CN101844231A - Method for preparing noble metal self-organized colloidal crystal - Google Patents
Method for preparing noble metal self-organized colloidal crystal Download PDFInfo
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Abstract
The invention provides a method for preparing a noble metal self-organized colloidal crystal, which relates to a method for preparing a colloidal crystal. The method solves the problems that a traditional template method for preparing a self-organizing colloidal crystal is difficult in preparing a three-dimensional superlattice and a solvent evaporation method is difficult to be controlled. The method comprises the steps of: adding HAuCl4 solution, AgNO3 solution and sodium citrate solution to water; mixing uniformly; adding the mixed solution to water subject to reflux for 10min-15min; reacting for 1h-1.5h; centrifugalizing and washing reaction products to obtain noble metal nano-particles; adding solvent to the noble metal nano-particles, performing ultrasonic processing to obtain a noble metal colloid suspension; placing a clean substrate vertically in the noble metal colloid suspension, and volatilizing the solvent to obtain the noble metal self-organized colloidal crystal. The noble metal self-organized colloidal crystal has a three-dimensional superlattice structure in a regular bar pattern, is easy to control, and can be used for enhancing polarization Raman.
Description
Technical field
The present invention relates to the preparation method of colloidal crystal.
Background technology
The development of many modern technologies all derives from the successful structure of novel micro-structural or the microminiaturization of existing structure, at integrated circuit, information recording device, MEMS, Miniature Sensor, in biological device of microstream device and the micro-optical component field, on micron and nanoscale, realize the little processing or the patterning of material surface structure and character, can realize faster response speed, more low-cost, more low energy consumption and more effect such as dominance energy, meanwhile, the development of micro-processing technology also is the physics that is taken place in microcosmic and the meso-scale scope, the research of chemistry and biological phenomenon provides opportunity.The precious metal colloid crystal is a diameter at sub-micron or Nano grade, the monodispersed inorganic or polymeric colloid microballoon of size, can self assembly form two dimension or three-dimensional tightly packed arrangement under effects such as gravity, electrostatic force or capillary force, the microsphere aggregation body that these are arranged in order is because it enjoys attention in the effect aspect the enhancing Raman spectrum.The preparation method of existing precious metal colloid crystal has masterplate method, solvent evaporation method etc.During template assemble nanometer particle, because selected rigging and the recognition reaction between the nano particle, and making template have directive significance to assembling process, assembling process is more perfect.Selected template can be solid matrix, single or multiple lift film, organic molecule or biomolecule etc.The template of assemble nanometer particle also is the surfactant or the stabilizing agent of control nano particle growth under normal conditions, and the protection of template and restriction can obviously improve the stability of nanoparticle, obtains three-dimensional superlattices but be difficult to assembling with this kind method; Solvent evaporation method so all difficult control of this class assembling process is very strict to the requirement of assembling condition, needs to add stabilizing agent because in the assembling process a little less than the molecular recognition effect.
Summary of the invention
The present invention is for the method that solves existing templates method self-organized colloidal crystal is difficult to obtain three-dimensional superlattices and solvent evaporation method problem rambunctious, and the preparation method of noble metal self-organized colloidal crystal is provided.
The preparation method of noble metal self-organized colloidal crystal of the present invention carries out according to the following steps: one, compound concentration is 0.4%～0.6%(quality) HAuCl
4The aqueous solution also is placed on refrigerator and cooled but to 3 ℃～5 ℃, and compound concentration is 0.05%～0.2%(quality) AgNO
3The aqueous solution, concentration are 0.05%～0.2%(quality) sodium citrate aqueous solution; Two, measure the HAuCl for preparing through step 1 respectively
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution and water, wherein HAuCl
4The aqueous solution and AgNO
3The volume parts of the aqueous solution is than being 100:4～5, HAuCl
4The aqueous solution is 100:180～220, HAuCl with the volume parts ratio of sodium citrate aqueous solution
4The aqueous solution is 1:45～50 with the volume parts ratio of water; Three, will account for water 95%(volume earlier through step 2 takes by weighing) water join in the reactor with reflux, be heated to boiling, keep backflow 10min～15min; Four, under stirring condition, the HAuCl that will take by weighing through step 2
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution join the water 5%(volume that accounts for through step 2 takes by weighing) water in, join in the described reactor of step 3 after mixing 4min～6min, keep backflow 1h～1.5h, be cooled to then below 15 ℃, centrifugation, washing solid product obtain noble metal nano particles; Five, be 0.1%～0.5%(quality by noble metal nano particles concentration) take by weighing the noble metal nano particles and the solvent that obtain through step 4, after joining noble metal nano particles in the solvent, be placed in the ice-water bath, and then be placed on and handle 5min～15min in the ultrasonic cleaner, obtain the precious metal colloid suspension; Six, be 3:7 preparation washing lotion by the volume ratio of hydrogen peroxide and sulfuric acid, and substrate immersed keep 24h～48h in the washing lotion and then rinse well that oven dry obtains clean substrate with deionized water; Seven, will stand in through the substrate of the cleaning that step 6 obtains in the precious metal colloid suspension that step 5 obtains, and the precious metal colloid suspension placed on the hot platform, when the volume of precious metal colloid suspension reduces 70%～80%, take out substrate, obtain noble metal self-organized colloidal crystal, wherein the temperature of hot platform is the temperature that is lower than 20 ℃～30 ℃ of the boiling points of the solvent described in the step 5.
