CN103407179A - Device and method for preparing film with high orientation degree - Google Patents
Device and method for preparing film with high orientation degree Download PDFInfo
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- CN103407179A CN103407179A CN2013102784201A CN201310278420A CN103407179A CN 103407179 A CN103407179 A CN 103407179A CN 2013102784201 A CN2013102784201 A CN 2013102784201A CN 201310278420 A CN201310278420 A CN 201310278420A CN 103407179 A CN103407179 A CN 103407179A
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000010408 film Substances 0.000 claims description 76
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000011521 glass Substances 0.000 claims description 11
- 239000010409 thin film Substances 0.000 claims description 11
- 230000009471 action Effects 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 238000010030 laminating Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000011160 research Methods 0.000 abstract description 6
- 239000002120 nanofilm Substances 0.000 abstract 2
- 238000000407 epitaxy Methods 0.000 abstract 1
- 229920001903 high density polyethylene Polymers 0.000 description 13
- 239000004700 high-density polyethylene Substances 0.000 description 13
- 229920006262 high density polyethylene film Polymers 0.000 description 7
- 229920002521 macromolecule Polymers 0.000 description 7
- 239000012528 membrane Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 239000004698 Polyethylene Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003028 elevating effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
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Abstract
The invention relates to a device for preparing a film with a high orientation degree and a method for preparing a film with a high orientation degree by use of the device. The method can be used for preparing a high-molecular nano film with a high orientation degree. According to the device, by adopting a method of heating to volatize a solvent in a high-molecular solution, a layer of uniform film is firstly formed on a hot platform and lifted from the hot platform through an automatic-lifting rotation roller so as to form a continuous oriented film between the hot platform and the roller; the thickness of the film is controlled by adjusting the rotation speed of the roller; and the final nano film can be applied to the research in terms of high-molecular epitaxy and electric conduction.
Description
[technical field]
The present invention relates to a kind of apparatus and method that prepare the high-orientation film, especially, based on high-orientation nano thin-film preparation facilities and the method for melting macromolecular material, belong to the film preparing technology field.
[background technology]
In recent years, along with the development of polymeric material field research, macromolecule membrane, due to its unique character, receives much concern in the middle of scientific research field.Especially in recent years the sudden emergence of photovoltaic industry, make and adopt macromolecule membrane substituted single crystal silicon sheet to reach its maturity in order to the research of manufacturing solar cell.
Simultaneously, comparable its isotropic homogeneous material of Physical and mechanical properties of orientation macromolecular material exceeds several orders of magnitude, and for example, comparable its non-orientation homogeneous material of the hardness of highly oriented polyethylene (PE) and intensity improves 100 times.Therefore, nearly decades the structure of height-oriented polymer and the research of performance are aroused great concern.
Preparing at present the method that is orientated macromolecule membrane mainly contains and adds hot-drawing method, solution plated film czochralski method.Wherein the macromolecule membrane thickness that makes of uniaxial tension method is larger, is generally micron level, and is subject to the impact of macromolecular material self performance, reaches easily fracture after certain level of stretch, can't make nano level oriented film.Although and the film thickness that solution plated film czochralski method makes can reach nanoscale, its degree of orientation is lower, and the method carrier such as the silicon chip that need to fix, application is restricted.
[summary of the invention]
[technical problem that will solve]
Purpose of the present invention is for providing a kind of device of nanoscale high-orientation macromolecule membrane.
Another object of the present invention is for providing the method for preparing the high-orientation film with the described device for preparing the high-orientation film.
A further object of the present invention is for providing the described application of device in the macromolecule membrane preparation for preparing the high-orientation film.
[technical scheme]
The invention discloses a kind of device for preparing high-orientation high molecular nanometer film, can be used for preparing the degree of orientation and the controlled high molecular nanometer film of thickness.
