CN103693611B - A kind of Kynoar/CNT taper micro-pillar array and preparation method thereof - Google Patents
A kind of Kynoar/CNT taper micro-pillar array and preparation method thereof Download PDFInfo
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Abstract
A kind of Kynoar/CNT taper micro-pillar array disclosed by the invention and preparation method thereof, form prefabricated array structure by electricity capillary force effect polymer, then make PVDF polymeric rheology stretch in electric field force driving effect and form vertical orientated, uniform sequential array structure。The invention has the beneficial effects as follows and utilize electric field force driving effect in preparation process, making PVDF obtain good piezoelectric property through electro rheological and drawing process, final acquisition has piezoelectric property PVDF/CNTs nucleocapsid taper micro-pillar array。
Description
Technical field
The invention belongs to technical field of micro-nano manufacture, be specifically related to a kind of Kynoar/CNT taper micro-pillar array, the preparation method that the invention still further relates to above-mentioned array。
Background technology
In nature, biological beard, lower limb must have the perception of acumen, as sea dog beard can the short arc water movement that causes of perception prey, the antenna of Blatta seu periplaneta can the various low amplitude vibrations of accurate perception surrounding。This perceptive function of biological antenna inspires research worker that its structure and mechanism of perception are studied, and prepares bionical Whisker Sensor。Owing to being limited by preparation technology, the structure of Whisker Sensor is designed to split-type structural。Sensor is assembled by bionical antenna and sensor element and forms。Although this Whisker Sensor can perception from the air-flow of any direction, but this sensor is not high to the perceptual sensitivity of weak gas flow。Reason is in that antenna only transmits vibration, and perceptual signal is converted into the signal of telecommunication according to different sensing principles by the sensing element of antenna root again, fails to realize vibration perception integrated with transmission。If antenna is inherently sensing element while perception is vibrated, it is nucleocapsid micro-column structure by sensing material and electrode design, and the arrangement in array simultaneously, then it is possible not only to perception weak gas flow signal and the sensitivity of sensor can be increased substantially。
PVDF, owing to having good piezoelectric property, has flexibility simultaneously and is prone to processing and forming, thus be especially suitable for and prepare this sensor。But show according to existing achievement in research, PVDF need to enter overstretching and polarization process process just can possess piezoelectric property, and this is the PVDF critical technological point being applied to nucleocapsid structure array。
Summary of the invention
It is an object of the invention to provide a kind of Kynoar/CNT taper micro-pillar array, solve PVDF in prior art and prepare the problem that nucleocapsid micro-column structure array cannot carry out stretching in the process of polarization。
The preparation method that it is a further object of the present invention to provide above-mentioned array。
The technical solution adopted in the present invention is, a kind of Kynoar/CNT taper micro-pillar array, including the silicon base set gradually from top to bottom, TiAlN thin film layer and patterned Ni layer, on patterned Ni layer, growth has carbon nano tube bundle electrod-array, populated with PVDF taper micro-pillar array around carbon nano tube bundle electrod-array。
Another technical scheme of the present invention is, the preparation method of a kind of Kynoar/CNT taper micro-pillar array, specifically implements according to following steps:
Step 1: one layer of TiAlN thin film layer of sputtering on a silicon substrate, then prepares patterned Ni layer on TiAlN thin film layer, grows carbon nano tube bundle electrod-array on patterned Ni layer;
Step 2: there is the surface spin coating PVDF polymer solution of carbon nano tube bundle electrod-array;
Step 3: the first electro-conductive glass is positioned over spin coating has above the silicon chip of PVDF polymer solution, and between mould and silicon chip, apply electric field, under the driving effect of electric field force, solution is assembled around carbon nano tube bundle electrod-array, forms polymer film layer;