Solvent described in the step 5 is water, methyl alcohol or ethanol.
Substrate described in the step 6 is glass substrate or silicon chip.
It is spherical or subglobose monodisperse particle noble metal nano particles between 1nm～50nm that the present invention prepares particle size earlier, be prepared into homodisperse soliquid with noble metal nano particles again, at last substrate is put into this soliquid, the noble metal self assembly is deposited on the substrate, obtain noble metal self-organized colloidal crystal, this noble metal self-organized colloidal crystal presents the bar paten of rule, and has three-dimensional superlattice structure.The noble metal of the present invention's assembling is Jin Heyin, utilizes the gentle circulation of temperature, and preparation process is simple, control easily, and do not add surfactant in the preparation process of soliquid, cost is reduced.This noble metal self-organized colloidal crystal can be used for strengthening the polarization Raman.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the noble metal nano particles that obtains of the specific embodiment 18 step 4; Fig. 2 is the petrographic microscope photo of the noble metal self-organized colloidal crystal of the specific embodiment 18 preparations; The stereoscan photograph of the noble metal self-organized colloidal crystal of Fig. 3 specific embodiment 19 preparations.
The specific embodiment
The specific embodiment one: the preparation method of the noble metal self-organized colloidal crystal of present embodiment carries out according to the following steps: one, compound concentration is 0.4%～0.6%(quality) HAuCl
4The aqueous solution also is placed on refrigerator and cooled but to 3 ℃～5 ℃, and compound concentration is 0.05%～0.2%(quality) AgNO
3The aqueous solution, concentration are 0.05%～0.2%(quality) sodium citrate aqueous solution; Two, measure the HAuCl for preparing through step 1 respectively
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution and water, wherein HAuCl
4The aqueous solution and AgNO
3The volume parts of the aqueous solution is than being 100:4～5, HAuCl
4The aqueous solution is 100:180～220, HAuCl with the volume parts ratio of sodium citrate aqueous solution
4The aqueous solution is 1:45～50 with the volume parts ratio of water; Three, will account for water 95%(volume earlier through step 2 takes by weighing) water join in the reactor with reflux, be heated to boiling, keep backflow 10min～15min; Four, under stirring condition, the HAuCl that will take by weighing through step 2
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution join the water 5%(volume that accounts for through step 2 takes by weighing) water in, join in the described reactor of step 3 after mixing 4min～6min, keep backflow 1h～1.5h, be cooled to then below 15 ℃, centrifugation, washing solid product obtain noble metal nano particles; Five, be 0.1%～0.5%(quality by noble metal nano particles concentration) take by weighing the noble metal nano particles and the solvent that obtain through step 4, after joining noble metal nano particles in the solvent, be placed in the ice-water bath, and then be placed on and handle 5min～15min in the ultrasonic cleaner, obtain the precious metal colloid suspension; Six, be 3:7 preparation washing lotion by the volume ratio of hydrogen peroxide and sulfuric acid, and substrate immersed keep 24h～48h in the washing lotion and then rinse well that oven dry obtains clean substrate with deionized water; Seven, will stand in through the substrate of the cleaning that step 6 obtains in the precious metal colloid suspension that step 5 obtains, and the precious metal colloid suspension placed on the hot platform, when the volume of precious metal colloid suspension reduces 70%～80%, take out substrate, obtain noble metal self-organized colloidal crystal, wherein the temperature of hot platform is the temperature that is lower than 20 ℃～30 ℃ of the boiling points of the solvent described in the step 5.