The invention also discloses the method for preparing the high-orientation film with the described device for preparing the high-orientation film.In the method for the invention, removal of solvents in the Polymer Solution that the mode of employing heating will prepare, and on hot platform, form the uniform fused films of one deck, by roller and the hot platform pressing that will rotate, film is taken up from hot platform, owing between film self and roller and hot platform, having certain absorption affinity, thereby between roller and hot platform, form the continuous oriented film of one deck, and by the rotating speed of dancer rools, control thickness and the degree of orientation of film.Wherein, in this device, add revolution counter, can show in real time the rotating speed of roller, thereby realized the control of preparation condition.And the lifting of the roller of employing step motor control, the inhomogeneous film breaks caused of shake while having avoided hand-held roller to lift, deflection and speed.
The present invention is achieved through the following technical solutions.
A kind of device for preparing the high-orientation film, this device comprise control system, heating part, rotating part and lifting part; It is characterized in that: the control system in this device comprises temperature controller (10), rotational speed regulation module (7), digital display rotational speed table (9), controllor for step-by-step motor (8); Heating part comprises hot platform (6); Rotating part comprises DC speed-reducing (11), encoder (12) and live-rollers (3); Lifting unit divides and comprises stepper motor (1) and screw rod lifting device (2); Wherein lifting partly is fixed on base plate, and rotating part is fastened on lifting and partly goes up, and its turning cylinder is to the motor shaft with the lifting part to vertical, and heating part is positioned under rotating part, and unsettled being fixed on base plate; Hot platform (6) homogeneous heating of heating part and directly be connected to control heating-up temperature with the temperature controller (10) in control system; The DC speed-reducing of rotating part (11) adopts shaft coupling coaxially to be connected with live-rollers (3) and encoder (12), and the rotational speed regulation module (7) in control system directly is connected to control the rotating speed of live-rollers (3) by cable and DC speed-reducing (11); Rotating speed detects via encoder (12), outputs in digital display rotational speed table (9); In the lifting part, stepper motor (1) adopts shaft coupling coaxially to be connected with screw rod lifting device (2), by controllor for step-by-step motor (8) programming Control stepper motor (1), thereby realizes that the fast lifting of screw rod lifting device (2) moves.
A preferred embodiment of the invention, is characterized in that the rotating speed of live-rollers (3), and the temperature of hot platform (6) and screw rod lifting device (2) rising or falling speed are controlled by control system.
A preferred embodiment of the invention, is characterized in that live-rollers (3) surface is processed, and makes itself and sample thin film adsorbed close.
Can carry out following mode processing to live-rollers (3) surface, to increase the bonding of live-rollers and film: on the live-rollers surface, be wound around the multilayer low-density polyethylene film in advance, because its fusing point is lower, after touching high-temperature stage, melt, make between live-rollers and hot platform upper film and form gunk-squeeze process, thereby film is mentioned to the formation oriented film from glass plate.
A preferred embodiment of the invention, is characterized in that on described hot platform (6) being fixed with a thin glass plate.
The method for preparing the high-orientation film with the aforesaid device for preparing the high-orientation film, is characterized in that the method comprises the steps:
A) by the control Temperature Setting of temperature controller (10), be 110-250 ℃, hot platform (6) starts heating;
The polymer solution that the concentration that b) will prepare is about 0.5-3% is poured on hot platform (6) surface and it is applied evenly;
C) standing 15-30 minute, after solvent evaporates, control live-rollers (3) and hot platform (6) laminating on screw rod lifting device (2), the rotating speed of regulating rotary action roller (3) is that 60-500 per minute turns simultaneously, and the film on hot platform (6) is adhered on live-rollers (3);
D) screw rod lifting device (2) separated rapidly with hot platform (6) and be elevated to setting height, the rotating speed of regulating rotary action roller (3), form the nanoscale film of orientation continuously thereby control between live-rollers (3) and hot platform (6) simultaneously.
Described setting height refers to the height between roller and glass plate, this distance be used for handled easily librarian use instrument or device by oriented film from device, taking off and set, usually can be 20-150mm.When after roller and glass contact, the film on glass plate being mentioned, just can form oriented film, if the distance of mentioning is too little, be close to glass plate, want to take off the film be between glass plate and roller just very difficult.A preferred embodiment of the invention is characterized in that: according to oriented film prepared by the method, its degree of orientation and thickness are controlled.
