CN104229729A - Method for transferring carbon nanotube vertical array to flexible polymer substrate - Google Patents
Method for transferring carbon nanotube vertical array to flexible polymer substrate Download PDFInfo
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- CN104229729A CN104229729A CN201410413702.2A CN201410413702A CN104229729A CN 104229729 A CN104229729 A CN 104229729A CN 201410413702 A CN201410413702 A CN 201410413702A CN 104229729 A CN104229729 A CN 104229729A
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Abstract
The invention discloses a method for transferring a carbon nanotube vertical array to a flexible polymer substrate. The method comprises the steps: firstly, preparing the carbon nanotube vertical array by adopting a chemical vapor deposition method, performing heating oxidation treatment to obtain the carbon nanotube vertical array which is easy to disconnect from a growth substrate, mechanically stripping the array so that the bottom end or the top end of the array is respectively contacted with the flexible polymer substrate, heating under certain pressure so that the polymer substrate is softened to permeate into the carbon nanotube array, cooling, solidifying, and then transferring the array to the polymer substrate, wherein any transferring medium such as an adhesive is not needed between the array and the polymer substrate, and top patterns of an original array can be kept.
Description
Technical field
The present invention relates to the application of CNT, specifically a kind of vertical carbon nanotube array and growth substrate of making departs from and is transferred to the method in flexible polymer substrate.
Background technology
Since the discovery of CNT, the one dimension tubular structure of its uniqueness, high draw ratio, and the characteristic such as the mechanical property of excellence, electric-conductivity heat-conductivity high causes the interest of many scientific research personnel and extensively studies, its wide application prospect also constantly shows.In recent years, scientists is attempted with nano material development bionic gecko pin, and the carbon nano pipe array of vertical orientation is similar to gecko sole bristle configurations, is the first material of imitative gecko sole bristle.
At present, prepare vertical (VA-CNTs) array of CNT and mainly adopt chemical vapour deposition technique, by Controlling Technology parameter, the array that high density arrays, length are controlled can be obtained respectively, and single wall or multi-walled carbon nano-tubes orthogonal array.And silicon is considered to the substrate being best suited for CNT vertical oriented growth, but in fragility at the bottom of rigid silicone matrix, the VA-CNTs array grown thereon is as the surperficial bad adaptability of dry adhesion material, and the problem such as array and the weak adhesion of growth substrate all governs the development of VA-CNTs array in imitative gecko sole bristle field.So transfer VA-CNTs array is one of key technology overcome the above problems to flexible substrate.
Technique simple gluing method can realize vertical carbon nanotube array to be transferred to (Zhu Y in the target substrate of various material, et al. Nanotechnology, 2008,19 (32): 325304.), adhesive, as the intermediate medium between array and target substrate, brings new interface problem; For large area, the transfer of highly less array, occur that transfer is imperfect, transfer efficiency is low; In addition, the solvent of preparation required for adhesive can cause CNT to shrink, thus the overall pattern of destroying carbon nanometer tube orthogonal array.The people such as Tsai (T. Y. Tsai, et al.Applied Physics Letters, 2009,95,013107) propose one without the need to intermediate transfer medium, by thermoplastic PC substrate, directly VA-CNTs array is transferred in Merlon (PC) substrate.The people such as Ye (Ye Y, et al. Journal of Materials Chemistry, 2011, 21 (3): 837-842.) at every root CNT and the uniform PGMA polymer coating of target substrate surface chemistry vapour deposition one deck, functionalization transfer is carried out to VA-CNTs array, cross-linking reaction between PGMA coating and VA-CNTs, both the mechanical property of VA-CNTs and wet stability had been improved, also the combination of VA-CNTs and target substrate is improved, functionalization transfer method complex process, high to equipment requirement, adjacent VA-CNTs may assemble bunchy by polymer overmold, porosity uniformity is difficult to control, CNTs-polymer composites may be formed completely by polymer-filled.In order to keep the electric conductivity even improving VA-CNTs array, low melting point eutectic (AuSn, SnAg, SnPb) (Kumar A, et al. Applied physics letters, 2006, 89 (16): 163120. Zhu L, et al. Nano letters, 2006, 6 (2): 243-247.) and more In (the Fu Y of low melting point, et al. Advanced Materials, 2010, 22 (44): 5039-5042.) solder is chosen as, by welding transfer VA-CNTs array in metallic substrates, the noble metal such as depositing Ti/Ni/Au improves solder to the wetability of metallic substrates on the metallic substrate in advance, so that the shear strength increased between VA-CNTs array and metallic substrates, process costs is relatively high, also there is the problems such as solder reflow.