Present embodiment elder generation preparation particle size is the spherical or subglobose monodisperse particle noble metal nano particles between 1nm～50nm, be prepared into homodisperse soliquid with noble metal nano particles again, at last substrate is put into this soliquid, the noble metal self assembly is deposited on the substrate, obtain noble metal self-organized colloidal crystal, this noble metal self-organized colloidal crystal presents the bar paten of rule, and has three-dimensional superlattice structure.The noble metal of present embodiment assembling is Jin Heyin, utilizes the gentle circulation of temperature, and preparation process is simple, control easily, and do not add surfactant in the preparation process of soliquid, cost is reduced.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the solvent described in the step 5 is water, methyl alcohol or ethanol.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is: the substrate described in the step 6 is glass substrate or silicon chip.Other is identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment was different with one of specific embodiment one to three is: the substrate described in the step 6 is glass substrate or silicon chip.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different with one of specific embodiment one to four is: compound concentration is 0.45%～0.55%(quality in the step 1) HAuCl
4The aqueous solution also is placed on refrigerator and cooled but to 3.5 ℃～4.5 ℃, and compound concentration is 0.07%～0.18%(quality) AgNO
3The aqueous solution, concentration are 0.07%～0.18%(quality) sodium citrate aqueous solution.Other is identical with one of specific embodiment one to four.
The specific embodiment six: what present embodiment was different with one of specific embodiment one to five is: compound concentration is the 0.50%(quality in the step 1) HAuCl
4The aqueous solution also is placed on refrigerator and cooled but to 4.0 ℃, and compound concentration is the 0.10%(quality) AgNO
3The aqueous solution, concentration are the 0.10%(quality) sodium citrate aqueous solution.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different with one of specific embodiment one to six is: HAuCl in the step 2
4The aqueous solution and AgNO
3The volume parts of the aqueous solution is than being 100:4.2～4.8, HAuCl
4The aqueous solution is 100:190～215, HAuCl with the volume parts ratio of sodium citrate aqueous solution
4The aqueous solution is 1:46～48 with the volume parts ratio of water.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different with one of specific embodiment one to seven is: HAuCl in the step 2
4The aqueous solution and AgNO
3The volume parts of the aqueous solution is than being 100:4.5, HAuCl
4The aqueous solution is 100:200, HAuCl with the volume parts ratio of sodium citrate aqueous solution
4The aqueous solution is 1:47 with the volume parts ratio of water.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different with one of specific embodiment one to eight is: keep backflow 11min～14min in the step 3.Other is identical with one of specific embodiment one to eight.
The specific embodiment ten: what present embodiment was different with one of specific embodiment one to nine is: keep backflow 12min in the step 3.Other is identical with one of specific embodiment one to nine.
The specific embodiment 11: what present embodiment was different with one of specific embodiment one to ten is: the return time in the step 4 is 1.1h～1.4h.Other is identical with one of specific embodiment one to ten.
The specific embodiment 11: what present embodiment was different with one of specific embodiment one to ten is: the return time in the step 4 is 1.3h.Other is identical with one of specific embodiment one to ten.
The specific embodiment 12: what present embodiment was different with one of specific embodiment one to 11 is: ultrasonic processing 6min～14min in the step 5.Other is identical with one of specific embodiment one to 11.
The specific embodiment 13: what present embodiment was different with one of specific embodiment one to 12 is: ultrasonic processing 10min in the step 5.Other is identical with one of specific embodiment one to 12.
The specific embodiment 14: what present embodiment was different with one of specific embodiment one to 13 is: in the step 6 substrate immersed and keep 26h～46h in the washing lotion.Other is identical with one of specific embodiment one to 13.
The specific embodiment 15: what present embodiment was different with one of specific embodiment one to 14 is: in the step 6 substrate immersed and keep 34h in the washing lotion.Other is identical with one of specific embodiment one to 14.
The specific embodiment 16: what present embodiment was different with one of specific embodiment one to 15 is: take out substrate in the step 7 when the volume of precious metal colloid suspension reduces 72%～78%.Other is identical with one of specific embodiment one to 15.
The specific embodiment 17: what present embodiment was different with one of specific embodiment one to 16 is: take out substrate in the step 7 when the volume of precious metal colloid suspension reduces 75%.Other is identical with one of specific embodiment one to 16.