A kind of application of device in the macromolecule membrane preparation for preparing the high-orientation film.
In embodiments of the invention, by the control Temperature Setting of temperature controller (10), be 110-250 ℃, be preferably set to 140-200 ℃, more preferably be set as 160-200 ℃, most preferably be set as 175 ℃-200 ℃.The concentration of polymer solution is set as 0.5-3%, is preferably set to 0.8-2.5%, more preferably is set as 1.0-1.5%.
The rotating speed of regulating rotary action roller (3) is that 60-500 per minute turns, and preferred 60-300 per minute turns, and more preferably 60-150 per minute turns.
[beneficial effect]
The present invention is owing to taking technique scheme, and it has the following advantages:
1, film thickness and degree of orientation are controlled.The thickness of film can be controlled by being poured on the rotating speed of solution amount and live-rollers on hot platform, and film thickness can reach nanoscale
2,, by live-rollers is carried out to different surface treatments, can be suitable for the preparation of multiple polymers nano thin-film.
3, can freely select thin-film carrier.Because nano thin-film has strong Electrostatic Absorption effect, after film prepared by additive method is attached on carrier, can't take off, but while by this method, carrying out film preparation, film is in vacant state, therefore available any carrier takes off film, carries out various testing researches, has greatly expanded the range of application of film.
4, preparation thin film alignment degree is high.In melting process, strand can be freely movable, and than the room temperature uniaxial tension, the degree of orientation is larger.Strand is along with draw direction is orientated, and after film left hot platform, temperature decrease was to glass transition temperature (Tg), and strand is frozen and keep current state of orientation.
5, automaticity is high, simple to operate.
[accompanying drawing explanation]
Fig. 1 is high-orientation film preparation device schematic diagram.
Fig. 2 is the control system schematic diagram of high-orientation film preparation device.
Fig. 3 is the rotating part schematic diagram of high-orientation film preparation device.
Fig. 4 is the lifting part schematic diagram of high-orientation film preparation device.
Fig. 5 is the perspective view of high-orientation film preparation device.
Fig. 6 is stereoscan photograph and the X-ray diffractogram of the density polyethylene film with high of preparation.
Fig. 7 is the atomic force microscopy of the density polyethylene film with high of preparation.
Description of reference numerals:
1 stepper motor,
2 screw rod lifting devices,
3 live-rollers,
The nano thin-film of 4 orientations,
5 films,
6 hot platforms,
7 rotational speed regulation knobs,
8 controllor for step-by-step motor,
9 digital display rotational speed tables,
10 temperature controllers,
11 DC speed-reducing,
12 encoders,
13 roller supports,
14 lifting supports,
15 ball screws,
[specific embodiment]
Below in conjunction with drawings and Examples, the present invention is described in detail.
As shown in Figure 1, the inventive system comprises an oriented film preparation facilities (Fig. 1), it comprises a control system (Fig. 2), a rotating part (Fig. 3) and a lifting part (Fig. 4).In Fig. 1, the sample solution prepared (concentration is about 1%) is poured on hot platform 6 and applies evenly, after solvent evaporates, forms thin film 5, and due to the heat effect of hot platform, film 5 is in molten condition.By the screw rod lifting device 2 drive live-rollers 3 of regulating stepper motor 1 driving, with certain rotating speed, press down and fit with the film 5 on hot platform 6, then raise rapidly live-rollers 3 to certain altitude (taking-up that does not affect film gets final product), now between live-rollers 3 and hot platform 6, form the nano thin-film 4 of one deck orientation.
Control system shown in Figure 2, comprise rotational speed regulation module 7, controllor for step-by-step motor 8, digital display rotational speed table 9 and temperature controller 10, rotational speed regulation module 7 directly shows numerical value in order to the rotating speed (rotating speed 0-500 rpm adjustable) of controlling live-rollers 3 and by digital display rotational speed table 9, controllor for step-by-step motor 8 is in order to rotating and the stand-by time of control step motor 1, thereby control the elevating movement of screw rod lifting device 2, temperature controller 10, in order to control from the temperature that heats platform 6, makes the quick volatile solute melting of solvent.
