CN101148246B - Method for manufacturing nanometer level microporous mould - Google Patents
Method for manufacturing nanometer level microporous mould Download PDFInfo
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- CN101148246B CN101148246B CN2006100627225A CN200610062722A CN101148246B CN 101148246 B CN101148246 B CN 101148246B CN 2006100627225 A CN2006100627225 A CN 2006100627225A CN 200610062722 A CN200610062722 A CN 200610062722A CN 101148246 B CN101148246 B CN 101148246B
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Abstract
The making process of mold with nanometer level pores includes the following steps: providing carbon nanotubes, forming protecting layer in at least one end surface of each of the carbon nanotubes, injecting solution or melt for the base body into the carbon nanotubes with protecting layer and curing, eliminating the protecting layer to form one complex structure of carbon nanotubes and base body, and eliminating carbon nanotubes to form the mold with nanometer level pores.
Description
Technical field
The present invention relates to a kind of manufacture method of micropore mold, relate in particular to a kind of manufacture method of nanometer level microporous mould.
Background technology
Along with improving and the research and the progress of world's nanometer technology of quantum physics and quantum chemistry, the basic module of materials of construction can reach the level of single atom, atom can be dressed up nano level material according to certain group of paths, and such manufacturing is called the nanometer manufacturing.Mould manufacturing now develops to large-scale and super precise and tiny processing two aspects: aspect large-scale processing, for example make the flat extrusion die of automobile, aircraft usefulness large-scale integral wallboard, formed the manufacturing process of comparative maturity; And aspect super precise and tiny processing, the nanometer product demand becomes how much levels to rise, and how the nano-fabrication technique of application of advanced is in the mould manufacturing, makes the super precise and tiny development trend that is processed to form industrialization and is die industry synchronously with global mould advanced technology.
In theory, nanometer technology can be widely used in the processing aspect.Nanoprocessing mode based on the nanometer assembling has been proposed, to realize nanometer product automation, industrialization at present.This processing mode imagination is carried out molecules align according to the shape of product, thereby realizes the no mould mode of production.Yet, this method is in fact also infeasible, because that at present the arrangement of molecule is adopted mainly is PSTM (ScanningTunnelling Microscopy, STM) or AFM (Atomic Force Microscopy, AFM), its operation is meticulous, and cost is too high, is difficult to realize make on a large scale nanometer product.
Therefore, necessaryly provide a kind of manufacture method that is applicable to the nanometer level microporous mould of extensive manufacturing nanometer product.
Summary of the invention
Below, will a kind of manufacture method that is applicable to the nanometer level microporous mould of extensive manufacturing nanometer product be described with some embodiment.
A kind of manufacture method of nanometer level microporous mould, it may further comprise the steps: a plurality of CNTs are provided, and these a plurality of CNTs are a carbon nano pipe array; Two ends at described a plurality of CNTs form a protective layer respectively; Inject matrix solution or fused solution between the described a plurality of CNTs that are formed with protective layer, and it is solidified, described matrix solution or fused solution are the macromolecular compound of anti-strong acid corrosion; Remove protective layer, form the composite construction of CNT and matrix; And the removal CNT, form nanometer level microporous mould.
The carbon nano pipe array of these a plurality of CNTs for adopting chemical vapour deposition technique, plasma-assisted chemical vapour deposition method or plasma auxiliary heat wire chemical vapour deposition process to make.
This carbon nano pipe array is formed on the substrate.
The formation of this protective layer further may further comprise the steps: a bearing basement that is formed with pressure sensitive adhesive is provided; The one side that will be formed with pressure sensitive adhesive is pressed in carbon nano pipe array and forms a protective layer away from the end of substrate, and the substrate of carbon nano pipe array itself is as another protective layer.
The formation of this protective layer further may further comprise the steps: a bearing basement that is formed with pressure sensitive adhesive is provided; The one side that will be formed with pressure sensitive adhesive is pressed in carbon nano pipe array and forms a protective layer away from the end of substrate; Substrate is thrown off; Another bearing basement that is formed with pressure sensitive adhesive is provided, and this another pressure sensitive adhesive is pressed in carbon nano pipe array throws off an end of substrate and form another protective layer.
This bearing basement is a polyester sheet.
The thickness of this protective layer is 0.05 millimeter.
