CN1958197A - Method for preparing Nano silver piece - Google Patents
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- CN1958197A CN1958197A CN 200610131640 CN200610131640A CN1958197A CN 1958197 A CN1958197 A CN 1958197A CN 200610131640 CN200610131640 CN 200610131640 CN 200610131640 A CN200610131640 A CN 200610131640A CN 1958197 A CN1958197 A CN 1958197A
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Abstract
A process for preparing the nano-flakes of monocrystalline silver features use of seed growing method in which the sodium citrate is used as wrapping agent and the surfactant is unnecessary. Its advantage is high purity and stability of product.
Description
Technical field
The present invention relates to a kind of Nano silver piece preparation method.
Background technology
Because metal nanoparticle has special optical property, especially Nano silver grain is particularly noticeable to their research.These special optical properties come from the interaction of free electron in light and the metal.The medium of size, pattern and periphery by selecting nano particle, metal nanoparticle resonant frequency are regulated and control arbitrarily in can be between visible and near infrared region.This character in the optical correlation field such as biology sensor, metal enhanced spectrum or the like a lot of practical applications are arranged.Document also reported and utilized the natrium citricum and the interaction of silver to prepare the Nano silver piece method, and for example Sun etc. has reported that the formation that utilizes natrium citricum can promote silver-colored triangular plate is (referring to Sun, Y. under illumination or heating; Xia, Y.Adv.Mater.2003,15,695. and Sun, Y.; Mayers, B.; Xia, Y.Nano Lett.2003,3,675.).Use the laser irradiation to contain Nano silver grain, silver ion and sodium citrate solution and also can prepare Nano silver piece (Maillard, M.; Huang, P.; Brus, L.Nano Lett.2003,3,1611.).But said method needs high temperature reflux or laser irradiation, and is difficult to control the size of Nano silver piece.Rarely has report especially for synthetic large-sized Nano silver piece.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of Nano silver piece.This method adopts the seed law to prepare Nano silver piece under natrium citricum is assisted.
Step of the present invention and condition are:
A kind of preparation method of Nano silver piece, step and condition are:
(1) preparation of seed
The silver source is: Ag
2SO
4, AgNO
3Or AgClO
4, the concentration in silver-colored source is 0.05mM-1mM;
Coating agent is: natrium citricum, and wherein the mol ratio in coating agent and silver-colored source is 3: 1;
Reducing agent is: sodium borohydride, and wherein the mol ratio between sodium borohydride and the silver-colored source is 6: 1;
In the solution of silver-colored source of pressing proportioning and coating agent, under stirring state, add sodium borohydride silver source by proportioning, obtain the Nano silver grain that size is 2.0～15.0nm, the Nano silver grain that makes thus is a seed;
(2) preparation of Nano silver piece
The silver source is: Ag
2SO
4, AgNO
3Or AgClO
4, the concentration in silver-colored source is 0.05mM-10mM;
Weak reductant is: hydrazine hydrate, ascorbic acid, HAS or HAN, and wherein the mol ratio in weak reductant and silver-colored source is 0.5-20: 1;
Coating agent is: natrium citricum, and wherein the mol ratio received with silver-colored source of citric acid is 0.1-10: 1;
Seed is: use the Nano silver grain of step (1) preparation to be seed, wherein the mol ratio in silver in the seed and silver-colored source is 0.00003-0.5: 1;
Prepare two parts of solution A and B, solution A is weak reductant, coating agent and the seed that contains by proportioning; Solution B is silver-colored source, under stirring state, by proportioning solution B is dropwise added solution A, obtains Nano silver piece.
Characteristics of the present invention are to be coating agent with little inorganic molecule natrium citricum, avoid using other surfactant.Nano silver piece purity height, the good stability of this method preparation.Molar ratio between silver in the control seed and the silver-colored source of use can obtain the Nano silver piece of size arbitrarily.Making the size range that makes Nano silver piece in this way is 25nm-500nm, and thickness is 10-30nm; The adjustable scope of dipole vibration peak is 450-1200nm in the face of Nano silver piece.This method is simple, convenient, for synthetic high-quality Nano silver piece provides a practicable approach.
Description of drawings
Fig. 1 is lie low transmission electron microscope picture on copper mesh of the Nano silver piece that uses seed law preparation under natrium citricum.The size (being the length of the medium line of Nano silver piece) of corresponding Nano silver piece is 116-131nm.
Fig. 2 is for standing in the transmission electron microscope picture on the copper mesh corresponding to the silver-colored sodium rice sheet among Fig. 1.The thickness of corresponding Nano silver piece is 12nm.
Fig. 3 is the ultra-violet absorption spectrum corresponding to the silver strip solution of Fig. 1.The dipole vibration absorption peak is 863nm in the corresponding surface.