Rotating part shown in Figure 3, comprise live-rollers 3, DC speed-reducing 11, encoder 12 and roller support 13.Wherein DC speed-reducing 11, live-rollers 3 and encoder 12 coaxially are connected, and DC speed-reducing 11 drives live-rollers 3 constant revolutions, and rotating speed detects via encoder 12, outputs in digital display rotational speed table 9 and directly shows.
Lifting part shown in Figure 4, comprise stepper motor 1, lifting support 14 and ball screw 15.Wherein the ball screw 15 band action roller supports 13 on stepper motor 1 driving lifting support 14 carry out elevating movement, thereby make live-rollers 3 with film 5, fit and separate.
Use oriented film preparation facilities of the present invention to prepare high density polyethylene (HDPE) (HDPE) high-orientation nano thin-film
At first high density polyethylene (HDPE) (HDPE) is dissolved in the middle of xylene solvent, controlling solution concentration is 1% left and right, then preheating heat platform to 165 ℃, be poured on the sample solution configured on the glass plate of placing on preheated hot platform, and apply evenly by glass bar.After solvent is heated volatilization fully, open control panel, adjust the live-rollers rotating speed and be about 120 rpms, and control it and with sample surfaces, contact fast and separate and rise to certain altitude, now at roller continuous HDPE film together with forming between glass plate, and by the mode that substrate attaches, film is taken off.Fig. 6 is the spectrogram of HDPE film in the X-ray diffraction test of preparation, and therefrom we can find that HDPE is orientated along draw direction.Fig. 7 is the photo of HDPE film under AFM of preparation, and therefrom we can find that its thickness is about 50nm.
Embodiment 3(comparative example, use the uniaxial tension method to prepare the HDPE film)
By commercially available high density polyethylene (HDPE) (HDPE) film, be placed on universal tensile testing machine and carry out extension test, found that, HDPE film elongation at break is about 400%, thickness gauge is measured and is shown that it is under 350% stretching ratio, average thickness is 30 microns, and this character with the uniaxial orientation HDPE film of commercially producing at present is consistent.
Embodiment 4(comparative example, use solution plated film czochralski method to prepare the HDPE film)
At first, high density polyethylene (HDPE) (HDPE) is dissolved in the middle of xylene solvent, controlling solution concentration is 1% left and right, clean silicon chip is placed on the fixture of plated film pulling machine, control silicon chip and sink to fully in the middle of solution, flood after about 10 minutes and with 10 microns speed per minute, silicon chip is slowly risen and proposes in the middle of solution.By AFM, its thickness is measured to discovery, its thickness is about 180nm.
From experimental result, finding out, its degree of orientation of film that the method obtains is lower.Carrier such as the silicon chip that need to fix of the method in addition, application is restricted.
Claims (7)
1. device for preparing the high-orientation film, this device comprises control system, heating part, rotating part and lifting part; It is characterized in that: the control system in this device comprises temperature controller (10), rotational speed regulation module (7), digital display rotational speed table (9), controllor for step-by-step motor (8); Heating part comprises hot platform (6); Rotating part comprises DC speed-reducing (11), encoder (12) and live-rollers (3); Lifting unit divides and comprises stepper motor (1) and screw rod lifting device (2); Wherein lifting partly is fixed on base plate, and rotating part is fastened on lifting and partly goes up, and its turning cylinder is to the motor shaft with the lifting part to vertical, and heating part is positioned under rotating part, and unsettled being fixed on base plate; Hot platform (6) homogeneous heating of heating part and directly be connected to control heating-up temperature with the temperature controller (10) in control system; The DC speed-reducing of rotating part (11) adopts shaft coupling coaxially to be connected with live-rollers (3) and encoder (12), and the rotational speed regulation module (7) in control system directly is connected to control the rotating speed of live-rollers (3) by cable and DC speed-reducing (11); Rotating speed detects via encoder (12), outputs in digital display rotational speed table (9); In the lifting part, stepper motor (1) adopts shaft coupling coaxially to be connected with screw rod lifting device (2), by controllor for step-by-step motor (8) programming Control stepper motor (1), thereby realizes that the fast lifting of screw rod lifting device (2) moves.
