, hydro-thermal reaction prepares Nano silver piece (see CN1958197A, IE20100205A1), and the method that more hydro-thermal prepares silver-colored triangular plate is all with oxyacid silver for presoma, at C 6h 5na 3o 7under existence, with NaBH 4for (see CN101947055A, CN103264166A, CN103586483A) prepared by reducing agent, or on this basis, then introduce hydrogen peroxide (H 2o 2) prepare Nano silver piece (see: US20080295646A1), also have with AgNO 3for presoma, with L-ascorbic acid (C 6h 8o 6) for reducing agent prepare the controlled Nano silver piece self assembly ping-pong ball SERS substrate of thickness (see: WO2014058904A1); Although hydro-thermal method can prepare the higher Nano silver piece of purity, the yield of Nano silver piece is mostly very low, is unfavorable for preparation in macroscopic quantity.
Hydro-thermal method is method most widely used in suitability for industrialized production, and people utilize hydro-thermal method by having prepared the nanometer sheet of different size and thickness to the adjustment of different material.Particularly crystal seed method to prepare in noble metal nano-plate application at most, is formed and being separated of crystal growth, realize the control synthesis of nanometer sheet because crystal seed method can realize nucleus.But the product that Nano silver piece grows as a kind of dynamics Controlling, in order to be beneficial to the growth of nanometer sheet, avoids the generation of secondary nucleation, all needs the silver ion (Ag in system when preparing Nano silver piece +) concentration controls at reduced levels, so when preparing the length of side and being greater than the Nano silver piece of 1um, need, by the growth of the nanometer sheet that repeatedly circulated, to be unfavorable for preparation in macroscopic quantity.According to LaMer law, we can carry out reaction speed, so people are by utilizing complex silver ammino solution as presoma or adopt additional covering as citric acid, acetonitrile etc. and Ag by controlling reaction machine unit +coordination reduces Ag free in solution +concentration, reaches the object of controlled synthesis.Ag free in solution +the reduction of concentration, can prevent the generation of secondary nucleation.But the complex of this silver is still lower for the regulation and control degree of silver ion free in solution, so forming deposited salt by additional anion and silver nitrate drops to minimum by the concentration of silver ions in solution, namely by reactants dissolved degree controlling mechanism preparation in macroscopic quantity single dispersing Nano silver piece: by introducing the difficulty soluble salt of silver, as isothiocyanic acid silver (AgCNS), silver chlorate (AgCl), silver bromide (AgBr), silver iodide (AgI), silver carbonate (Ag 2cO 3), sulfurous silver cyanate (Ag 2sO 3), silver oxalate (Ag 2c 2o 4) or additional anion, as isothiocyanic acid radical ion (CNS -), chlorion (Cl -), bromide ion (Br -), iodide ion (I -), carbanion (CO 3 2-), sulfite ion (SO 3 2-), oxalate denominationby (C 2o 4 2-) control Ag free in reaction system +concentration and control reaction rate, thus realize the dynamics Controlling of the Nano silver piece growth to certain length of side and thickness, anion in system can reuse, under nanometer sheet crystal seed existence condition, using PVP as dispersant, citric acid as surfactant, by adding a large amount of AgNO in reaction system 3realize the preparation in macroscopic quantity of Nano silver piece.The single dispersing Nano silver piece concentration that this method obtains can reach 5.85g/L, it is 70 times of the maximum concentration of report at present, and the method completes the process of the different size Nano silver piece of preparation in macroscopic quantity by one-step method, avoids the inconvenience being cycled to repeat growing nano sheet and bringing; Preparation process completes at ambient temperature, and aqueous systems cost is low, and process conditions are easily controlled, and is applicable to the preparation in macroscopic quantity of Nano silver piece, is suitable for Nano silver piece large-scale production.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of can the method for the at room temperature single dispersing Nano silver piece that preparation in macroscopic quantity size is controlled, obtained Nano silver piece purity is high, and preparation process mild condition, time are short, are suitable for the large-scale production of Nano silver piece.
