CN102806358B - Synthesis method of water-soluble monodisperse spherical silver nanocrystals - Google Patents
Synthesis method of water-soluble monodisperse spherical silver nanocrystals Download PDFInfo
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- CN102806358B CN102806358B CN201210315235.0A CN201210315235A CN102806358B CN 102806358 B CN102806358 B CN 102806358B CN 201210315235 A CN201210315235 A CN 201210315235A CN 102806358 B CN102806358 B CN 102806358B
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Abstract
A synthesis method of water-soluble monodisperse spherical silver nanocrystals includes steps of firstly, preparing solution from a required raw material, namely sodium citrate, additives and soluble silver salt with high-purity water; weighing vitamin-C solution, sodium citrate solution, additive solution and soluble sliver salt solution according to the volume ratio of (5-20):100:(3-5):25, adding the vitamin-C solution into boiling water, and mixing the sodium citrate solution, additive solution and soluble silver solution for 3-6 minutes and then adding the mixture into the boiling water containing vitamin-C; and finally keeping the water boiling, heating and refluxing for one hour, and then cooling the solution to the room temperature so as to obtain the monodisperse spherical sliver nanocrystals. Compared with the other synthesis method, the synthesis method is simple in operation and capable of preparing high-quality water-soluble monodisperse spherical sliver nanocrystals which are incapable of being prepared by other conventional methods.
Description
Technical field
The present invention relates to a kind of synthetic method of water-soluble mono dispersing ball silver nanoparticle crystal, specifically utilize the auxiliary natrium citricum reduction soluble silver salt of additive to prepare the method for water-soluble mono dispersing ball silver nanoparticle crystal.
Background technology
In the silver nanoparticle crystal of all patterns, only have spherical silver nanocrystal to go for Mie theory.Mie theory provides a kind of method of the Maxwell of analysis equation.In addition, spherical silver nanocrystal also has many application, SERS for example, unimolecule mark and identification etc.In the method for countless synthesizing spherical silver nanoparticle crystal, only in organic solvent, just can obtain at present monodisperse spherical silver nanoparticle crystal.But poisonous organic solvent and organic ligand, be unfavorable for their application in the fields such as biology.At present, in the aqueous solution, prepare the spherical silver nanocrystal that spherical silver nanocrystal or a difficult point, particularly diameter dimension are greater than 10 nanometers.Preparation difficulty due to water-soluble, monodispersed spherical silver nanocrystal, also cannot realize the quantitative analysis of silver nanoparticle crystal to Study of cytotoxicity now.Natrium citricum is a kind of biocompatibility part, and easily by replacements such as other biological molecule, antibody, therefore, the stable spherical silver nanocrystal of natrium citricum part has vast application prospect.
At present, at natrium citricum reduction soluble silver salt, prepare in the whole bag of tricks of monodispersed spherical silver nanocrystal, although simple to operate, but due to silver-colored growth characteristic, the product obtaining often different-shape silver nanoparticle crystal (for example, bar-shaped, triangular plate and elliposoidal) mix products.Although in some documents, by decomposing auxiliary law by laser light, obtain monodispersed spherical silver nanocrystal, be not suitable for production in enormous quantities.
Summary of the invention
The present invention is directed to existing natrium citricum reduction soluble silver salt and prepare the deficiency of monodispersed spherical silver nanocrystal, provide a kind of technique simple, the synthetic synthetic method of water-soluble mono dispersing ball silver nanoparticle crystal efficiently.