The specific embodiment 18: the preparation method of the metal self-organized colloidal crystal of present embodiment carries out according to the following steps: one, compound concentration is the 0.5%(quality) HAuCl
4The aqueous solution also is placed on refrigerator and cooled but to 4 ℃, and compound concentration is the 0.1%(quality) AgNO
3The aqueous solution, concentration are the 0.1%(quality) sodium citrate aqueous solution; Two, measure the HAuCl for preparing through step 1 respectively
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution and water, wherein HAuCl
4The aqueous solution and AgNO
3The volume parts of the aqueous solution is than being 100:4.5, HAuCl
4The aqueous solution is 100:200, HAuCl with the volume parts ratio of sodium citrate aqueous solution
4The aqueous solution is 1:50 with the volume parts ratio of water; Three, will account for water 95%(volume earlier through step 2 takes by weighing) water join in the reactor with reflux, be heated to boiling, keep backflow 10min; Four, under stirring condition, the HAuCl that will take by weighing through step 2
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution join the water 5%(volume that accounts for through step 2 takes by weighing) water in, join in the described reactor of step 3 after mixing 5min, keep backflow 1h, be cooled to then below 15 ℃, centrifugation, washing solid product obtain noble metal nano particles; Five, be the 0.4%(quality by noble metal nano particles concentration) take by weighing the noble metal nano particles and the water that obtain through step 4, after noble metal nano particles is added to the water, be placed in the ice-water bath, and then be placed on and handle 10min in the ultrasonic cleaner, obtain the precious metal colloid suspension; Six, be 3:7 preparation washing lotion by the volume ratio of hydrogen peroxide and sulfuric acid, and substrate immersed keep 36h in the washing lotion, and then rinse well that oven dry obtains clean substrate with deionized water; Seven, will stand in through the substrate of the cleaning that step 6 obtains in the precious metal colloid suspension that step 5 obtains, and the precious metal colloid suspension placed on the hot platform, hot platform temperature is 80 ℃, when the volume of precious metal colloid suspension reduces 80%, take out substrate, obtain noble metal self-organized colloidal crystal.
Substrate described in the step 6 is a glass substrate.
The transmission electron microscope photo of the noble metal nano particles that present embodiment obtains through step 4 as shown in Figure 1, as can be seen from Figure 1, the noble metal nano particles that obtains through present embodiment four is for spherical, perhaps be approximately spherical, become single dispersed, no agglomeration, its average diameter is 25nm; The noble metal self-organized colloidal crystal that obtains through present embodiment the petrographic microscope photo as shown in Figure 2, as can be seen from Figure 2, noble metal self-organized colloidal crystal presents the bar paten of rule, and has three-dimensional superlattice structure.The width of every crystal is 40 μ m～60 μ m, and stripe pitch is 4 μ m～60 μ m; The noble metal of this noble metal self-organized colloidal crystal present embodiment assembling is Jin Heyin, utilizes the gentle circulation of temperature, and preparation process is simple, control easily, and do not add surfactant in the preparation process of soliquid, cost is reduced.
The specific embodiment 19: what present embodiment and the specific embodiment 18 were different is: the substrate described in the step 6 is a silicon chip.Other is identical with the specific embodiment 18.
The stereoscan photograph of the noble metal self-organized colloidal crystal that obtains through present embodiment as shown in Figure 3, as can be seen from Figure 3, noble metal self-organized colloidal crystal is arranged as bar shaped, the width 40 μ m～60um of every crystal, stripe pitch is 40 μ m～60um.The noble metal of this noble metal self-organized colloidal crystal present embodiment assembling is Jin Heyin, utilizes the gentle circulation of temperature, and preparation process is simple, control easily, and do not add surfactant in the preparation process of soliquid, cost is reduced.