Technical scheme of the present invention is as follows:
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) under 20-40 DEG C of water bath condition, be add polyvinylpyrrolidone (PVP) and citric acid (C in the Nano silver piece crystal seed suspension of 9-10mg/L to concentration 6h 8o 7) stir, form homogeneous mixed solution, Nano silver piece crystal seed: PVP:C 6h 8o 7mol ratio be (0.03-0.1): (15-50): (3-15);
(2) by PVP and NH 4sCN or NaCl or NaBr or NaI or Na 2cO 3or Na 2sO 3or Na 2c 2o 4be added to the water and stir, the mol ratio of PVP and water is 1:(50-500), NH 4the mol ratio of SCN or NaCl or NaBr or NaI and water is 1:(200-350), Na 2cO 3or Na 2sO 3or Na 2c 2o 4be 1:(400-700 with the mol ratio of water);
Then, under 20-45 DEG C of water bath condition, add with the speed of 0.1-5mL/min the AgNO that concentration is 10-25g/L 3the aqueous solution; AgNO 3with NH 4the mol ratio of SCN or NaCl or NaBr or NaI is 1:(0.8-1.5), AgNO 3with Na 2cO 3or Na 2sO 3or Na 2c 2o 4mol ratio be 1:(0.4-0.75); Continue reaction 0.5-3h after reinforced, by solid product with the speed centrifugation of 2000-8000r/min, and wash solid product with water 1 ~ 4 time, then in atmosphere in 40-90 DEG C of oven dry, obtain AgCNS, AgCl, AgBr, AgI, Ag 2cO 3, Ag 2sO 3or Ag 2c 2o 4crystal grain;
By AgCNS, AgCl, AgBr, AgI, Ag of obtaining 2cO 3, Ag 2sO 3or Ag 2c 2o 4grain dispersion, in water, is mixed with the suspension that concentration is 30-50wt%, stand-by;
(3) AgCNS, AgCl, AgBr, AgI, Ag that step (2) is obtained is added in the mixed solution obtained to step (1) 2cO 3, Ag 2sO 3or Ag 2c 2o 4suspension; Or in the mixed solution that step (1) obtains, add NH 4sCN, NaCl, NaBr, NaI, Na 2cO 3, Na 2sO 3or Na 2c 2o 4;
Then reducing agent hydrazine hydrate (N is added 2h 4h 2o), after reaction 2-20min, then the AgNO that concentration is 5-20g/L is added 3the aqueous solution, reaction 10-60min, by the solid product centrifuge washing obtained, obtains single dispersing Nano silver piece;
In reaction system, described AgNO 3: AgCNS or AgCl or AgBr or AgI:N 2h 4h 2the mol ratio of O is (8-20): (0.5-2500): (15-50), described AgNO 3: Ag 2cO 3or Ag 2sO 3or Ag 2c 2o 4: N 2h 4h 2the mol ratio of O is (8-20): (0.25-1250): (15-50), described AgNO 3: NH 4sCN or NaCl or NaBr or NaI:N 2h 4h 2the mol ratio of O is (8-20): (0.5-2500): (15-50), described AgNO 3: Na 2cO 3or Na 2sO 3or Na 2c 2o 4: N 2h 4h 2the mol ratio of O is (8-20): (0.25-1250): (15-50).
According to the present invention, preferably, Nano silver piece crystal seed: PVP:C in step (1) 6h 8o 7mol ratio be (0.035-0.1): (15-45): (4-14).
According to the present invention, preferably, the mol ratio of the PVP described in step (2) and water is 1:(60-400), NH 4the mol ratio of SCN or NaCl or NaBr or NaI and water is 1:(250-300); Na 2cO 3or Na 2sO 3or Na 2c 2o 4be 1:(500-600 with the mol ratio of water);
Preferably, AgNO 3the concentration of the aqueous solution is 15-20g/L, and adding speed is 0.2-4mL/min; Described AgCNS, AgCl, AgBr, AgI, Ag 2cO 3, Ag 2sO 3or Ag 2c 2o 4the concentration of suspension is 40-50wt%.
According to the present invention, preferably, the AgNO described in step (3) 3: AgCNS or AgCl or AgBr or AgI:N 2h 4h 2the mol ratio of O is (10-20): (0.5-2000): (15-45); AgNO 3: Ag 2cO 3or Ag 2sO 3or Ag 2c 2o 4: N 2h 4h 2the mol ratio of O is (10-20): (0.25-1000): (15-45); AgNO 3: NH 4sCN or NaCl or NaBr or NaI:N 2h 4h 2the mol ratio of O is (10-20): (0.5-2000): (15-45); AgNO 3: Na 2cO 3or Na 2sO 3or Na 2c 2o 4: N 2h 4h 2the mol ratio of O is (10-20): (0.25-1000): (15-45).
According to the present invention, the Nano silver piece crystal seed suspension described in step (1) can prepare by prior art (can be see: Nanoscale 2014,6,4513);
Preferably, prepare as follows:
Under room temperature, in 200mL water, add the C that 10-15mL concentration is 0.07-0.08mol/L 6h 5na 3o 7solution, 195-210 μ L concentration is the AgNO of 0.1mol/L 3solution and 470-485 μ L concentration are the H of 30wt% 2o 2solution, stirs; Then the concentration adding 1.0-1.5mL brand-new in solution is fast the NaBH of 0.1mol/L 4solution, vigorous stirring, until solution becomes blueness, then by reacted solution left standstill 20-30h, obtains Nano silver piece crystal seed suspension.The obtained Nano silver piece crystal seed length of side 20 ± 5nm, thickness are 5 ± 2nm.
The single dispersing Nano silver piece length of side that the present invention obtains is 130-500nm, and thickness is 10-32nm.