Summary of the invention
Technical problem to be solved by this invention is to provide and a kind ofly shifts the method for vertical carbon nanotube array to flexible polymer substrate, both the top structure of former array can have been retained, avoid again introducing the intermediate mediums such as adhesive, this transfer method is the direct effect of vertical carbon nanotube array and flexible polymer, avoids the introducing of other media and brings new interface problem.
A kind of vertical carbon nanotube array that shifts of the present invention is to the method in flexible polymer substrate, and it comprises the following steps:
(1) vertical carbon nanotube array is prepared;
(2) strip step 1) obtained vertical carbon nanotube array, obtain the vertical carbon nanotube array departing from growth substrate self-supporting;
(3) top or bottom that depart from the array of growth substrate self-supporting are contacted with flexible polymer substrate; Realize top transfer and bottom transfer respectively;
(4) between array and polymeric substrates, 0.2-2N/cm is kept
2pressure, impel vertical carbon nanotube array embed elastomeric state polymeric substrates in; Be heated to more than glass transition temperature and after insulation, make it soften and be in elastomeric state, be cooled to cold curing; Complete array transfer.
Array top wherein after the transfer of bottom remains the structure that former array top bends winding, and the array top after the transfer of top remains the structure aligned bottom former array.
Above-mentioned steps 1) described vertical carbon nanotube array generally adopts chemical vapour deposition technique to prepare.
In step 2) in process, heated oxide process is carried out to prepared vertical carbon nanotube array, the combination of array and growth substrate is weakened, then peel off with blade Aided Machine, obtain the array departing from growth substrate self-supporting.
In addition, the present invention is in above-mentioned steps 3) following several change can also be had:
The array departing from growth substrate self-supporting is divided into two rows, and the bottom of often arranging is placed in the upper and lower surface of same flexible polymer substrate respectively; I.e. two-sided transfer.
Two row's flexible polymer substrates are placed in the array top and bottom that depart from growth substrate self-supporting respectively, form a kind of one deck sandwich.
The array departing from growth substrate self-supporting is superposed in order successively with flexible polymer substrate, forms multilayer sandwich structure.
The present invention proposes a kind ofly vertical carbon nanotube array and growth substrate are departed from and is transferred to the method in flexible polymer substrate, and technique is simple, cost is low, effective in short-term, and has following beneficial effect:
1, this method can retain the top structure of primary long VA-CNTs array, realizes the transfer of large area array; A kind of two-sided VA-CNTs array adhesive can be prepared, i.e. two-sided transfer; The array departing from growth substrate self-supporting can also be superposed in order successively with polymeric substrates, form sandwich.
2, in transfer process, as the flexible polymer of target substrate from being heated to elastomeric state again to being cooled to room temperature, still good pliability can be kept, by thermal deformation uniform ground, and it is good to the wellability of carbon nano pipe array, under the effect of heating and cooling iterative cycles, original character under room temperature can be kept.
3, this transfer method is carbon nano pipe array and flexible polymer substrate direct effect, the interfacial effect that the introducing avoiding various intermediate medium brings and the phenomenon causing array contraction to destroy with pattern.
4, this transfer method is not by the restriction of vertical carbon nanotube array size, density size.