Claims (10)
1. the preparation method of noble metal self-organized colloidal crystal, it is characterized in that the preparation method of noble metal self-organized colloidal crystal carries out according to the following steps: one, compound concentration is 0.4%～0.6%(quality) HAuCl
4The aqueous solution also is placed on refrigerator and cooled but to 3 ℃～5 ℃, and compound concentration is 0.05%～0.2%(quality) AgNO
3The aqueous solution, concentration are 0.05%～0.2%(quality) sodium citrate aqueous solution; Two, measure the HAuCl for preparing through step 1 respectively
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution and water, wherein HAuCl
4The aqueous solution and AgNO
3The volume parts of the aqueous solution is than being 100:4～5, HAuCl
4The aqueous solution is 100:180～220, HAuCl with the volume parts ratio of sodium citrate aqueous solution
4The aqueous solution is 1:45～50 with the volume parts ratio of water; Three, will account for water 95%(volume earlier through step 2 takes by weighing) water join in the reactor with reflux, be heated to boiling, keep backflow 10min～15min; Four, under stirring condition, the HAuCl that will take by weighing through step 2
4The aqueous solution, AgNO
3The aqueous solution, sodium citrate aqueous solution join the water 5%(volume that accounts for through step 2 takes by weighing) water in, join in the described reactor of step 3 after mixing 4min～6min, keep backflow 1h～1.5h, be cooled to then below 15 ℃, centrifugation, washing solid product obtain noble metal nano particles; Five, be 0.1%～0.5%(quality by noble metal nano particles concentration) take by weighing the noble metal nano particles and the solvent that obtain through step 4, after joining noble metal nano particles in the solvent, be placed in the ice-water bath, and then be placed on and handle 5min～15min in the ultrasonic cleaner, obtain the precious metal colloid suspension; Six, be 3:7 preparation washing lotion by the volume ratio of hydrogen peroxide and sulfuric acid, and substrate immersed keep 24h～48h in the washing lotion and then rinse well that oven dry obtains clean substrate with deionized water; Seven, will stand in through the substrate of the cleaning that step 6 obtains in the precious metal colloid suspension that step 5 obtains, and the precious metal colloid suspension placed on the hot platform, when the volume of precious metal colloid suspension reduces 70%～80%, take out substrate, obtain noble metal self-organized colloidal crystal, wherein the temperature of hot platform is the temperature that is lower than 20 ℃～30 ℃ of the boiling points of the solvent described in the step 5.
2. the preparation method of noble metal self-organized colloidal crystal according to claim 1 is characterized in that the solvent described in the step 5 is water, methyl alcohol or ethanol.
3. the preparation method of noble metal self-organized colloidal crystal according to claim 1 and 2 is characterized in that the substrate described in the step 6 is glass substrate or silicon chip.
4. the preparation method of noble metal self-organized colloidal crystal according to claim 3 is characterized in that compound concentration is 0.45%～0.55%(quality in the step 1) HAuCl
4The aqueous solution also is placed on refrigerator and cooled but to 3.5 ℃～4.5 ℃, and compound concentration is 0.07%～0.18%(quality) AgNO
3The aqueous solution, concentration are 0.07%～0.18%(quality) sodium citrate aqueous solution.
5. according to the preparation method of claim 1,2 or 4 described noble metal self-organized colloidal crystals, it is characterized in that HAuCl in the step 2
4The aqueous solution and AgNO
3The volume parts of the aqueous solution is than being 100:4.2～4.8, HAuCl
4The aqueous solution is 100:190～215, HAuCl with the volume parts ratio of sodium citrate aqueous solution
4The aqueous solution is 1:46～48 with the volume parts ratio of water.
6. the preparation method of noble metal self-organized colloidal crystal according to claim 5 is characterized in that keeping in the step 3 backflow 11min～14min.
7. according to the preparation method of claim 1,2,4 or 6 described noble metal self-organized colloidal crystals, it is characterized in that the return time in the step 4 is 1.1h～1.4h.
8. the preparation method of noble metal self-organized colloidal crystal according to claim 7 is characterized in that ultrasonic processing 6min～14min in the step 5.
9. according to the preparation method of claim 1,2,4,6 or 8 described noble metal self-organized colloidal crystals, it is characterized in that in the step 6 substrate immersed and keep 26h～46h in the washing lotion.
10. the preparation method of noble metal self-organized colloidal crystal according to claim 9 is characterized in that taking out in the step 7 substrate when the volume of precious metal colloid suspension reduces 72%～78%.
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| CN105170995A (en) * | 2015-09-21 | 2015-12-23 | 陕西师范大学 | Method for wrapping gold-silver alloy nanometer particles through silicon dioxide |
| CN108430676A (en) * | 2015-12-15 | 2018-08-21 | 意大利科技研究基金会 | The method for synthesizing metal nanoparticle in aqueous environment without using shape directed agents |
| CN105965029A (en) * | 2016-06-02 | 2016-09-28 | 山东大学 | Method for synthesizing water-soluble monodisperse spherical-like gold-silver alloy nano-particles |
| 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 |
| CN107498065A (en) * | 2017-09-06 | 2017-12-22 | 烟台智本知识产权运营管理有限公司 | The synthesis of gold size nano-particle |
| CN110316696A (en) * | 2019-04-01 | 2019-10-11 | 复旦大学 | A kind of method that can largely prepare binary superlattices lotion ball |
| CN114260461A (en) * | 2021-12-28 | 2022-04-01 | 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 |
| 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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