The present invention by reactants dissolved degree controlling mechanism preparation in macroscopic quantity single dispersing Nano silver piece, that is: by introduce silver difficulty soluble salt, as AgCNS, AgCl, AgBr, AgI, Ag 2cO 3, Ag 2sO 3or Ag 2c 2o 4suspension or NH 4sCN, NaCl, NaBr, NaI, Na 2cO 3, Na 2sO 3or Na 2c 2o 4control Ag free in reaction system +concentration and control reaction rate, thus the dynamics Controlling realizing the Nano silver piece growth to certain length of side and thickness, the CNS in system -, Cl -, Br -, I -, CO 3 2-, SO 3 2-or C 2o 4 2-can reuse, by adding AgNO in a large number in reaction system 3realize the preparation in macroscopic quantity of Nano silver piece, and by regulating CNS in solution -, Cl -, Br -, I -, CO 3 2-, SO 3 2-or C 2o 4 2-amount regulate the length of side and the thickness of Nano silver piece, realize the controlled synthesis of Nano silver piece size.The single dispersing Nano silver piece concentration that the inventive method obtains can reach 5.85g/L, it is 70 times of the maximum concentration of report at present, and the method completes the process of the different size Nano silver piece of preparation in macroscopic quantity by one-step method, avoids the inconvenience being cycled to repeat growing nano sheet and bringing; Preparation process completes at ambient temperature, and aqueous systems cost is low, and process conditions are easily controlled, and is applicable to the preparation in macroscopic quantity of Nano silver piece, is suitable for Nano silver piece large-scale production.
Characteristics and advantages of the present invention is:
1, first the present invention obtains Nano silver piece as crystal seed, in seeded growth process, by adding AgCNS, AgCl, AgBr, AgI, Ag in system under aqueous systems 2cO 3, Ag 2sO 3or Ag 2c 2o 4suspension or NH 4sCN, NaCl, NaBr, NaI, Na 2cO 3, Na 2sO 3or Na 2c 2o 4, use reducing agent N 2h 4h 2o wherein a part will be reduced to silver, because the Ksp of deposited salt is less, so Ag free in whole system +less, reaction speed can be made like this to slow down, realize the dynamics Controlling of Nano silver piece growth, the growth being beneficial to Nano silver piece controls, the AgNO added 3enter into solution, can with free CNS -, Cl -, Br -, I -, CO 3 2-, SO 3 2-or C 2o 4 2-form AgCNS, AgCl, AgBr, AgI, Ag 2cO 3, Ag 2sO 3or Ag 2c 2o 4, make system maintain Ag +dynamic equilibrium, to reach the object of controlled synthesis Nano silver piece.
In the preparation process of 2, single dispersing Nano silver piece of the present invention, the length of side and the thickness of Nano silver piece are controlled.The size uniformity of gained Nano silver piece, controlled, purity and yield high, utilize the signs such as SEM, TEM, in product, do not find the product that there is other patterns such as particle.
3, preparation process of the present invention is simple to operate, and the reaction time is short, and cost is low.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the AgCNS crystal grain that embodiment 1 obtains.
Fig. 2 is the TEM photo of embodiment 1-16 Nano silver piece crystal seed used.
Fig. 3 is the TEM photo of the Nano silver piece that embodiment 1 obtains.
Fig. 4 is the SEM photo of the Nano silver piece that embodiment 2 obtains.
Detailed description of the invention:
Below by specific embodiment, also the present invention will be further described by reference to the accompanying drawings, but be not limited thereto.
Raw materials usedly in embodiment be convenient source, commercial products.Wherein PVP is PVP-K30, and mean molecule quantity is 45,000 ~ 58,000.
Nano silver piece crystal seed suspension used in embodiment 1-16, prepares as follows:
Under room temperature, in 200mL water, add the C that 12mL concentration is 0.075mol/L 6h 5na 3o 7solution, 200 μ L concentration are the AgNO of 0.1mol/L 3solution and 480 μ L concentration are the H of 30wt% 2o 2solution, stirs; Then the concentration adding 1.2mL brand-new in solution is fast the NaBH of 0.1mol/L 4solution, vigorous stirring, until solution becomes blueness, then by reacted solution left standstill 24h, obtains the Nano silver piece crystal seed suspension that concentration is 9.72mg/L.
Fig. 2 is the TEM photo of obtained Nano silver piece crystal seed.As shown in Figure 2, the length of side of obtained Nano silver piece crystal seed is 20 ± 5nm, and thickness is 5 ± 2nm.
