CN1751983A - Non close parked metal hollow ball shell ordered network structure material and its making method - Google Patents
Non close parked metal hollow ball shell ordered network structure material and its making method Download PDFInfo
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- CN1751983A CN1751983A CN200510094918.8A CN200510094918A CN1751983A CN 1751983 A CN1751983 A CN 1751983A CN 200510094918 A CN200510094918 A CN 200510094918A CN 1751983 A CN1751983 A CN 1751983A
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- ordered network
- metal hollow
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- 239000002184 metal Substances 0.000 title claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 title claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 20
- 239000004793 Polystyrene Substances 0.000 claims abstract description 18
- 229920002223 polystyrene Polymers 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 3
- 239000011805 ball Substances 0.000 claims description 26
- 229910052755 nonmetal Inorganic materials 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 15
- 238000009938 salting Methods 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002082 metal nanoparticle Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 238000005234 chemical deposition Methods 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000013528 metallic particle Substances 0.000 claims description 3
- 239000011806 microball Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 238000000137 annealing Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 238000005530 etching Methods 0.000 claims description 2
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical group [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical group OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 19
- 230000001413 cellular effect Effects 0.000 abstract 1
- 210000003850 cellular structure Anatomy 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000011257 shell material Substances 0.000 description 23
- 238000005516 engineering process Methods 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000004794 expanded polystyrene Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- -1 size Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
A cellular material is composed of the hollow metallic balls which are orderly arranged in the pipes made of the same metal as said hollow metallic ball. Its preparing process includes such steps as making a template of said cellular structure, copying it by polystyrene to obtain a secondary template, immersing it in a mixture of metal salt solution and reducer solution, chemical depositing to generate continuous metallic film in the pores of polystyrene and removing polystyrene.
Description
One, technical field
The present invention relates to a kind of non close parked metal hollow ball shell ordered network structure material and method for making thereof.
Two, background technology
Metal nanoparticle has direct and potential using value at aspects such as photonic propulsion, catalysis, biomedicine, drug delivery, electronics, has therefore obtained extensive concern both domestic and external and research.The shape of metal nanoparticle, size, composition and structures shape their character.For example, the ordered structure of metal nanoparticle can produce the surface phasmon concussion, and this character can be applicable to bioscience and photonic propulsion.Therefore development of new metal nano ordered structural material and realize that its controllable parameters is necessary with the application that adapts to different field.
Three, summary of the invention
1, goal of the invention: the objective of the invention is to utilize improved secondary template duplicating technology and in conjunction with the method for wet-chemical deposition, and a kind of sub-micron/micron non close parked metal hollow ball shell ordered network structure and method for making thereof of controllable parameters is provided.
2, technical scheme: non close parked metal hollow ball shell ordered network structure material of the present invention, it is characterized in that it has the hollow metal spherical shell of orderly arrangement, link to each other by the hollow metal pipeline between the adjacent spherical shell, formed non-close stacking order network structure.
The preparation method of non close parked metal hollow ball shell ordered network structure of the present invention may further comprise the steps:
(1) on quartz substrate, arranges the nonmetal microballoon of sub-micron/micron by self-assembling technique, obtain the two dimension or the cubical array of large tracts of land high-sequential, handle through high annealing and chemical attack then, form the nonmetal microballoon ordered network structure of non-Mi Dui; Wherein self-assembling technique belongs to known technology, this patent can adopt applicant formerly a patent No. be the disclosed technology of ZL031319890;
(2) utilize the mode of sputter or the mode of thermal evaporation, the metal nanoparticle that 5～8nm is thick is deposited on the surface of nonmetal microballoon;
(3) toluene solution that will contain polystyrene is filled into the gap that surface deposition has the nonmetal microballoon ordered network structure of metal nanoparticle, remove nonmetal microballoon with chemical corrosion method then, thereby the ordered network structure of non-Mi Dui is copied on the polystyrene moulding;
(4) polystyrene moulding of porous is put into the metallic growth solution that contains main salting liquid and reductant solution, these two kinds of solution mix according to certain volume ratio, through chemical deposition, metallic particles preferred growth in the hole of template, form uniform, continuous metallic film, utilize chemical corrosion method to remove polystyrene at last.