The synthetic method of water-soluble monodispersed spherical silver nanocrystal of the present invention, comprises the following steps:
(1) using high purity water that needed raw material natrium citricum, auxiliary additive and soluble silver salt are mixed with respectively to mass percent concentration is that 1% sodium citrate solution, concentration are the silver soluble salting liquid that the auxiliary additive solution of 0.1 mM/l-100 mM/ls and mass percent concentration are 1%; Auxiliary additive refers to and can generate sedimentary material (as copper bromide, KI, sodium chloride, sodium sulphate, sodium phosphate, sodium carbonate or vulcanized sodium etc.) with silver ion; Soluble silver salt refers to silver nitrate or silver perchlorate;
(2) ratio of 5-20:100:3-5:25 takes respectively sodium citrate solution, auxiliary additive solution and the silver soluble salting liquid that concentration is the vitamin c solution of 100 mM/ls and step (1) preparation by volume;
(3) vitamin c solution is added just in the boiling water of ebuillition of heated;
(4) sodium citrate solution, auxiliary additive solution and the mixing of silver soluble salting liquid, after 3-6 minute, are added rapidly and contained in ascorbic boiling water;
(5) keep boiling, add hot reflux and be cooled to room temperature after 1 hour, can obtain monodispersed spherical silver nanocrystal.
The present invention adopts the auxiliary natrium citricum reduction soluble silver salt of additive to prepare monodispersed spherical silver nanocrystal, compare other synthetic method, the method is simple to operate, can obtain high-quality, water-soluble monodispersed spherical silver nanocrystal that other existing method cannot obtain.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the monodispersed spherical silver nanocrystal of embodiment 1 gained.
The specific embodiment
Embodiment 1
First the glassware used vial of 10 milliliters (there-necked flask and) is put into chloroazotic acid and soak after 2 hours, with sodium nitrate saturated solution and high purity water, clean dry for standby.Use high purity water that needed raw material natrium citricum, silver nitrate and copper bromide are configured to respectively to solution, wherein the mass percent concentration of sodium citrate solution is 1%, and the mass percent concentration of liquor argenti nitratis ophthalmicus is 1%, and the concentration of copper bromide solution is 4 mM/ls.There-necked flask be fixed on warm table and add the high purity water of 47.5 milliliters, being heated to rapidly boiling.The vitamin C of 50 microlitres (100 mM/ls) is added in boiling water.Then 1 milliliter of sodium citrate solution, 50 microlitre copper bromides and 250 microlitre liquor argenti nitratis ophthalmicuses were mixed after 3 minutes, add rapidly and contain in ascorbic boiling water.Finally keep boiling, add hot reflux after 1 hour, be cooled to room temperature, can obtain monodispersed spherical silver nanocrystal, the transmission electron microscope photo of spherical silver nanocrystal as shown in Figure 1.
Embodiment 2
The difference one of the present embodiment and embodiment is that the concentration of copper bromide solution is 10 mM/ls, the 2nd, the vitamin C of 75 microlitres (100 mM/ls) is added in boiling water, all the other conditions are all identical with embodiment 1, can obtain equally monodispersed spherical silver nanocrystal.
Embodiment 3
The difference one of the present embodiment and embodiment is that the concentration of copper bromide solution is 10 mM/ls, the 2nd, the vitamin C of 100 microlitres (100 mM/ls) is added in boiling water, all the other conditions are all identical with embodiment 1, can obtain equally monodispersed spherical silver nanocrystal.
Embodiment 4
First the glassware used vial of 10 milliliters (there-necked flask and) is put into chloroazotic acid and soak after 2 hours, with sodium nitrate saturated solution and high purity water, clean dry for standby.Use high purity water that needed raw material natrium citricum, silver nitrate and KI are made into sodium citrate solution, liquor argenti nitratis ophthalmicus and liquor kalii iodide, wherein the mass percent concentration of sodium citrate solution is 1%, the mass percent concentration of liquor argenti nitratis ophthalmicus is 1%, and the concentration of liquor kalii iodide is 0.1 mM/l.Then the vitamin C of 50 microlitres (100 mM/ls) is added in boiling water.Then 1 milliliter of sodium citrate solution, 30 microlitre liquor kalii iodides and 250 microlitre liquor argenti nitratis ophthalmicuses were mixed after 5 minutes, add rapidly and contain in ascorbic boiling water.Finally keep boiling, add hot reflux after 1 hour, be cooled to room temperature, can obtain monodispersed spherical silver nanocrystal.