5, this transfer method technique is simple, and the mode such as Resistant heating, LASER HEATING is all applicable to heating according to claim 5 makes polymeric substrates soften to elastomeric state.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of bottom of the present invention transfer and top transfer;
Fig. 2 is the structural representation of the two-sided transfer of the present invention;
Fig. 3 is the structural representation of one deck sandwich of the present invention;
Fig. 4 is the structural representation of multilayer sandwich structure of the present invention;
Fig. 5 is heated oxide process schematic diagram in present invention process process.
Detailed description of the invention
Below in conjunction with accompanying drawing 1-5, the present invention is elaborated.
Embodiment 1
Adopt chemical vapour deposition technique at Si/SiO
2vertical carbon nanotube array is prepared in substrate, array is placed in quartz tube furnace and is heated to 400-500 DEG C, and pass into air oxidation, weaken the combination of array and growth substrate, blow with blade up-stripping or slight air-flow, obtain the vertical carbon nanotube array departing from growth substrate self-supporting.
As Fig. 1, PETG (PET) substrate is placed in the array top of self-supporting, at 0.4N/cm
2contact under, be heated to 270-280 DEG C in resistance furnace, insulation 10min, stop heating, be cooled to cold curing, carbon nano pipe array is transferred in PET base.
In Fig. 1
si/SiO
2substrate;
depart from Si/SiO
2the CNTA of substrate self-supporting;
polymeric substrates;
slide.Fig. 2 is heated oxide process schematic diagram in present invention process process.
Embodiment 2
Adopt chemical vapour deposition technique at Si/SiO
2vertical carbon nanotube array is prepared in substrate, array is placed in quartz tube furnace and is heated to 400-500 DEG C, and pass into air oxidation, array sample is taken out after cooling to room temperature with the furnace, blow with blade up-stripping or slight air-flow, obtain the vertical carbon nanotube array departing from growth substrate self-supporting.
By dry after Merlon (PC) substrate in ethanol ultrasonic cleaning 2min before transfer, then by depart from growth substrate self-supporting vertical carbon nanotube array and after Merlon (PC) substrate is shifted by bottom respectively and top branch mode assembles, put into tube furnace and be heated to 250-260 DEG C, insulation 5-10min, applies 0.8N/cm between array and PC
2contact, promote PC be infiltrated up in vertical carbon nanotube array, impel array and PC good combination.Stop heating, be cooled to room temperature, vertical carbon nanotube array is transferred in PC substrate.
Embodiment 3
Adopt chemical vapour deposition technique at Si/SiO
2vertical carbon nanotube array is prepared in substrate, array is placed in quartz tube furnace and passes into air heat oxidation, temperature range is 400-500 DEG C, array sample is taken out after cooling to room temperature with the furnace, blow with blade up-stripping or slight air-flow, obtain the vertical carbon nanotube array departing from growth substrate self-supporting.
Dimethyl silicone polymer (PDMS) mixes formulated by host with curing agent mass ratio 10:1, PDMS colloidal sol is dripped on silicon chip and naturally spreads out, and 3-5min is solidified in the baking oven of 80 DEG C, PDMS forms uniform thin layer on silicon chip, namely prepares PDMS substrate.The vertical carbon nanotube array departing from growth substrate self-supporting is divided into two rows, and the bottom of often arranging contacts with the upper and lower surface of same PDMS substrate respectively; I.e. two-sided transfer (Fig. 2).Put into the baking oven of 80 DEG C afterwards, PDMS is tightly combined with vertical carbon nanotube array after continuing to solidify about 5-10min, takes out subsequently, is cooled to room temperature in atmosphere, and transfer vertical carbon nanotube array is in PDMS substrate.
Embodiment 4
Adopt chemical vapour deposition technique at Si/SiO
2vertical carbon nanotube array is prepared in substrate, array is placed in quartz tube furnace and passes into air heat oxidation, temperature range is 400-500 DEG C, array sample is taken out after cooling to room temperature with the furnace, blow with blade up-stripping or slight air-flow, obtain the vertical carbon nanotube array departing from growth substrate self-supporting.