In step (1), said sub-micron/nonmetal diameter of micro ball of micron is 200nm～10 μ m; The temperature of The high temperature anneal is 950～1000 ℃; The etching time that chemical attack is handled is 10～20min.
In the step (4), the mixing according to a certain percentage of said metallic growth mixed solution by main salting liquid and reductant solution.Wherein main salting liquid consists of slaine 1%～5%, additive 0.1%～1%, solvent 94%～98%; Reductant solution consist of reducing agent 1%～12%, additive 0～18%, solvent 80%～99%; The volume ratio of main salting liquid and reductant solution is 1: 1～5: 1.
Preparation method of the present invention mainly adopts improved secondary template method.At first with the nonmetal microballoon ordered network structure of non-Mi Dui as a template; Utilize polystyrene that the structure of a template is duplicated then, form the expanded polystyrene secondary template; Again secondary template is put into the mixed solution of forming by slaine and reducing agent,, in the polystyrene hole, formed continuous metal film by chemical deposition; Remove polystyrene moulding at last, promptly obtain sub-micron/micron non close parked metal hollow ball shell ordered network structure material.
3, beneficial effect: the present invention compared with prior art has following outstanding advantage: (1) structural parameters can be controlled, and the diameter of spherical shell and the size of pipeline can be controlled, and comprise that cycle of structure and dutycycle etc. all can control; (2) sample degree of order height can carry out certain optical measurement; (3) monodispersity of metal spherical shell size is good, and it is even to obtain metal-back by chemical deposition, densification, purity height; (4) technology is simple, and is less demanding to equipment, with low cost.
Four, description of drawings
Fig. 1 is the scanning electricity border figure of two-dimentional non close parked metal hollow ball shell ordered network structure.
Fig. 2 is the scanning electricity border figure of three-dimensional non close parked metal hollow ball shell ordered network structure.
Five, the specific embodiment
Embodiment 1: selected sub-micron/nonmetal microballoon of micron is a silicon dioxide microsphere, and diameter of micro ball is 1550nm; Main salting liquid is gold chloride 1.2%, sodium chloride 0.6%, deionized water 98.2%; Reductant solution is tartaric acid 1.3%, NaOH 17.6%, absolute ethyl alcohol 22.3%, deionized water 58.8%.
The non close parked metal hollow ball shell ordered network structure material of the present invention preparation has the hollow metal spherical shell of orderly arrangement, is linked to each other by the hollow metal pipeline between the adjacent spherical shell, has formed non-close stacking order network structure.This example Metal Ball shell material is a gold, and the average diameter of hollow gold goal shell is 1295 ± 8nm, and the average length of hollow golden pipeline is 180 ± 5nm, and the average diameter of golden pipeline is 185 ± 6nm.
Nanometer non close parked metal hollow ball shell ordered network structure preparation methods is:
1, the preparation of the nonmetal microballoon ordered network structure of non-Mi Dui.Arrange nonmetal microballoon by self-assembling technique on quartz substrate, obtain the two dimension (or cubical array) of large tracts of land high-sequential, pass through The high temperature anneal then, temperature is 950 ℃, and the time is 3h; Use 1% hydroflouric acid solution corrosion 15min then, form the nonmetal microballoon ordered network structure of non-Mi Dui.
2, utilize the mode (or mode of sputter) of thermal evaporation, the gold nano grain that 5～8nm is thick is deposited on the surface of nonmetal microballoon.
3, the preparation of expanded polystyrene template.Promptly be filled into the gap of nonmetal microballoon ordered network structure by the toluene solution that will contain polystyrene, utilize 10% hydrofluoric acid aqueous acid to remove nonmetal microballoon then, the ordered network structure with non-Mi Dui copies on the polystyrene moulding by this method.