Embodiment 1
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) be added to by the PVP of 0.222g in 50mL Nano silver piece crystal seed suspension, stirring and dissolving under 30 DEG C of conditions, adds the C of 0.13134g 6h 8o 7, form homogeneous mixed solution;
(2) by PVP and NH 4sCN is added to the water and stirs, and the mol ratio of PVP and water is 1:50, NH 4the mol ratio of SCN and water is 1:350; Then, under 45 DEG C of water bath condition, add with the speed of 5mL/min the AgNO that concentration is 10g/L 3the aqueous solution, AgNO 3with NH 4the mol ratio of SCN is 1:1, reaction 0.5h is continued after reinforced, by solid product with the speed centrifugation of 8000r/min, and wash solid product with water 4 times, then in atmosphere in 90 DEG C of oven dry, AgCNS crystal grain is obtained, by AgCNS grain dispersion in water, be mixed with the AgCNS suspension that concentration is 45wt%, stand-by;
(3) in step (1), then add AgCNS suspension obtained in 0.2mL step (2) or the NH of 0.076g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.
Fig. 3 is the TEM photo of the Nano silver piece that the present embodiment obtains.As shown in Figure 3, the length of side of gained Nano silver piece is 140 ± 5nm, and thickness is 32 ± 2nm.
Embodiment 2
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) PVP of 0.222g is joined in 50mL Nano silver piece crystal seed suspension, under 30 DEG C of conditions after stirring and dissolving, add the C of 0.13134g 6h 8o 7, form homogeneous mixed solution;
(2) by PVP and NH 4sCN is added to the water and stirs, and the mol ratio of PVP and water is 1:50, NH 4the mol ratio of SCN and water is 1:350; Then, under 45 DEG C of water bath condition, add with the speed of 5mL/min the AgNO that concentration is 10g/L 3the aqueous solution, AgNO 3with NH 4the mol ratio of SCN is 1:1, reaction 0.5h is continued after reinforced, by solid product with the speed centrifugation of 8000r/min, and wash solid product with water 4 times, then in atmosphere in 90 DEG C of oven dry, AgCNS crystal grain is obtained, by AgCNS grain dispersion in water, be mixed with the AgCNS suspension that concentration is 45wt%, stand-by;
(3) in step (1), then add the NH of the obtained AgCNS suspension of 0.1mL step (2) or 0.038g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), after 30 DEG C of stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Continue stirring reaction 30min after adding, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.
Fig. 4 is the SEM photo of the Nano silver piece that the present embodiment obtains.As shown in Figure 4, the length of side of gained Nano silver piece is 185 ± 5nm, and thickness is 24 ± 2nm.
Embodiment 3
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) PVP of 0.222g is joined in 50mL Nano silver piece crystal seed suspension, under 30 DEG C of conditions after stirring and dissolving, add the C of 0.13134g 6h 8o 7, form homogeneous mixed solution;
(2) by PVP and NH 4sCN is added to the water and stirs, and the mol ratio of PVP and water is 1:60, NH 4the mol ratio of SCN and water is 1:250; Then, under 30 DEG C of water bath condition, add with the speed of 1mL/min the AgNO that concentration is 15g/L 3the aqueous solution, AgNO 3with NH 4the mol ratio of SCN is 1:1, reaction 1h is continued after reinforced, by solid product with the speed centrifugation of 3000r/min, and wash solid product with water 3 times, then in atmosphere in 60 DEG C of oven dry, AgCNS crystal grain is obtained, by AgCNS grain dispersion in water, be mixed with the AgCNS suspension that concentration is 45wt%, stand-by;
(3) in step (1), then add the NH of the obtained AgCNS suspension of 0.04mL step (2) or 0.0152g 4sCN, then add 120 μthe N of L 2h 4h 2o (85wt%), after 30 DEG C of stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3; Continue stirring reaction 30min after adding, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%, and the length of side of gained Nano silver piece is 220 ± 20nm, and thickness is 18 ± 2nm.
Embodiment 4
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) PVP of 0.222g is joined in 50mL Nano silver piece crystal seed suspension, under 30 DEG C of conditions after stirring and dissolving, add the C of 0.13134g 6h 8o 7, form homogeneous mixed solution;
(2) by PVP and NH 4sCN is added to the water and stirs, and the mol ratio of PVP and water is 1:400, NH 4the mol ratio of SCN and water is 1:300; Then, under 40 DEG C of water bath condition, add with the speed of 3mL/min the AgNO that concentration is 20g/L 3the aqueous solution, AgNO 3with NH 4the mol ratio of SCN is 1:1, reaction 2h is continued after reinforced, by solid product with the speed centrifugation of 4000r/min, and wash solid product with water 2 times, then in atmosphere in 80 DEG C of oven dry, AgCNS crystal grain is obtained, by AgCNS grain dispersion in water, be mixed with the AgCNS suspension that concentration is 45wt%, stand-by;
(3) in step (1), then add the NH of the obtained AgCNS suspension of 0.002mL step (2) or 0.00076g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), after 30 DEG C of stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Continue stirring reaction 30min after adding, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%, and the length of side of gained Nano silver piece is 500 ± 50nm, and thickness is 10 ± 2nm.