2. the device for preparing the high-orientation film according to claim 1, is characterized in that the rotating speed of live-rollers (3), and the temperature of hot platform (6) and screw rod lifting device (2) rising or falling speed are all controlled by control system.
3. the device for preparing the high-orientation film according to claim 1, is characterized in that live-rollers (3) surface is processed, and makes its adsorbed close sample thin film.
4. the device for preparing the high-orientation film according to claim 1, is characterized in that on described hot platform (6) being fixed with a thin glass plate.
5. right to use requires the 1 described device for preparing the high-orientation film to prepare the method for high-orientation film, it is characterized in that the method comprises the steps:
A) by the control Temperature Setting of temperature controller (10), be 110-250 ℃, hot platform (6) starts heating;
The polymer solution that the concentration that b) will prepare is about 0.5-3% is poured on hot platform (6) surface and it is applied evenly;
C) standing 15-30 minute, after solvent evaporates, control live-rollers (3) and hot platform (6) laminating on screw rod lifting device (2), the rotating speed of regulating rotary action roller (3) is that 60-300 per minute turns simultaneously, and the film on hot platform (6) is adhered on live-rollers (3);
D) screw rod lifting device (2) separated rapidly with hot platform (6) and be elevated to setting height, the rotating speed of regulating rotary action roller (3), form the nanoscale film of orientation continuously thereby control between live-rollers (3) and hot platform (6) simultaneously.
6. the method for preparing the high-orientation film claimed in claim 5, it is characterized in that: according to oriented film prepared by the method, its degree of orientation and thickness are controlled.
7. a kind of application of device in the macromolecular orientation film preparation for preparing the high-orientation film claimed in claim 1.
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|---|---|---|---|
| CN201310278420.1A CN103407179B (en) | 2013-07-04 | 2013-07-04 | A kind of apparatus and method preparing film with high orientation degree |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310278420.1A CN103407179B (en) | 2013-07-04 | 2013-07-04 | A kind of apparatus and method preparing film with high orientation degree |
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| CN103407179A true CN103407179A (en) | 2013-11-27 |
| CN103407179B CN103407179B (en) | 2015-08-19 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004302093A (en) * | 2003-03-31 | 2004-10-28 | Iinuma Gauge Seisakusho:Kk | Rubbing device and method, and liquid crystal display element |
| US20050275781A1 (en) * | 2004-06-14 | 2005-12-15 | Boe Hydis Technology Co., Ltd. | Rubbing apparatus for LCD |
| CN101522395A (en) * | 2006-10-06 | 2009-09-02 | 3M创新有限公司 | Process for making an optical film |
| CN101770115A (en) * | 2008-12-30 | 2010-07-07 | 北京京东方光电科技有限公司 | Alignment film rubbing process and device |
| CN102385194A (en) * | 2011-11-17 | 2012-03-21 | 昆山龙腾光电有限公司 | Alignment layer film thickness adjusting system and method |
-
2013
- 2013-07-04 CN CN201310278420.1A patent/CN103407179B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004302093A (en) * | 2003-03-31 | 2004-10-28 | Iinuma Gauge Seisakusho:Kk | Rubbing device and method, and liquid crystal display element |
| US20050275781A1 (en) * | 2004-06-14 | 2005-12-15 | Boe Hydis Technology Co., Ltd. | Rubbing apparatus for LCD |
| CN101522395A (en) * | 2006-10-06 | 2009-09-02 | 3M创新有限公司 | Process for making an optical film |
| CN101770115A (en) * | 2008-12-30 | 2010-07-07 | 北京京东方光电科技有限公司 | Alignment film rubbing process and device |
| CN102385194A (en) * | 2011-11-17 | 2012-03-21 | 昆山龙腾光电有限公司 | Alignment layer film thickness adjusting system and method |
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