Step 4: the silicon chip with polymer film layer is placed in top, second electro-conductive glass with circle or square array electrode is positioned over below silicon chip, between silicon chip and the second electro-conductive glass, apply electric field, under electric field force drives, form PVDF taper micro-pillar array。
The feature of the present invention also resides in,
Step 1 therein is specifically implemented according to following steps: () adopts the TiAlN thin film layer of magnetron sputtering technique uniform sputter 50-100nm on a silicon substrate;() adopts photoetching and Lift-off technique to prepare the patterned Ni layer of 50-500nm;() adopts pecvd process to prepare the carbon nano tube bundle electrod-array that characteristic size is 10-100 μm。
In step 2 therein, the configuration of PVDF polymer solution and spin coating are specifically implemented according to following steps: be dissolved under 15 DEG C of-20 DEG C of environment in dimethylformamide DMF by Kynoar PVDF powder, it is configured to the polymer solution that concentration is 10-70g/L, after stirring 30-60 minute with magnetic stirrer, it is placed in vacuum 1/2-2 hour, seals and place 12-72 hour;This solution curtain coating is spun in the substrate with carbon pipe electrode layer。
Step 3 therein specifically according to following steps implement: utilize the first electro-conductive glass as on put electrode masterplate, between the first electro-conductive glass and silicon chip apply 10-80V/ μm of electric field voltage, keep 1-3 hour。
Step 4 therein is specifically implemented according to following steps: prepare circle or square array electrode by designing requirement at the second conductive glass surface;The silicon base being coated with polymer film layer inverts in top, second electro-conductive glass with array pattern is placed below, applying field intensity in the environment that temperature is 170-200 DEG C between silicon base and the second electro-conductive glass is the voltage of 50-800V/ μm, keep 1-3 hour, after removing electric field, it is cooled to 80 DEG C gradually, makes annealing treatment 3-36 hour, obtain taper micro-column structure。
The invention has the beneficial effects as follows, form prefabricated array structure by electricity capillary force effect polymer, then make PVDF polymeric rheology stretch in electric field force driving effect and form vertical orientated, uniform sequential array structure。The invention has the beneficial effects as follows and utilize electric field force driving effect in preparation process, making PVDF obtain good piezoelectric property through electro rheological and drawing process, final acquisition has piezoelectric property PVDF/CNTs nucleocapsid taper micro-pillar array。
Accompanying drawing explanation
Fig. 1 is the schematic diagram preparing carbon nano pipe array figure in silicon base;
Fig. 2 is the schematic diagram of spin coating PVDF polymeric layer solution layer on the silicon base with carbon nano pipe array;
The solvent volatilization formation PVDF thin film that Fig. 3 is in PVDF layer of polymer solution covers array carbon nanotube surface, applies the schematic diagram of electric field between face is arranged on this substrate electro-conductive glass and substrate;
Fig. 4 is that the silicon chip that will be covered with carbon nano-array and polymer P VDF thin layer is placed in top, by placed below for the electro-conductive glass with square or circular array, and applies the schematic diagram of electric field between silicon chip and electro-conductive glass;
Fig. 5 is that the PVDF thin polymer film being covered in around carbon nano pipe array is at high temperature become the schematic diagram of tapered array by fusion drawn under electric field force driving effect。
In figure, 1. silicon base, 2.TiN thin layer, 3. patterned Ni layer, 4. carbon nano tube bundle electrod-array, 5.PVDF polymer solution, 6. polymer film layer, 7. the first electro-conductive glass, 8. circle or square array electrode, 9. the second electro-conductive glass, 10.PVDF taper micro-pillar array。
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail。
The structure of Kynoar of the present invention/CNT taper micro-pillar array is as shown in Figure 5, including the silicon base 1 set gradually from top to bottom, TiAlN thin film layer 2, patterned Ni layer 3, on patterned Ni layer 3, growth has carbon nano tube bundle electrod-array 4, carbon nano tube bundle electrod-array 4 surrounding populated with PVDF taper micro-pillar array 10。
The preparation method of Kynoar of the present invention/CNT taper micro-pillar array, specifically implements according to following steps:
Step 1: as it is shown in figure 1, sputter one layer of TiAlN thin film layer 2 on a silicon substrate 1, then at TiAlN thin film layer 2 patterned Ni layer 3 prepared above, grow carbon nano tube bundle electrod-array 4 on this patterned Ni layer 3;
Specifically implement according to following steps: () adopts the TiAlN thin film layer 2 of magnetron sputtering technique uniform sputter 50-100nm on a silicon substrate 1;() adopts photoetching and Lift-off technique to prepare the graphical Ni layer 3 of 50-500nm;() adopts pecvd process to prepare the carbon nano tube bundle electrod-array 4 that characteristic size is 10-100 μm;
Step 2: as in figure 2 it is shown, have the surface spin coating PVDF polymer solution 5 of carbon nano tube bundle electrod-array 4;PVDF polymer solution 5 configures and spin coating is particularly as follows: by Kynoar PVDF powder, it is dissolved in dimethylformamide DMF under 15 DEG C of-20 DEG C of environment, it is configured to the polymer solution that concentration is 10-70g/L, after stirring 30-60 minute with magnetic stirrer, it is placed in vacuum 1/2-2 hour, seals and place 12-72 hour;This solution curtain coating is spun in the substrate with carbon pipe electrode layer, obtains layer of polymer solution;
Step 3: as shown in Figure 3, first electro-conductive glass 7 is positioned over spin coating have above the silicon chip of PVDF polymer solution 5, and between mould and silicon chip, applies electric field, under the driving effect of electric field force, solution is assembled to carbon nano tube bundle electrod-array 4 surrounding, forms polymer film layer 6。Utilize the first electro-conductive glass 7 as on put electrode masterplate, between the first electro-conductive glass 7 and CNTs electrod-array masterplate apply 10-80V/ μm of electric field voltage, keep 1-3 hour。Solution assembles formation thin layer to CNTs electrode gradually。
Step 4: as shown in Figure 4, the silicon chip with polymer film layer 6 is placed in top, second electro-conductive glass 9 with circle or square array electrode 8 is positioned over below silicon chip, between silicon chip and the second electro-conductive glass 9, applies electric field, under electric field force drives, form PVDF taper micro-pillar array 10。
Specifically implement according to following steps: prepare circle or square array electrode 8 by designing requirement at conductive glass surface;The silicon base 1 being coated with polymer film layer 6 inverts in top, second electro-conductive glass 9 with array pattern is placed below, applying field intensity in the environment that temperature is 170-200 DEG C between silicon base 1 and the second electro-conductive glass 9 is the voltage of 50-80V/ μm, keeps 1-3 hour。After removing electric field, it is cooled to 80 DEG C gradually, makes annealing treatment 3-36 hour, obtain taper micro-column structure。
The invention has the beneficial effects as follows, form prefabricated array structure by electricity capillary force effect polymer, then make PVDF polymeric rheology stretch in electric field force driving effect and form vertical orientated, uniform sequential array structure。The invention has the beneficial effects as follows and utilize electric field force driving effect in preparation process, making PVDF obtain good piezoelectric property through electro rheological and drawing process, final acquisition has piezoelectric property PVDF/CNTs nucleocapsid taper micro-pillar array。
Embodiment 1
1) preparation of carbon nano pipe array: () adopts the TiAlN thin film layer 2 of magnetron sputtering technique uniform sputter 50nm on a silicon substrate 1;() adopts photoetching and Lift-off technique to prepare the graphical Ni layer 3 of 50nm;() adopts pecvd process to prepare the carbon nano tube bundle electrod-array 4 that characteristic size is 10 μm;
2) configuration of PVDF polymer solution and spin coating: by Kynoar PVDF powder, it is dissolved under 15 DEG C of environment in dimethylformamide DMF, is configured to the polymer solution that concentration is 10g/L, after stirring 30 minutes with magnetic stirrer, it is placed in vacuum 1/2 hour, seals and place 12 hours;This solution curtain coating is spun in the substrate with carbon pipe electrode layer, obtains layer of polymer solution;