Embodiment 5
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) (2) are with embodiment 1;
(3) in step (1), add the NH of the obtained AgCNS suspension of 0.2mL step (2) or 0.076g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), after 30 DEG C of stirring reaction 15min, then adds the AgNO that 40mL concentration is 8.5g/L 3solution; Continue stirring reaction 30min after adding, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.5266g, and yield is 99.1%, and the length of side of gained Nano silver piece is 200 ± 20nm, and thickness is 20 ± 2nm.
Embodiment 6
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) PVP of 0.222g is joined in 50mL Nano silver piece crystal seed suspension, under 25 DEG C of conditions after stirring and dissolving, add the C of 0.13134g 6h 8o 7, form homogeneous mixed solution;
(2) with embodiment 2;
(2) in step (1), then add the NH of the obtained AgCNS suspension of 0.2mL step (2) or 0.076g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%, and the length of side of gained Nano silver piece is 140 ± 5nm, and thickness is 32 ± 2nm.
Embodiment 7
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) PVP of 0.222g is joined in 50mL Nano silver piece crystal seed suspension, under 40 DEG C of conditions after stirring and dissolving, add the C of 0.13134g 6h 8o 7, form homogeneous mixed solution;
(2) with embodiment 2;
(3) in step (1), then add the NH of the obtained AgCNS suspension of 0.2mL step (2) or 0.076g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%, and the length of side of gained Nano silver piece is 320 ± 20nm, and thickness is 20 ± 2nm.
Embodiment 8
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1), (2) are with embodiment 4;
(3) in step (1), then add the NH of the obtained AgCNS suspension of 0.2mL step (2) or 0.076g 4sCN, then the N adding 480 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%, and the length of side of gained Nano silver piece is 140 ± 5nm, and thickness is 32 ± 2nm.
Embodiment 9
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) PVP of 0.333g is joined in 50mL Nano silver piece crystal seed suspension, under 30 DEG C of conditions after stirring and dissolving, add the C of 0.13134g 6h 8o 7, form homogeneous mixed solution;
(2) with embodiment 3;
(3) in step (1), then add the NH of the obtained AgCNS suspension of 0.2mL step (2) or 0.076g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%, and the length of side of gained Nano silver piece is 130 ± 5nm, and thickness is 40 ± 2nm.
Embodiment 10
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) PVP of 0.222g is joined in 50mL Nano silver piece crystal seed suspension, under 30 DEG C of conditions after stirring and dissolving, add the C of 0.39402g 6h 8o 7, form homogeneous mixed solution;
(2) with embodiment 4;
(3) in step (1), then add the NH of the obtained AgCNS suspension of 0.2mL step (2) or 0.076g 4sCN, then the N adding 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%, and the length of side of gained Nano silver piece is 250 ± 10nm, and thickness is 18 ± 2nm.
Embodiment 11
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) with embodiment 1;
(2) be added to the water by PVP and NaCl and stir, the mol ratio of PVP and water is the mol ratio of 1:50, NaCl and water is 1:200; Then, under 20 DEG C of water bath condition, add with the speed of 0.1mL/min the AgNO that concentration is 25g/L 3the aqueous solution, AgNO 3be 1:1 with the mol ratio of NaCl, continue reaction 3h after reinforced, by solid product with the speed centrifugation of 2000r/min, and wash solid product with water 4 times, then in atmosphere in 40 DEG C of oven dry, obtain AgCl crystal grain; By AgCl grain dispersion in water, be mixed with the AgCl suspension that concentration is 45wt%, stand-by;
(3) in step (1), then add the NaCl of the obtained AgCl suspension of 0.2mL step (2) or 0.058g, then add the N of 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.The length of side of gained Nano silver piece is 250 ± 10nm, and thickness is 12 ± 2nm.
Embodiment 12
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) with embodiment 1;
(2) be added to the water by PVP and NaBr and stir, the mol ratio of PVP and water is the mol ratio of 1:50, NaBr and water is 1:200; Then, under 20 DEG C of water bath condition, add with the speed of 0.1mL/min the AgNO that concentration is 25g/L 3the aqueous solution, AgNO 3be 1:1 with the mol ratio of NaBr, continue reaction 3h after reinforced, by solid product with the speed centrifugation of 2000r/min, and wash solid product with water 4 times, then in atmosphere in 40 DEG C of oven dry, obtain AgBr crystal grain; By AgBr grain dispersion in water, be mixed with the AgBr suspension that concentration is 45wt%, stand-by;
(3) in step (1), then add the NaBr of the obtained AgBr suspension of 0.2mL step (2) or 0.103g, then add the N of 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.The length of side of gained Nano silver piece is 180 ± 10nm, and thickness is 20 ± 5nm.