4, the polystyrene moulding of porous is put into the metallic growth solution that contains main salting liquid and reductant solution, these two kinds of solution mix according to volume ratio at 10: 3, through chemical deposition, metallic particles preferred growth in the hole of template, form uniform, continuous gold thin film, utilize chemical corrosion method to remove polystyrene at last.
Embodiment 2: present embodiment is substantially the same with embodiment 1 described non close parked metal hollow ball shell ordered network structure material and preparation method, but the volume ratio of selected main salting liquid and reductant solution is 5: 2.
Embodiment 3: present embodiment is substantially the same with embodiment 1 described non close parked metal hollow ball shell ordered network structure material and preparation method, but selected main salting liquid is silver nitrate 3.3%, ammoniacal liquor 0.7%, deionized water 96%; Reductant solution is formaldehyde 1.1%, absolute ethyl alcohol 95%, deionized water 3.9%.Main salting liquid is mixed according to volume ratio with reductant solution at 1: 1.Therefore formed sub-micron/micron non close parked metal silver hollow ball shell ordered network structure.
Embodiment 4: present embodiment is substantially the same with embodiment 1 described non close parked metal hollow ball shell ordered network structure material and preparation method, but selected main salting liquid is silver nitrate 5%, ammoniacal liquor 0.9%, deionized water 94.1%; Reductant solution is formaldehyde 11.9%, absolute ethyl alcohol 28.4%, deionized water 59.7%.Main salting liquid is mixed according to volume ratio with reductant solution at 5: 1.Therefore formed sub-micron/micron non close parked metal silver hollow ball shell ordered network structure.
Claims (10)
1, a kind of non close parked metal hollow ball shell ordered network structure material is characterized in that it has the metal hollow ball shell of orderly arrangement, is linked to each other by the metal hollow pipeline between the adjacent spherical shell, forms non-close stacking order network structure.
2, the described non close parked metal hollow ball shell ordered network structure preparation methods of claim 1 is characterized in that this method may further comprise the steps:
(1) on quartz or silicon substrate, arranges the nonmetal microballoon of sub-micron/micron by self-assembling technique, obtain the two dimension or the cubical array of large tracts of land high-sequential, handle through high annealing and chemical attack then, form the nonmetal microballoon ordered network structure of non-Mi Dui;
(2) utilize the mode of sputter or the mode of thermal evaporation, the metal nanoparticle that 5～8nm is thick is deposited on the surface of nonmetal microballoon;
(3) toluene solution that will contain polystyrene is filled into the gap that surface deposition has the nonmetal microballoon ordered network structure of metal nanoparticle, remove nonmetal microballoon with chemical corrosion method then, thereby the ordered network structure of non-Mi Dui is copied on the polystyrene moulding;
(4) polystyrene moulding of porous is put into the metallic growth solution that contains main salting liquid and reductant solution, these two kinds of solution mix according to certain volume ratio, through chemical deposition, metallic particles preferred growth in the hole of template, form uniform, continuous metallic film, utilize chemical corrosion method to remove polystyrene at last.
3, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 2 is characterized in that in step (1), and said sub-micron/nonmetal diameter of micro ball of micron is 200nm～10 μ m.
4, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 2 is characterized in that in step (1), the temperature of The high temperature anneal is 950～1000 ℃.
5, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 2 is characterized in that in step (1), and the etching time that chemical attack is handled is 10～20min.
6, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 2, it is characterized in that in step (4), said main salting liquid consist of slaine 1%～5%, additive 0.1%～1%, solvent 94%～98%.
7, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 2, it is characterized in that in step (4), said reductant solution consist of reducing agent 1%～12%, additive 0～18%, solvent 80%～99%.
8, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 6 is characterized in that slaine is gold chloride or silver nitrate in the composition of main salting liquid; Additive is sodium chloride or ammoniacal liquor; Solvent is a deionized water.
9, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 7 is characterized in that reducing agent is tartaric acid or formaldehyde in the composition of reductant solution; Additive is a NaOH; Solvent is absolute ethyl alcohol and deionized water, and volume ratio between the two is 3: 10～25: 1.
10, non close parked metal hollow ball shell ordered network structure preparation methods according to claim 2 is characterized in that in step (4), the volume ratio of said main salting liquid and reductant solution is 1: 1～5: 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100494045C (en) * | 2007-03-19 | 2009-06-03 | 南京大学 | Method for preparing micron/submicron metal ring and open-mouth metal ring |
| CN102167278A (en) * | 2010-02-26 | 2011-08-31 | 中国科学院合肥物质科学研究院 | Zinc oxide micro/nano composite structure array film and preparation method thereof |
| CN103043597A (en) * | 2011-10-13 | 2013-04-17 | 聊城大学 | Method for preparing metal micro-nano array electrode by using ZnO crystal as template |
| CN109518162A (en) * | 2018-12-18 | 2019-03-26 | 同济大学 | A kind of preparation method of bionical net mitochondrial structure thin-film material |
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| JP3277233B2 (en) * | 1990-07-18 | 2002-04-22 | ジ・オーストラリアン・ナショナル・ユニバーシティー | Formation of porous material |
| WO2002033461A2 (en) * | 2000-10-16 | 2002-04-25 | Ozin Geoffrey A | Method of self-assembly and optical applications of crystalline colloidal patterns on substrates |
| CN1136954C (en) * | 2001-12-07 | 2004-02-04 | 华南理工大学 | Process for preparing colloid crystal with ordered 3D structure |
| US20030129311A1 (en) * | 2002-01-10 | 2003-07-10 | Wen-Chiang Huang | Method of producing quantum-dot powder and film via templating by a 2-d ordered array of air bubbles in a polymer |
| CN1216678C (en) * | 2003-06-25 | 2005-08-31 | 南京大学 | Capillary attration colloidal microball self-organization and two-dimensional, three-dimensional colloidal crystal preparing method |
| CN100359030C (en) * | 2003-07-28 | 2008-01-02 | 南京大学 | Ordered 2D and 3D nano structure metal material comprising hollow metal spheres and its prepn process |
| CN1290759C (en) * | 2003-12-23 | 2006-12-20 | 南开大学 | Magnetic hetero nano fiber self assembling super crystal lattice structure material and its preparing method |
| CN1289180C (en) * | 2004-09-10 | 2006-12-13 | 南京大学 | Method for preparing two-dimensional or three dimensional colloid crystal |
| CN1286711C (en) * | 2005-03-09 | 2006-11-29 | 吉林大学 | Method for constructing non-close packing colloid balls ordered arrangement using soft-graving technology |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100494045C (en) * | 2007-03-19 | 2009-06-03 | 南京大学 | Method for preparing micron/submicron metal ring and open-mouth metal ring |
| CN102167278A (en) * | 2010-02-26 | 2011-08-31 | 中国科学院合肥物质科学研究院 | Zinc oxide micro/nano composite structure array film and preparation method thereof |
| CN102167278B (en) * | 2010-02-26 | 2013-11-27 | 中国科学院合肥物质科学研究院 | Zinc oxide micro/nano composite structure array film and preparation method thereof |
| CN103043597A (en) * | 2011-10-13 | 2013-04-17 | 聊城大学 | Method for preparing metal micro-nano array electrode by using ZnO crystal as template |
| CN103043597B (en) * | 2011-10-13 | 2015-05-20 | 聊城大学 | Method for preparing metal micro-nano array electrode by using ZnO crystal as template |
| CN109518162A (en) * | 2018-12-18 | 2019-03-26 | 同济大学 | A kind of preparation method of bionical net mitochondrial structure thin-film material |
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