The vertical carbon nanotube array of self-supporting is placed in respectively PC substrate top and bottom, i.e. two-sided transfer; PC substrate is placed in respectively vertical carbon nanotube array top and the bottom of self-supporting, forms one deck sandwich (Fig. 3); The vertical carbon nanotube array of self-supporting is superposed in order successively with PC substrate, forms multilayer sandwich structure (Fig. 4); Load 0.8N/cm
2contact after, these three kinds of package assemblies are placed in tube furnace and are heated to 250-260 DEG C, insulation 5-10min, PC is fully infiltrated, is combined with array, cool to cold curing with the furnace.Obtain two-sided transfer array, one deck of array and PC and multilayer sandwich structure.
Embody rule approach of the present invention is a lot, and the above is only the preferred embodiment of the present invention, should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvement, these improvement also should be considered as protection scope of the present invention.
Claims (10)
1. shift vertical carbon nanotube array to the method in flexible polymer substrate, it is characterized in that comprising the following steps:
(1) vertical carbon nanotube array is prepared;
(2) strip step 1) obtained vertical carbon nanotube array, obtain the vertical carbon nanotube array departing from growth substrate self-supporting;
(3) top or bottom that depart from the array of growth substrate self-supporting are contacted with flexible polymer substrate;
(4) between array and polymeric substrates, 0.2-2N/cm is kept
2pressure, be heated to more than glass transition temperature and after being incubated 5-10min, cool to cold curing with the furnace; Complete array transfer.
2. transfer vertical carbon nanotube array according to claim 1 is to the method in flexible polymer substrate, it is characterized in that: vertical carbon nanotube array described in step 1) adopts chemical vapour deposition technique preparation.
3. transfer vertical carbon nanotube array according to claim 2 is to the method in flexible polymer substrate, it is characterized in that: step 2) in process, heated oxide process is carried out to prepared vertical carbon nanotube array, heated oxide temperature is 400-500 DEG C, the combination of array and growth substrate is weakened, peel off with blade Aided Machine again, obtain the array departing from growth substrate self-supporting.
4. shift vertical carbon nanotube array to the method in flexible polymer substrate, it is characterized in that comprising the following steps:
(1) vertical carbon nanotube array is prepared;
(2) strip step 1) obtained vertical carbon nanotube array, obtain the vertical carbon nanotube array departing from growth substrate self-supporting;
(3) array departing from growth substrate self-supporting is divided into two rows, the bottom of often arranging is placed in the upper and lower surface of same flexible polymer substrate respectively;
(4) between array and polymeric substrates, 0.2-2N/cm is kept
2pressure, be heated to more than glass transition temperature and after being incubated 5-10min, cool to cold curing with the furnace; Complete array transfer.
5. transfer vertical carbon nanotube array according to claim 4 is to the method in flexible polymer substrate, it is characterized in that: vertical carbon nanotube array described in step 1) adopts chemical vapour deposition technique preparation.
6. transfer vertical carbon nanotube array according to claim 5 is to the method in flexible polymer substrate, it is characterized in that: step 2) in process, heated oxide process is carried out to prepared vertical carbon nanotube array, heated oxide temperature is 400-500 DEG C, the combination of array and growth substrate is weakened, peel off with blade Aided Machine again, obtain the array departing from growth substrate self-supporting.
7. shift vertical carbon nanotube array to the method in flexible polymer substrate, it is characterized in that comprising the following steps:
(1) vertical carbon nanotube array is prepared;
(2) strip step 1) obtained vertical carbon nanotube array, obtain the vertical carbon nanotube array departing from growth substrate self-supporting;
(3) two row's flexible polymer substrates are placed in the array top and bottom that depart from growth substrate self-supporting respectively, form a kind of one deck sandwich;
(4) between array and polymeric substrates, 0.2-2N/cm is kept
2pressure, be heated to more than glass transition temperature and after being incubated 5-10min, cool to cold curing with the furnace; Complete array transfer.