The specific embodiment
Embodiment 1:
(1) preparation of seed: containing 0.05mM AgNO
3In the 100mL pure water of 0.15mM natrium citricum, add 1mL 30mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned seed that has made of 1.0mL.The composition of solution B: 30mL contains 0.6mMAgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 83～95nm.
Embodiment 2:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.7mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 63～76nm.
Embodiment 3:
(1) preparation of seed: containing 1mM AgNO
3In the 100mL pure water of 3mM natrium citricum, add 1mL 600mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece; Prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.5mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 70～83nm.
Embodiment 4:
(1) preparation of seed: containing 0.2mM AgClO
4In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 2mL.The composition of solution B: 30mL contains 0.6mMAgClO
4The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 45～61nm.
Embodiment 5:
(1) preparation of seed: containing 0.2mM Ag
2SO
4In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 2mL.The composition of solution B: 30mL contains 0.6mMAg
2SO
4The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 45～61nm.
Embodiment 6:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.2mL.The composition of solution B: 30mL contains 0.6mM AgClO
4The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 103-119nm.
Embodiment 7:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.2mL.The composition of solution B: 30mL contains 0.6mM Ag
2SO
4The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 103-119nm.
Embodiment 8:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM ascorbic acid, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.7mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 63-76nm.
Embodiment 9:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM HAS, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.7mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 63-79nm.
Embodiment 10:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM HAN, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.7mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 63-79nm.
Embodiment 11:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.4mL.The composition of solution B: 30mL contains 0.6mMAgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 80-93nm.
Embodiment 12:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.15mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.4mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 80-93nm.
Embodiment 13:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.03mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.05mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 136-155nm.
Embodiment 14:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 3mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.05mL.The composition of solution B: 30mL contains 0.6mMAgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 136-155nm.
Embodiment 15:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.4mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 15mL.The composition of solution B: 30mL contains 0.6mMAgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 25-30nm.
Embodiment 16:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.4mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.001mL.The composition of solution B: 30mL contains 0.6mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 470-500nm.
Embodiment 17:
(1) preparation of seed: containing 0.2mM AgNO
3In the 100mL pure water of 0.6mM natrium citricum, add 1mL 120mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece: prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 0.6mM hydrazine hydrate, 0.2mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 0.05mL.The composition of solution B: 30mL contains 0.05mM AgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 70～86nm.
Embodiment 18:
(1) preparation of seed: containing 1mM AgNO
3In the 100mL pure water of 3mM natrium citricum, add 1mL 600mM NaBH rapidly
4, stirring 1 hour, the size of the Nano silver grain that obtains is 2.0～15.0nm.
(2) preparation of Nano silver piece; Prepare two parts of solution A and B.The composition of solution A: in the 60mL pure water solution that contains 4mM hydrazine hydrate, 0.6mM natrium citricum, add the above-mentioned Yin Nami seed that has made of 10mL.The composition of solution B: 30mL contains 10mMAgNO
3The aqueous solution.Solution B dropwise adds (1mL/min) in the solution A subsequently, adds the back and continues to stir 10min.The silver strip size that obtains is 75～90nm.
Claims (1)
1, a kind of preparation method of Nano silver piece is characterized in that, step and condition are:
(1) preparation of seed
The silver source is: Ag
2SO
4, AgNO
3Or AgClO
4, the concentration in silver-colored source is 0.05mM-1mM;
Coating agent is: natrium citricum, and wherein the mol ratio in coating agent and silver-colored source is 3: 1;
Reducing agent is: sodium borohydride, and wherein the mol ratio between sodium borohydride and the silver-colored source is 6: 1;
In the solution of silver-colored source of pressing proportioning and coating agent, under stirring state, add sodium borohydride silver source by proportioning, obtain the Nano silver grain that size is 2.0～15.0nm, the Nano silver grain that makes thus is a seed;
(2) preparation of Nano silver piece
The silver source is: Ag
2SO
4, AgNO
3Or AgClO
4, the concentration in silver-colored source is 0.05mM-10mM;
Weak reductant is: hydrazine hydrate, ascorbic acid, HAS or HAN, and wherein the mol ratio in weak reductant and silver-colored source is 0.5-20: 1;
Coating agent is: natrium citricum, and wherein the mol ratio received with silver-colored source of citric acid is 0.1-10: 1;
Seed is: use the Nano silver grain of step (1) preparation to be seed, wherein the mol ratio in silver in the seed and silver-colored source is 0.00003-0.5: 1;
Prepare two parts of solution A and B, solution A is weak reductant, coating agent and the seed that contains by proportioning; Solution B is silver-colored source, under stirring state, by proportioning solution B is dropwise added solution A, obtains Nano silver piece.
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| CN100443222C CN100443222C (en) | 2008-12-17 |
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