Embodiment 13
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) with embodiment 1;
(2) be added to the water by PVP and NaI and stir, the mol ratio of PVP and water is the mol ratio of 1:50, NaI and water is 1:200; Then, under 20 DEG C of water bath condition, add with the speed of 0.1mL/min the AgNO that concentration is 25g/L 3the aqueous solution, AgNO 3be 1:1 with the mol ratio of NaI, continue reaction 3h after reinforced, by solid product with the speed centrifugation of 2000r/min, and wash solid product with water 4 times, then in atmosphere in 40 DEG C of oven dry, obtain AgI crystal grain; By AgI grain dispersion in water, be mixed with the AgI suspension that concentration is 45wt%, stand-by;
(3) in step (1), then add the NaI of the obtained AgI suspension of 0.2mL step (2) or 0.150g, then add the N of 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.The length of side of gained Nano silver piece is 250 ± 10nm, and thickness is 12 ± 2nm.
Embodiment 14
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) with embodiment 1;
(2) by PVP and Na 2cO 3be added to the water and stir, the mol ratio of PVP and water is 1:50, Na 2cO 3be 1:200 with the mol ratio of water; Then, under 20 DEG C of water bath condition, add with the speed of 0.1mL/min the AgNO that concentration is 25g/L 3the aqueous solution, AgNO 3with Na 2cO 3mol ratio be 1:1, continue reaction 3h after reinforced, by solid product with the speed centrifugation of 2000r/min, and wash solid product with water 4 times, then in atmosphere in 40 DEG C of oven dry, obtain Ag 2cO 3crystal grain; By Ag 2cO 3grain dispersion, in water, is mixed with the Ag that concentration is 45wt% 2cO 3suspension, stand-by;
(3) in step (1), then add the Ag that 0.2mL step (2) is obtained 2cO 3the Na of suspension or 0.106g 2cO 3, then add the N of 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.The length of side of gained Nano silver piece is 220 ± 10nm, and thickness is 18 ± 2nm.
Embodiment 15
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) with embodiment 1;
(2) by PVP and Na 2sO 3be added to the water and stir, the mol ratio of PVP and water is 1:50, Na 2sO 3be 1:200 with the mol ratio of water; Then, under 20 DEG C of water bath condition, add with the speed of 0.1mL/min the AgNO that concentration is 25g/L 3the aqueous solution, AgNO 3with Na 2sO 3mol ratio be 1:1, continue reaction 3h after reinforced, by solid product with the speed centrifugation of 2000r/min, and wash solid product with water 4 times, then in atmosphere in 40 DEG C of oven dry, obtain Ag 2sO 3crystal grain; By Ag 2sO 3grain dispersion, in water, is mixed with the Ag that concentration is 45wt% 2sO 3suspension, stand-by;
(3) in step (1), then add the Ag that 0.2mL step (2) is obtained 2sO 3the Na of suspension or 0.126g 2sO 3, then add the N of 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.The length of side of gained Nano silver piece is 220 ± 10nm, and thickness is 18 ± 2nm.
Embodiment 16
A preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) with embodiment 1;
(2) by PVP and Na 2c 2o 4be added to the water and stir, the mol ratio of PVP and water is 1:50, Na 2c 2o 4be 1:200 with the mol ratio of water; Then, under 20 DEG C of water bath condition, add with the speed of 0.1mL/min the AgNO that concentration is 25g/L 3the aqueous solution, AgNO 3with Na 2c 2o 4mol ratio be 1:1, continue reaction 3h after reinforced, by solid product with the speed centrifugation of 2000r/min, and wash solid product with water 4 times, then in atmosphere in 40 DEG C of oven dry, obtain Ag 2c 2o 4crystal grain; By Ag 2c 2o 4grain dispersion, in water, is mixed with the Ag that concentration is 45wt% 2c 2o 4suspension, stand-by;
(3) in step (1), then add the Ag that 0.2mL step (2) is obtained 2c 2o 4the Na of suspension or 0.134g 2c 2o 4, then add the N of 120 μ L 2h 4h 2o (85wt%), at 30 DEG C after stirring reaction 15min, then adds the AgNO that 20mL concentration is 8.5g/L 3solution; Add rear continuation stirring reaction 30min, the solid product centrifuge washing then will obtained, obtains the Nano silver piece of 0.1866g, and yield is 99.0%.The length of side of gained Nano silver piece is 3000 ± 10nm, and thickness is 15 ± 2nm.