3) prepared by the precast construction of taper microstructure array: the first electro-conductive glass 7 is positioned over spin coating has above the silicon chip of PVDF polymer solution 5, and between mould and silicon chip, apply electric field, under the driving effect of electric field force, solution is assembled to carbon nano tube bundle electrod-array 4 surrounding, forms polymer film layer 6。Utilize the first electro-conductive glass 7 as on put electrode masterplate, between the first electro-conductive glass 7 and CNTs electrod-array masterplate apply 10V/ μm of electric field voltage, keep 1 hour。Solution assembles the precast construction forming thin layer gradually to CNTs electrode。
4) preparation of taper micro array structure: prepare circular shape array electrode 8 by designing requirement at conductive glass surface;The silicon base 1 being coated with polymer film layer 6 inverts in top, and second electro-conductive glass 9 with array pattern is placed below, and applying field intensity in the environment that temperature is 170 DEG C between silicon base 1 and the second electro-conductive glass 9 is the voltage of 50V/ μm, keeps 1 hour。After removing electric field, it is cooled to 80 DEG C gradually, makes annealing treatment 3 hours, obtain taper micro-column structure。
Embodiment 2
1) preparation of carbon nano pipe array: () adopts the TiAlN thin film layer 2 of magnetron sputtering technique uniform sputter 100nm on a silicon substrate 1;() adopts photoetching and Lift-off technique to prepare the graphical Ni layer 3 of 500nm;() adopts pecvd process to prepare the carbon nano tube bundle electrod-array 4 that characteristic size is 100 μm;
2) configuration of PVDF polymer solution and spin coating: by Kynoar PVDF powder, it is dissolved under 20 DEG C of environment in dimethylformamide DMF, is configured to the polymer solution that concentration is 70g/L, after stirring 60 minutes with magnetic stirrer, it is placed in vacuum 2 hours, seals and place 72 hours;This solution curtain coating is spun in the substrate with carbon pipe electrode layer, obtains layer of polymer solution;
3) prepared by the precast construction of taper microstructure array: the first electro-conductive glass 7 is positioned over spin coating has above the silicon chip of PVDF polymer solution 5, and between mould and silicon chip, apply electric field, under the driving effect of electric field force, solution is assembled to carbon nano tube bundle electrod-array 4 surrounding, forms polymer film layer 6。Utilize the first electro-conductive glass 7 as on put electrode masterplate, between the first electro-conductive glass 7 and CNTs electrod-array masterplate apply 80V/ μm of electric field voltage, keep 3 hours。Solution assembles the precast construction forming thin layer gradually to CNTs electrode。
4) preparation of taper micro array structure: prepare square array electrode 8 by designing requirement at conductive glass surface;The silicon base 1 being coated with polymer film layer 6 inverts in top, and second electro-conductive glass 9 with array pattern is placed below, and applying field intensity in the environment that temperature is 200 DEG C between silicon base 1 and the second electro-conductive glass 9 is the voltage of 80V/ μm, keeps 3 hours。After removing electric field, it is cooled to 80 DEG C gradually, makes annealing treatment 36 hours, obtain taper micro-column structure。
Embodiment 3
1) preparation of carbon nano pipe array: () adopts the TiAlN thin film layer 2 of magnetron sputtering technique uniform sputter 75nm on a silicon substrate 1;() adopts photoetching and Lift-off technique to prepare the graphical Ni layer 3 of 250nm;() adopts pecvd process to prepare the carbon nano tube bundle electrod-array 4 that characteristic size is 60 μm;
2) configuration of PVDF polymer solution and spin coating: by Kynoar PVDF powder, it is dissolved under 18 DEG C of environment in dimethylformamide DMF, is configured to the polymer solution that concentration is 50g/L, after stirring 45 minutes with magnetic stirrer, it is placed in vacuum 1 hour, seals and place 36 hours;This solution curtain coating is spun in the substrate with carbon pipe electrode layer, obtains layer of polymer solution;
3) prepared by the precast construction of taper microstructure array: the first electro-conductive glass 7 is positioned over spin coating has above the silicon chip of PVDF polymer solution 5, and between mould and silicon chip, apply electric field, under the driving effect of electric field force, solution is assembled to carbon nano tube bundle electrod-array 4 surrounding, forms polymer film layer 6。Utilize the first electro-conductive glass 7 as on put electrode masterplate, between the first electro-conductive glass 7 and CNTs electrod-array masterplate apply 45V/ μm of electric field voltage, keep 2 hours。Solution assembles the precast construction forming thin layer gradually to CNTs electrode。