8. transfer vertical carbon nanotube array according to claim 7 is to the method in flexible polymer substrate, it is characterized in that: vertical carbon nanotube array described in step 1) adopts chemical vapour deposition technique preparation.
9. transfer vertical carbon nanotube array according to claim 8 is to the method in flexible polymer substrate, it is characterized in that: step 2) in process, heated oxide process is carried out to prepared vertical carbon nanotube array, heated oxide temperature is 400-500 DEG C, the combination of array and growth substrate is weakened, peel off with blade Aided Machine again, obtain the array departing from growth substrate self-supporting.
10. shift vertical carbon nanotube array to the method in flexible polymer substrate, it is characterized in that comprising the following steps:
(1) vertical carbon nanotube array is prepared;
(2) strip step 1) obtained vertical carbon nanotube array, obtain the vertical carbon nanotube array departing from growth substrate self-supporting;
(3) array departing from growth substrate self-supporting is superposed in order successively with flexible polymer substrate, form multilayer sandwich structure;
(4) between array and polymeric substrates, 0.2-2N/cm is kept
2pressure, be heated to more than glass transition temperature and after being incubated 5-10min, cool to cold curing with the furnace; Complete array transfer.
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| CN106658779A (en) * | 2016-12-15 | 2017-05-10 | 复旦大学 | Intelligent wearable resistance heating fabric and preparation method thereof |
| CN107934908A (en) * | 2017-05-15 | 2018-04-20 | 北京大学深圳研究生院 | Nano materials and preparation method thereof |
| CN108622879A (en) * | 2017-03-22 | 2018-10-09 | 中国科学院金属研究所 | A kind of dry contact transfer method of vertical carbon nanotube array |
| CN110718398A (en) * | 2018-07-13 | 2020-01-21 | 天津大学 | High-capacity carbon nanotube-cobaltosic sulfide nickel composite material and preparation method and application thereof |
| CN110885059A (en) * | 2019-04-23 | 2020-03-17 | 厦门大学 | Power generation method of carbon nanotube array |
| CN111380614A (en) * | 2018-12-29 | 2020-07-07 | 清华大学 | Infrared detector and infrared imager |
| CN113243045A (en) * | 2019-01-22 | 2021-08-10 | 深圳市柔宇科技股份有限公司 | Flexible display panel and manufacturing method thereof |
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Cited By (10)
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| CN106658779A (en) * | 2016-12-15 | 2017-05-10 | 复旦大学 | Intelligent wearable resistance heating fabric and preparation method thereof |
| CN108622879A (en) * | 2017-03-22 | 2018-10-09 | 中国科学院金属研究所 | A kind of dry contact transfer method of vertical carbon nanotube array |
| CN108622879B (en) * | 2017-03-22 | 2021-09-24 | 中国科学院金属研究所 | Dry contact transfer method of carbon nano tube vertical array |
| CN107934908A (en) * | 2017-05-15 | 2018-04-20 | 北京大学深圳研究生院 | Nano materials and preparation method thereof |
| CN110718398A (en) * | 2018-07-13 | 2020-01-21 | 天津大学 | High-capacity carbon nanotube-cobaltosic sulfide nickel composite material and preparation method and application thereof |
| CN111380614A (en) * | 2018-12-29 | 2020-07-07 | 清华大学 | Infrared detector and infrared imager |
| CN113243045A (en) * | 2019-01-22 | 2021-08-10 | 深圳市柔宇科技股份有限公司 | Flexible display panel and manufacturing method thereof |
| CN113243045B (en) * | 2019-01-22 | 2022-11-29 | 深圳市柔宇科技股份有限公司 | Flexible display panel and manufacturing method thereof |
| CN110885059A (en) * | 2019-04-23 | 2020-03-17 | 厦门大学 | Power generation method of carbon nanotube array |
| CN110885059B (en) * | 2019-04-23 | 2023-05-09 | 厦门大学 | Power generation method of carbon nano tube array |
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Application publication date: 20141224 |