Before in the described CNT that is formed with protective layer, injecting matrix solution or fused solution, further comprise a step that vacuumizes in advance.
The removal method of described protective layer may further comprise the steps: throw off bearing basement, remove pressure sensitive adhesive with dimethylbenzene, ethyl acetate or petroleum ether dissolution.
Described CNT can adopt the solvent corrosion of highly acid or strong oxidizing property to remove, and forms nanometer level microporous mould.
The removal of described CNT further may further comprise the steps: adopting the mass percent concentration ratio is 3: 1 the concentrated sulfuric acid and the mixed solution of red fuming nitric acid (RFNA), when 60 degrees centigrade of environment temperatures, reflux in the composite construction of above-mentioned CNT and matrix 30 minutes to 2 hours, utilize the corrosiveness of strong acid solvent to remove CNT.
This matrix material is polytetrafluoroethylene (PTFE), silicon rubber, polyester, polyvinyl chloride, polyvinyl alcohol, polyethylene, polypropylene, epoxy resin, Merlon, polyformaldehyde or polyacetals.
Compared to prior art, the manufacture method processing procedure of described nanometer level microporous mould is simple, processing ease, and cost is low, is easy to large-scale practical application.
Description of drawings
Fig. 1 is the schematic flow sheet of the manufacture method of embodiment of the invention nanometer level microporous mould.
Fig. 2 is the structural representation of embodiment of the invention nanometer level microporous mould.
Fig. 3 is the application schematic diagram of embodiment of the invention nanometer level microporous mould.
The specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing.
See also Fig. 1, the manufacture method of embodiment of the invention nanometer level microporous mould 10 mainly comprises following step:
(1) provides a plurality of CNTs 14.
A plurality of CNTs 14 may be selected to be many walls or single-wall carbon nanotube array in the present embodiment, it can adopt chemical vapour deposition technique, plasma-assisted chemical vapour deposition method or plasma auxiliary heat wire chemical vapour deposition process to make, thereby, a plurality of CNTs 14 are formed on the substrate 12 usually, and this substrate 12 can be taken off easily, and does not influence the array of CNT.
The present embodiment carbon nano pipe array growth method comprises: at first at the metallic iron catalyst layer of a silicon substrate 12 surface-coated one about 5 nano thickness; Under 300 ℃ of temperature, in air, heat-treat; Then under 700 ℃ of temperature, chemical vapor deposition growth carbon nano pipe array on silicon substrate 12, the diameter range of CNT 14 is 1～100 nanometer in this array.
(2) at described CNT 14 at least one terminal protective layers 16 that form.
At first on a bearing basement 162, evenly smear one deck pressure sensitive adhesive 164; Then pressure sensitive adhesive 164 is pressed in a plurality of CNTs 14 ends away from silicon substrate 12; promptly form an end and be coated with protective layer 16 CNT 14 of (comprising bearing basement 162 and pressure sensitive adhesive 164); at this moment, silicon substrate 12 itself can be used as another protective layer of CNT 14.In addition; also can all form protective layer 16 in the present embodiment at CNT 14 two ends; particularly; after can further silicon substrate 12 being taken off; repeat above-mentioned steps again; the end of the CNT 14 that exposes after silicon substrate 12 is taken off is protective mulch 16 also, and this protective layer 16 comprises pressure sensitive adhesive 164 and bearing basement 162 equally, thereby forms the two terminal CNTs 14 of protective mulch 16 respectively.In the present embodiment, above-mentioned bearing basement 162 can adopt polyester sheet, and pressure sensitive adhesive 164 can adopt the YM881 type pressure sensitive adhesive of being produced by Fushun light industry.In addition, protective layer 16 thickness are preferably 0.05 millimeter in the present embodiment.
(3) inject matrix 18 solution or fused solution at described 14 of a plurality of CNTs that are formed with protective layer 16, and make its curing.
To immerse in matrix 18 solution or the fused solution through the CNT 14 that step (two) is handled; or matrix solution or matrix fused solution injected the CNT 14 that two ends are formed with protective layer 16; then it is solidified under vacuum or solidified 24 hours, obtain to be marked with the CNT 14 of matrix 18.Wherein, matrix 18 is chosen as the macromolecular compound of ability strong acid corrosion, and is concrete optional from macromolecular materials such as polytetrafluoroethylene (PTFE), silicon rubber, polyester, polyvinyl chloride, polyvinyl alcohol, polyethylene, polypropylene, epoxy resin, Merlon, polyformaldehyde, polyacetals.Be preferably polytetrafluoroethylene (PTFE) in the present embodiment.