Claims (10)

1. a preparation in macroscopic quantity method for single dispersing Nano silver piece, step is as follows:
(1) under 20-40 DEG C of water bath condition, be add polyvinylpyrrolidone (PVP) and citric acid (C in the Nano silver piece crystal seed suspension of 9-10mg/L to concentration 6h 8o 7) stir, form homogeneous mixed solution, Nano silver piece crystal seed: PVP:C 6h 8o 7mol ratio be (0.03-0.1): (15-50): (3-15);
(2) by PVP and NH 4sCN or NaCl or NaBr or NaI or Na 2cO 3or Na 2sO 3or Na 2c 2o 4be added to the water and stir, the mol ratio of PVP and water is 1:(50-500), NH 4the mol ratio of SCN or NaCl or NaBr or NaI and water is 1:(200-350), Na 2cO 3or Na 2sO 3or Na 2c 2o 4be 1:(400-700 with the mol ratio of water);
Then, under 20-45 DEG C of water bath condition, add with the speed of 0.1-5mL/min the AgNO that concentration is 10-25g/L 3the aqueous solution; AgNO 3with NH 4the mol ratio of SCN or NaCl or NaBr or NaI is 1:(0.8-1.5), AgNO 3with Na 2cO 3or Na 2sO 3or Na 2c 2o 4mol ratio be 1:(0.4-0.75); Continue reaction 0.5-3h after reinforced, by solid product with the speed centrifugation of 2000-8000r/min, and wash solid product with water 1 ~ 4 time, then in atmosphere in 40-90 DEG C of oven dry, obtain AgCNS, AgCl, AgBr, AgI, Ag 2cO 3, Ag 2sO 3or Ag 2c 2o 4crystal grain;
By AgCNS, AgCl, AgBr, AgI, Ag of obtaining 2cO 3, Ag 2sO 3or Ag 2c 2o 4grain dispersion, in water, is mixed with the suspension that concentration is 30-50wt%, stand-by;
(3) AgCNS, AgCl, AgBr, AgI, Ag that step (2) is obtained is added in the mixed solution obtained to step (1) 2cO 3, Ag 2sO 3or Ag 2c 2o 4suspension; Or in the mixed solution that step (1) obtains, add NH 4sCN, NaCl, NaBr, NaI, Na 2cO 3, Na 2sO 3or Na 2c 2o 4;
Then reducing agent hydrazine hydrate (N is added 2h 4h 2o), after reaction 2-20min, then the AgNO that concentration is 5-20g/L is added 3the aqueous solution, reaction 10-60min, by the solid product centrifuge washing obtained, obtains single dispersing Nano silver piece;
In reaction system, described AgNO 3: AgCNS or AgCl or AgBr or AgI:N 2h 4h 2the mol ratio of O is (8-20): (0.5-2500): (15-50), described AgNO 3: Ag 2cO 3or Ag 2sO 3or Ag 2c 2o 4: N 2h 4h 2the mol ratio of O is (8-20): (0.25-1250): (15-50), described AgNO 3: NH 4sCN or NaCl or NaBr or NaI:N 2h 4h 2the mol ratio of O is (8-20): (0.5-2500): (15-50), described AgNO 3: Na 2cO 3or Na 2sO 3or Na 2c 2o 4: N 2h 4h 2the mol ratio of O is (8-20): (0.25-1250): (15-50).
2. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, the Nano silver piece crystal seed described in step (1): PVP:C 6h 8o 7mol ratio be (0.035-0.1): (15-45): (4-14).
3. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, the mol ratio of the PVP described in step (2) and water is 1:(60-400).
4. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, NH in step (2) 4the mol ratio of SCN or NaCl or NaBr or NaI and water is 1:(250-300), Na 2cO 3or Na 2sO 3or Na 2c 2o 4be 1:(500-600 with the mol ratio of water).
5. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, AgNO in step (2) 3the concentration of the aqueous solution is 15-20g/L, and adding speed is 0.2-4mL/min.
6. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, AgCNS, AgCl, AgBr, AgI, the Ag described in step (2) 2cO 3, Ag 2sO 3or Ag 2c 2o 4the concentration of suspension is 40-50wt%.
7. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, the AgNO described in step (3) 3: AgCNS or AgCl or AgBr or AgI:N 2h 4h 2the mol ratio of O is (10-20): (0.5-2000): (15-45).
8. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, the AgNO described in step (3) 3: Ag 2cO 3or Ag 2sO 3or Ag 2c 2o 4: N 2h 4h 2the mol ratio of O is (10-20): (0.25-1000): (15-45).
9. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, the AgNO described in step (3) 3: NH 4sCN or NaCl or NaBr or NaI:N 2h 4h 2the mol ratio of O is (10-20): (0.5-2000): (15-45); Described AgNO 3: Na 2cO 3or Na 2sO 3or Na 2c 2o 4: N 2h 4h 2the mol ratio of O is (10-20): (0.25-1000): (15-45).
10. the preparation in macroscopic quantity method of single dispersing Nano silver piece according to claim 1, is characterized in that, the Nano silver piece crystal seed suspension described in step (1) prepares as follows:
Under room temperature, in 200mL water, add the C that 10-15mL concentration is 0.07-0.08mol/L 6h 5na 3o 7solution, 195-210 μ L concentration is the AgNO of 0.1mol/L 3solution and 470-485 μ L concentration are the H of 30wt% 2o 2solution, stirs; Then the concentration adding 1.0-1.5mL brand-new in solution is fast the NaBH of 0.1mol/L 4solution, vigorous stirring, until solution becomes blueness, then by reacted solution left standstill 20-30h, obtains Nano silver piece crystal seed suspension.