Embodiment 5
The difference of the present embodiment and embodiment is that the vitamin C of 75 microlitres (100 mM/ls) is added in boiling water, and all the other conditions are all identical with embodiment 4, can obtain equally monodispersed spherical silver nanocrystal.
Embodiment 6
The difference of the present embodiment and embodiment is that the vitamin C of 100 microlitres (100 mM/ls) is added in boiling water, and all the other conditions are all identical with embodiment 4, can obtain equally monodispersed spherical silver nanocrystal.
Embodiment 7
First the glassware used vial of 10 milliliters (there-necked flask and) is put into chloroazotic acid and soak after 2 hours, with sodium nitrate saturated solution and high purity water, clean dry for standby.Use high purity water that needed raw material natrium citricum, silver nitrate and sodium chloride are made into sodium citrate solution, liquor argenti nitratis ophthalmicus and sodium chloride solution, wherein the mass percent concentration of sodium citrate solution is 1%, the mass percent concentration of liquor argenti nitratis ophthalmicus is 1%, and the concentration of sodium chloride solution is 100 mM/ls.Then the vitamin C of 50 microlitres is added in boiling water.Then 1 milliliter of sodium citrate solution, 40 microlitre sodium chloride solutions and 250 microlitre liquor argenti nitratis ophthalmicuses were mixed after 6 minutes, add rapidly and contain in ascorbic boiling water.Finally keep boiling, add hot reflux after 1 hour, be cooled to room temperature, can obtain monodispersed spherical silver nanocrystal.
Embodiment 8
The difference of the present embodiment and embodiment is that the vitamin C of 100 microlitres (100 mM/ls) is added in boiling water, and all the other conditions are all identical with embodiment 7, can obtain equally monodispersed spherical silver nanocrystal.
Embodiment 9
The difference of the present embodiment and embodiment is that the vitamin C of 200 microlitres (100 mM/ls) is added in boiling water, and all the other conditions are all identical with embodiment 7, can obtain equally monodispersed spherical silver nanocrystal.
Embodiment 10
First the glassware used vial of 10 milliliters (there-necked flask and) is put into chloroazotic acid and soak after 2 hours, with sodium nitrate saturated solution and high purity water, clean dry for standby.Use high purity water that needed raw material natrium citricum, silver nitrate and vulcanized sodium are made into sodium citrate solution, liquor argenti nitratis ophthalmicus and sodium sulfide solution, wherein the mass percent concentration of sodium citrate solution is 1%, the mass percent concentration of liquor argenti nitratis ophthalmicus is 1%, and the concentration of sodium sulfide solution is 0.1 mM/l.Then the vitamin C of 50 microlitres is added in boiling water.Then 1 milliliter of sodium citrate solution, 30 microlitre sodium sulfide solutions and 250 microlitre liquor argenti nitratis ophthalmicuses were mixed after 4 minutes, add rapidly and contain in ascorbic boiling water.Finally keep boiling, add hot reflux after 1 hour, be cooled to room temperature, can obtain monodispersed spherical silver nanocrystal.
Embodiment 11
First the glassware used vial of 10 milliliters (there-necked flask and) is put into chloroazotic acid and soak after 2 hours, with sodium nitrate saturated solution and high purity water, clean dry for standby.Use high purity water that needed raw material natrium citricum, silver perchlorate and sodium sulphate are made into sodium citrate solution, liquor argenti nitratis ophthalmicus and metabisulfite solution, wherein the mass percent concentration of sodium citrate solution is 1%, the mass percent concentration of silver perchlorate solution is 1%, and the concentration of metabisulfite solution is 80 mM/ls.Then the vitamin C of 50 microlitres is added in boiling water.Then 1 milliliter of sodium citrate solution, 30 microlitre metabisulfite solutions and 250 microlitre liquor argenti nitratis ophthalmicuses were mixed after 5 minutes, add rapidly and contain in ascorbic boiling water.Finally keep boiling, add hot reflux after 1 hour, be cooled to room temperature, can obtain monodispersed spherical silver nanocrystal.