4) preparation of taper micro array structure: prepare circular shape array electrode 8 by designing requirement at conductive glass surface;The silicon base 1 being coated with polymer film layer 6 inverts in top, and second electro-conductive glass 9 with array pattern is placed below, and applying field intensity in the environment that temperature is 180 DEG C between silicon base 1 and the second electro-conductive glass 9 is the voltage of 70V/ μm, keeps 2 hours。After removing electric field, it is cooled to 80 DEG C gradually, makes annealing treatment 24 hours, obtain taper micro-column structure。
Claims (5)
1. the preparation method of Kynoar/CNT taper micro-pillar array, it is characterised in that specifically implement according to following steps:
Step 1: silicon base (1) one layer of TiAlN thin film layer (2) of upper sputtering, then above patterned Ni layer (3) is prepared at TiAlN thin film layer (2), patterned Ni layer (3) upper growth carbon nano tube bundle electrod-array (4);
Step 2: there is surface spin coating PVDF polymer solution (5) of carbon nano tube bundle electrod-array (4);
Step 3: the first electro-conductive glass (7) is positioned over spin coating silicon base (1) top of PVDF polymer solution (5), and between the first electro-conductive glass (7) and silicon base (1), apply electric field, under the driving effect of electric field force, solution is around assembled to carbon nano tube bundle electrod-array (4), forms polymer film layer (6);
Step 4: the silicon base (1) with polymer film layer (6) is placed in top, second electro-conductive glass (9) will with circle or square array electrode (8) is positioned over silicon base (1) lower section, between silicon base (1) and the second electro-conductive glass (9), apply electric field, under electric field force drives, form PVDF taper micro-pillar array (10)。
2. the preparation method of Kynoar according to claim 1/CNT taper micro-pillar array, it is characterized in that, described step 1 is specifically implemented according to following steps: () adopts magnetron sputtering technique at the TiAlN thin film layer (2) of the upper uniform sputter 50-100nm of silicon base (1);() adopts photoetching and Lift-off technique to prepare the patterned Ni layer (3) of 50-500nm;() adopts pecvd process to prepare carbon nano tube bundle electrod-array (4) that characteristic size is 10-100 μm。
3. the preparation method of Kynoar according to claim 1/CNT taper micro-pillar array, it is characterized in that, in described step 2, PVDF polymer solution (5) configuration and spin coating are specifically implemented according to following steps: be dissolved in dimethylformamide by Kynoar PVDF powder under 15-20 DEG C of environment, it is configured to the polymer solution that concentration is 10-70g/L, after stirring 30-60 minute with magnetic stirrer, it is placed in vacuum 1/2-2 hour, seals and place 12-72 hour;This solution curtain coating is spun in the silicon base (1) with carbon nano tube bundle electrod-array (4)。
4. the preparation method of Kynoar according to claim 1/CNT taper micro-pillar array, it is characterized in that, described step 3 is specifically implemented according to following steps: utilizes and puts electrode masterplate in the first electro-conductive glass (7) conduct, between the first electro-conductive glass (7) and silicon base (1), apply the voltage of field intensity 10-80V/ μm, keep 1-3 hour。
5. the preparation method of Kynoar according to claim 1/CNT taper micro-pillar array, it is characterized in that, described step 4 is specifically implemented according to following steps: prepare circle or square array electrode (8) by designing requirement on the second electro-conductive glass (9) surface;The silicon base (1) being coated with polymer film layer (6) inverts in top, second electro-conductive glass (9) with array pattern is placed below, applying field intensity in the environment that temperature is 170-200 DEG C between silicon base (1) and the second electro-conductive glass (9) is the voltage of 50-800V/ μm, keep 1-3 hour, after removing electric field, it is cooled to 80 DEG C gradually, makes annealing treatment 3-36 hour, obtain taper micro-column structure。
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CN101776495A (en) * | 2010-03-12 | 2010-07-14 | 浙江大学 | Micro/nano fiber structure-based touch sensor and preparation method thereof |
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