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104551007A (en) * 2015-01-13 2015-04-29 山东大学 Large-scale preparation method of silver nano-sheets
CN105268995A (en) * 2015-12-02 2016-01-27 广东南海启明光大科技有限公司 Method for preparing nano-silver plate
CN108356284A (en) * 2018-03-29 2018-08-03 景德镇陶瓷大学 A kind of preparation method of silver nanocubes
CN109773211A (en) * 2019-03-26 2019-05-21 南京工业大学 Preparation method for coating nano silver particles on surface of flake silver powder
CN110253033A (en) * 2019-07-30 2019-09-20 三明学院 A method of quickly preparing triangular silver nanosheet at room temperature
CN110449598A (en) * 2019-09-06 2019-11-15 辽宁星空新能源发展有限公司 A kind of method that rapid precipitation prepares two-dimensional metallic silver simple substance nanometer sheet
CN110899722A (en) * 2019-12-26 2020-03-24 无锡晶睿光电新材料有限公司 Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof
CN111250729A (en) * 2020-04-02 2020-06-09 海泰纳鑫科技(成都)有限公司 Method for adjusting size of silver nanosheet
CN115570144A (en) * 2022-09-20 2023-01-06 天津理工大学 Preparation method of silver nanosheet with controllable thickness

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1958197A (en) * 2006-11-16 2007-05-09 中国科学院长春应用化学研究所 Method for preparing Nano silver piece
KR20080063976A (en) * 2007-01-03 2008-07-08 주식회사 세화엔스텍 Manufacture of high purity silver nano-powder with reducing agent
CN101947655A (en) * 2010-10-25 2011-01-19 江苏技术师范学院 Preparation method of triangular silver nanosheet
CN102407342A (en) * 2011-10-31 2012-04-11 山东大学 Preparation method of nano silver powder with accurately controllable particle size
CN102672200A (en) * 2012-06-06 2012-09-19 南京医科大学第二附属医院 Water phase preparation method of spherical silver nanoparticle with adjustable size
JP2012246560A (en) * 2011-05-31 2012-12-13 Daicel Corp Method of manufacturing silver-containing nanoparticle, silver-containing nanoparticle, and silver coating composition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1958197A (en) * 2006-11-16 2007-05-09 中国科学院长春应用化学研究所 Method for preparing Nano silver piece
KR20080063976A (en) * 2007-01-03 2008-07-08 주식회사 세화엔스텍 Manufacture of high purity silver nano-powder with reducing agent
CN101947655A (en) * 2010-10-25 2011-01-19 江苏技术师范学院 Preparation method of triangular silver nanosheet
JP2012246560A (en) * 2011-05-31 2012-12-13 Daicel Corp Method of manufacturing silver-containing nanoparticle, silver-containing nanoparticle, and silver coating composition
CN102407342A (en) * 2011-10-31 2012-04-11 山东大学 Preparation method of nano silver powder with accurately controllable particle size
CN102672200A (en) * 2012-06-06 2012-09-19 南京医科大学第二附属医院 Water phase preparation method of spherical silver nanoparticle with adjustable size

Cited By (10)

* Cited by examiner, † Cited by third party
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CN104551007A (en) * 2015-01-13 2015-04-29 山东大学 Large-scale preparation method of silver nano-sheets
CN105268995A (en) * 2015-12-02 2016-01-27 广东南海启明光大科技有限公司 Method for preparing nano-silver plate
CN108356284A (en) * 2018-03-29 2018-08-03 景德镇陶瓷大学 A kind of preparation method of silver nanocubes
CN108356284B (en) * 2018-03-29 2021-04-09 景德镇陶瓷大学 Preparation method of silver nanocubes
CN109773211A (en) * 2019-03-26 2019-05-21 南京工业大学 Preparation method for coating nano silver particles on surface of flake silver powder
CN110253033A (en) * 2019-07-30 2019-09-20 三明学院 A method of quickly preparing triangular silver nanosheet at room temperature
CN110449598A (en) * 2019-09-06 2019-11-15 辽宁星空新能源发展有限公司 A kind of method that rapid precipitation prepares two-dimensional metallic silver simple substance nanometer sheet
CN110899722A (en) * 2019-12-26 2020-03-24 无锡晶睿光电新材料有限公司 Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof
CN111250729A (en) * 2020-04-02 2020-06-09 海泰纳鑫科技(成都)有限公司 Method for adjusting size of silver nanosheet
CN115570144A (en) * 2022-09-20 2023-01-06 天津理工大学 Preparation method of silver nanosheet with controllable thickness

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