In addition; present embodiment step (three) can further comprise a step that vacuumizes in advance; can do to vacuumize by a plurality of CNTs 14 that in advance this are formed with protective layer 16 and handle about 30 minutes,, help matrix 18 solution or fused solution and inject to discharge the air of 14 of a plurality of CNTs.
(4) remove protective layer 16.
Bearing basement 162 in the protective layer 16 can directly be thrown off, and pressure sensitive adhesive 164 can dissolve removal then, as adopting dimethylbenzene, ethyl acetate or petroleum ether dissolution.In addition, in the present embodiment with the silicon substrate 12 of carbon nano-tube 14 as protective layer can directly throw off.At this moment, expose matrix 18 first surface 182 and with its opposing second surface 184, and two ends of the CNT 14 that covered of original protected seam 16 also expose, and stretch out two surfaces 182,184 of matrix 18 respectively.Thereby removing protective layer 16 backs formed is that two ends expose the CNT 14 on matrix 18 surfaces and the composite construction of matrix 18.
(5) CNT 14 in the above-mentioned composite construction is removed in corrosion.
The solvent corrosion of present embodiment employing highly acid or strong oxidizing property is removed the CNT 14 in the above-mentioned composite construction.Preferably, it is 3: 1 the concentrated sulfuric acid and the mixed solution of red fuming nitric acid (RFNA) that present embodiment adopts the mass percent concentration ratio, when 60 degrees centigrade of environment temperatures, refluxed in the composite construction of above-mentioned CNT 14 and matrix 18 about 30 minutes to 2 hours, and utilized the corrosiveness of strong acid solvent to remove CNT 14 in the composite construction.Erode after the CNT, the matrix 18 with anti-strong acid corrosion stays and forms a nanometer level microporous mould 10.
See also Fig. 2, the nanometer level microporous mould 10 that the embodiment of the invention is made comprises a matrix 18, and this matrix 18 is a film, and it further comprises a first surface 182 and and first surface 182 opposing second surface 184.Be distributed with a plurality of nano level through holes 186 that are arranged mutually parallel in this matrix 18.These a plurality of through holes 186 are basically perpendicular to the first surface 182 and the second surface 184 of matrix 18, and extend through whole substrate 18 along first surface 182 to second surface 184.In the present embodiment, the hole diameter of this through hole 186 is 1～100 nanometer, and the spacing between the through hole 186 is 20～200 nanometers, and the thickness of this nanometer level microporous mould 10 is 0.1～1 millimeter.
See also Fig. 3, the application schematic diagram of the nanometer level microporous mould of making for present embodiment 10.The nanometer level microporous mould 10 of present embodiment can be used for making the nanoscale arrays of other materials.
At first, fill the material of a nanoscale arrays to be formed in above-mentioned nanometer level microporous mould 10, present embodiment is example with the gold.
Secondly, remove above-mentioned nanometer level microporous mould 10, promptly form the nano level array 20 of this material.
In the present embodiment, this nanometer level microporous mould 10 is a macromolecular material, can remove this nanometer level microporous mould 10 by methods such as chemical attack, high-temperature calcinations, forms nano level golden array 20.
In addition, present embodiment nanometer level microporous mould 10 also can be applicable to stamping technique, forms nano level rat structure at material surface.
Compared to prior art, the manufacture method of present embodiment nanometer level microporous mould is owing to used carbon nano pipe array to be used as motherboard, the high directionality of CNT has obtained reservation, and arrangement by the control carbon nano-tube catalyst, can obtain the hole of different queueing disciplines, reach the purpose of accurate control hole location, improved the order and the controllability of mould.
In addition, those skilled in the art also can do other variations in spirit of the present invention, and certainly, the variation that these are done according to spirit of the present invention all should be included within the present invention's scope required for protection.