Embodiment 12
First the glassware used vial of 10 milliliters (there-necked flask and) is put into chloroazotic acid and soak after 2 hours, with sodium nitrate saturated solution and high purity water, clean dry for standby.Use high purity water that needed raw material natrium citricum, silver nitrate and sodium carbonate are made into sodium citrate solution, liquor argenti nitratis ophthalmicus and sodium carbonate liquor, wherein the mass percent concentration of sodium citrate solution is 1%, the mass percent concentration of liquor argenti nitratis ophthalmicus is 1%, and the concentration of sodium carbonate liquor is 0.1 mM/l.Then the vitamin C of 50 microlitres is added in boiling water.Then 1 milliliter of sodium citrate solution, 100 microlitre sodium carbonate liquors and 250 microlitre liquor argenti nitratis ophthalmicuses were mixed after 5 minutes, add rapidly and contain in ascorbic boiling water.Finally keep boiling, add hot reflux after 1 hour, be cooled to room temperature, can obtain monodispersed spherical silver nanocrystal.
Embodiment 13
First the glassware used vial of 10 milliliters (there-necked flask and) is put into chloroazotic acid and soak after 2 hours, with sodium nitrate saturated solution and high purity water, clean dry for standby.Use high purity water that needed raw material natrium citricum, silver perchlorate and sodium phosphate are made into sodium citrate solution, silver perchlorate solution and sodium radio-phosphate,P-32 solution, wherein the mass percent concentration of sodium citrate solution is 1%, the mass percent concentration of silver perchlorate solution is 1%, and the concentration of sodium radio-phosphate,P-32 solution is 0.1 mM/l.Then the vitamin C of 50 microlitres is added in boiling water.Then 1 milliliter of sodium citrate solution, 100 microlitre sodium radio-phosphate,P-32 solutions and 250 microlitre liquor argenti nitratis ophthalmicuses were mixed after 5 minutes, add rapidly and contain in ascorbic boiling water.Finally keep boiling, add hot reflux after 1 hour, be cooled to room temperature, can obtain monodispersed spherical silver nanocrystal.
Claims (1)
1. a synthetic method for water-soluble monodispersed spherical silver nanocrystal, is characterized in that, comprises the following steps:
(1) using high purity water that needed raw material natrium citricum, auxiliary additive and soluble silver salt are mixed with respectively to mass percent concentration is that 1% sodium citrate solution, concentration are the silver soluble salting liquid that the auxiliary additive solution of 0.1 mM/l-100 mM/ls and mass percent concentration are 1%; Auxiliary additive refers to and can generate sedimentary material with silver ion; Soluble silver salt refers to silver nitrate or silver perchlorate;
(2) ratio of 5-20:100:3-5:25 takes respectively sodium citrate solution, auxiliary additive solution and the silver soluble salting liquid that concentration is the vitamin c solution of 100 mM/ls and step (1) preparation by volume;
(3) vitamin c solution is added just in the boiling water of ebuillition of heated;
(4) sodium citrate solution, auxiliary additive solution and the mixing of silver soluble salting liquid, after 3-6 minute, are added rapidly and contained in ascorbic boiling water;
(5) keep boiling, add hot reflux and be cooled to room temperature after 1 hour, can obtain monodispersed spherical silver nanocrystal.
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| CN105252019A (en) * | 2015-11-20 | 2016-01-20 | 济南大学 | Preparation method of highly-dispersed spherical nano-silver |
| CN105965029B (en) * | 2016-06-02 | 2017-12-01 | 山东大学 | The synthetic method of water-soluble monodispersed spherical gold-silver alloy nano particle |
| CN109663929B (en) * | 2019-01-24 | 2021-07-23 | 兰州石化职业技术学院 | Preparation method of regular nano gold particles |
| CN114260461B (en) * | 2021-12-28 | 2023-11-03 | 成都市天甫金属粉体有限责任公司 | Multi-fold spherical silver powder and preparation method and application thereof |
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