Claims (12)
1. the manufacture method of a nanometer level microporous mould, it may further comprise the steps:
A plurality of CNTs are provided, and these a plurality of CNTs are a carbon nano pipe array;
Two ends at described a plurality of CNTs form a protective layer respectively;
Inject matrix solution or fused solution between the described a plurality of CNTs that are formed with protective layer, and it is solidified, described matrix solution or fused solution are the macromolecular compound of anti-strong acid corrosion;
Remove protective layer, form the composite construction of CNT and matrix; And
Remove CNT, form nanometer level microporous mould.
2. the manufacture method of nanometer level microporous mould as claimed in claim 1, it is characterized in that the carbon nano pipe array of these a plurality of CNTs for adopting chemical vapour deposition technique, plasma-assisted chemical vapour deposition method or plasma auxiliary heat wire chemical vapour deposition process to make.
3. the manufacture method of nanometer level microporous mould as claimed in claim 2 is characterized in that, this carbon nano pipe array is formed on the substrate.
4. the manufacture method of nanometer level microporous mould as claimed in claim 3 is characterized in that, the formation of this protective layer further may further comprise the steps: a bearing basement that is formed with pressure sensitive adhesive is provided; The one side that will be formed with pressure sensitive adhesive is pressed in carbon nano pipe array and forms a protective layer away from the end of substrate, and the substrate of carbon nano pipe array itself is as another protective layer.
5. the manufacture method of nanometer level microporous mould as claimed in claim 3 is characterized in that, the formation of this protective layer further may further comprise the steps: a bearing basement that is formed with pressure sensitive adhesive is provided; The one side that will be formed with pressure sensitive adhesive is pressed in carbon nano pipe array and forms a protective layer away from the end of substrate; Substrate is thrown off; Another bearing basement that is formed with pressure sensitive adhesive is provided, and this another pressure sensitive adhesive is pressed in carbon nano pipe array throws off an end of substrate and form another protective layer.
6. as the manufacture method of claim 4 or 5 described nanometer level microporous moulds, it is characterized in that this bearing basement is a polyester sheet.
7. the manufacture method of nanometer level microporous mould as claimed in claim 1 is characterized in that, the thickness of this protective layer is 0.05 millimeter.
8. the manufacture method of nanometer level microporous mould as claimed in claim 1 is characterized in that, inject matrix solution or fused solution between the described a plurality of CNTs that are formed with protective layer before, further comprises a step that vacuumizes in advance.
9. as the manufacture method of claim 4 or 5 described nanometer level microporous moulds, it is characterized in that the removal method of described protective layer may further comprise the steps: throw off bearing basement, remove pressure sensitive adhesive with dimethylbenzene, ethyl acetate or petroleum ether dissolution.
10. the manufacture method of nanometer level microporous mould as claimed in claim 1 is characterized in that, described CNT can adopt the solvent corrosion of highly acid or strong oxidizing property to remove, and forms nanometer level microporous mould.
11. the manufacture method of nanometer level microporous mould as claimed in claim 10, it is characterized in that, the removal of described CNT further may further comprise the steps: adopting the mass percent concentration ratio is 3: 1 the concentrated sulfuric acid and the mixed solution of red fuming nitric acid (RFNA), when 60 degrees centigrade of environment temperatures, reflux in the composite construction of above-mentioned CNT and matrix 30 minutes to 2 hours, utilize the corrosiveness of strong acid solvent to remove CNT.
12. the manufacture method of nanometer level microporous mould as claimed in claim 1, it is characterized in that this matrix material is polytetrafluoroethylene (PTFE), silicon rubber, polyester, polyvinyl chloride, polyvinyl alcohol, polyethylene, polypropylene, epoxy resin, Merlon, polyformaldehyde or polyacetals.
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| CN2006100627225A CN101148246B (en) | 2006-09-22 | 2006-09-22 | Method for manufacturing nanometer level microporous mould |
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| CN2006100627225A CN101148246B (en) | 2006-09-22 | 2006-09-22 | Method for manufacturing nanometer level microporous mould |
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| CN101148246B true CN101148246B (en) | 2011-01-26 |
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| CN1467311A (en) * | 2002-06-19 | 2004-01-14 | ���ǵ�����ʽ���� | Method of manufacturing inorganic nanotube |
| CN1609283A (en) * | 2003-10-21 | 2005-04-27 | 东莞理工学院 | Preparation method of ordered porous anodic alumina template |
| CN1699452A (en) * | 2004-05-19 | 2005-11-23 | 中国航空工业第一集团公司北京航空材料研究院 | High volume fraction carbon nanotube array - resin base composite materials and method for preparing same |
| US20050276743A1 (en) * | 2004-01-13 | 2005-12-15 | Jeff Lacombe | Method for fabrication of porous metal templates and growth of carbon nanotubes and utilization thereof |
| CN1786054A (en) * | 2004-12-12 | 2006-06-14 | 青岛大学 | Method of preparing small caliber polymer nano-tube by universal polymer and physical method |
| CN1803586A (en) * | 2005-12-19 | 2006-07-19 | 广东工业大学 | Method for preparing silicon nitride nanowire by utilizing carbon nanotube template method |
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2006
- 2006-09-22 CN CN2006100627225A patent/CN101148246B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1467311A (en) * | 2002-06-19 | 2004-01-14 | ���ǵ�����ʽ���� | Method of manufacturing inorganic nanotube |
| CN1609283A (en) * | 2003-10-21 | 2005-04-27 | 东莞理工学院 | Preparation method of ordered porous anodic alumina template |
| US20050276743A1 (en) * | 2004-01-13 | 2005-12-15 | Jeff Lacombe | Method for fabrication of porous metal templates and growth of carbon nanotubes and utilization thereof |
| CN1699452A (en) * | 2004-05-19 | 2005-11-23 | 中国航空工业第一集团公司北京航空材料研究院 | High volume fraction carbon nanotube array - resin base composite materials and method for preparing same |
| CN1786054A (en) * | 2004-12-12 | 2006-06-14 | 青岛大学 | Method of preparing small caliber polymer nano-tube by universal polymer and physical method |
| CN1803586A (en) * | 2005-12-19 | 2006-07-19 | 广东工业大学 | Method for preparing silicon nitride nanowire by utilizing carbon nanotube template method |
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| CI01 | Publication of corrected invention patent application |
Correction item: Patentee|Address|Co-patentee Correct: Tsinghua University|100084 Tsinghua Foxconn nanometer science and technology research center, Tsinghua University, Beijing, Haidian District 310|Hongfujin Precision Industry (Shenzhen) Co., Ltd. False: Hongfujin Precision Industry (Shenzhen) Co., Ltd.|518109 Guangdong city of Shenzhen province Baoan District Longhua Town Industrial Zone tabulaeformis tenth East Ring Road No. 2 two Number: 04 Volume: 27 |
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| CI03 | Correction of invention patent |
Correction item: Patentee|Address|Co-patentee Correct: Tsinghua University|100084 Tsinghua Foxconn nanometer science and technology research center, Tsinghua University, Beijing, Haidian District 310|Hongfujin Precision Industry (Shenzhen) Co., Ltd. False: Hongfujin Precision Industry (Shenzhen) Co., Ltd.|518109 Guangdong city of Shenzhen province Baoan District Longhua Town Industrial Zone tabulaeformis tenth East Ring Road No. 2 two Number: 04 Page: The title page Volume: 27 Correction item: Patentee|Address|Co-patentee Correct: Tsinghua University|100084 Haidian District Tsinghua Tsinghua University - Foxconn nanotechnology research center room,, Beijing|Hongfujin Precision Industry (Shenzhen) Co., Ltd. False: Hongfujin Precision Industry (Shenzhen) Co., Ltd.|518109 Guangdong city of Shenzhen province Baoan District Longhua Town Industrial Zone tabulaeformis tenth East Ring Road No. 2 two Number: 04 Page: The title page Volume: 27 |
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Free format text: CORRECT: PATENTEE; ADDRESS; CO-PATENTEE; FROM: HONGFUJIN PRECISION INDUSTRY (SHENZHEN) CO., LTD.;518109 NO. 2, EAST RING 2ND ROAD, YOUSONG 10TH INDUSTRIAL ZONE, LONGHUA TOWN, BAOAN DISTRICT, SHENZHEN CITY, GUANGDONG PROVINCE TO: TSINGHUA UNIVERSITY;100084 310#, TSINGHUA-FOXCONN NANOTECHNOLOGY RESEARCH CENTER, TSINGHUA UNIVERSITY, HAIDIAN DISTRICT, BEIJING; HONGFUJIN PRECISION INDUSTRY (SHENZHEN) CO., LTD. |