CN107564603A - Transparent graphene conductive film based on flexible glass and preparation method thereof - Google Patents
Transparent graphene conductive film based on flexible glass and preparation method thereof Download PDFInfo
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- CN107564603A CN107564603A CN201710573181.0A CN201710573181A CN107564603A CN 107564603 A CN107564603 A CN 107564603A CN 201710573181 A CN201710573181 A CN 201710573181A CN 107564603 A CN107564603 A CN 107564603A
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Abstract
The invention discloses a kind of transparent graphene conductive film based on flexible glass and preparation method thereof, comprise the following steps：R2R CVD methods realize the growth of flexible Copper substrate transparent conductive graphene membrane；Copper-base graphite alkene cold rolling is sticked into hot stripping film, Copper substrate is removed through pickling, then is transferred to through heat rolling in flexible glass, while removes hot stripping film, obtains the transparent graphene conductive film based on flexible glass.On same flexible glass so repeatedly, electrical property and the multi-layer graphene transparent conductive film of optical property enhancing be can obtain.A four line touch panels are made with hollow template and silk-screen printing；Print silver electrode and point is spaced, top panel and lower panel are carefully assembled and form graphene-based flexible touch-screen electronic instrument.
Description
Technical field
The present invention relates to flexible electronic transparent conductive film and its technology of preparing, especially a kind of transparent graphite of flexible glass
Volume to volume (R2R) method of alkene film, and the flexible glass graphene conductive transparent membrane prepared using this method.
Background technology
Flexible electronic is exactly the emerging electricity being produced on electronic device on flexible Drawability plastics, glass or thin metal matrix plate
Sub- technology, with its unique flexibility, ductility and efficient, inexpensive manufacturing process, led in information, the energy, medical treatment, national defence etc.
Domain has wide application prospect, such as flexible electronic displays, thin-film solar cell panel, electronics surface mount.Flexible electrical
Son have it is soft, deformable, light, portable, can the characteristic such as large-area applications, and by widely applying new material and new technology to produce
A large amount of new opplications are born, including RFID, Flexible Displays, OLED are luminous, sensor, flexible photovoltaic, logical AND store, flexible electrical
Pond.In future, " paster " is pasted on the back of the hand with regard to that can detect ultraviolet degree of illumination；Pacemaker no longer changes battery；
Battery can directly wind production simultaneously.In recent years, this new branch of science of flexible electronic caused domestic and international scientific and technological circle with
The extensive concern of industrial quarters, the R＆D process that numerous companies put into this sciemtifec and technical sphere is attract, accelerate flexible electronic
Practical product exploitation and commercialization process.In development in science and technology " 13 " planning, country passes through policy guide and money
Gold, which is helped, to promote the flexible research and industrialization with printed electronic of China energetically.China is electronic industry big country, but is not skill
Art is made the country prosperous, and flexible electronic is the chance that China strives for electronic industry great-leap-forward development.Flexible electronic has broad mass market, market rule
Mould is expanded rapidly, can turn into national pillar industry.
Flexible electronic transparent conductive film is exactly that caused film is not only conductive with more the transparency, is flexible
Thin film solar, display screen, electroluminescent device, thin film transistor (TFT), electric capacity and electric resistance touch screen, transparent heater etc. it is important
Material.Compared with rigid substrate transparent conductive film, it also with flexibility and may extend away in addition to the conductive and transparency
Property, it is the important materials for developing flexible electronic device.
The content of the invention
Goal of the invention：A kind of R2R CVD production is provided and is based on flexible electronic glass transparent conductive graphene membrane, goes forward side by side one
Step provides the film plating process of volume to volume matrix transfer, provides basic flexible glass transparent for the development of flexible electronic device and leads
Graphene film production method.
Technical scheme：The present invention uses following technical scheme：
A kind of transparent graphene conductive film based on flexible glass, transparent graphene conductive film is grown in soft
On the property flexible glass of 25-100 microns rather than on current nonbreakable glass.
A kind of preparation method of the transparent graphene conductive film based on flexible glass, including three parts：
(1) R2R CVD growths copper-base graphite alkene transparent conductive film；
(2) R2R shifts copper-base graphite alkene transparent conductive film to flexible glass；
(3) manufacture of the transparent graphene conductive film touch-screen electronic device based on flexible glass.
Further, in described (1) part, R2R CVD growths use R2R CVD stoves, and R2R CVD stoves have double with one heart
Quartz ampoule, interior quartz ampoule are rotations, partly there is gas port therebetween, so as to CH4 enter outer tube wall and outer wall of inner tube it
Between, realize that R2R graphene films produce.
Further, what it was prepared comprises the following steps that：
Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter by step 1., is led in outer tube
Enter the hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes；
Step 2. step 1 is passed through the CH of 30SCCM flows in quartz inner pipe while implementation4With the H of 10SCCM flows2,
Keep pipe to be pressed in 500mTorr 30 minutes, then pass to hydrogen in the case where pipe presses 100mTorr with 15 DEG C/sec of fast quickly coolings of cooling rate
But normal temperature is arrived；
The Copper thin film and hot stripping film that step 3. obtains step 2 processing are also cross rolling surface one group of rolling close to each other
Wheel, the graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers；
Copper-based portion is immersed in plastics pickling basin by step 4. to be removed copper corrosion and falls and clean residual acid with deionized water
Liquid, dry；
Step 5. be put between two rollers 25-100 microns flexible glass and insert post hot stripping film graphene it is slow
It is heated to 85-125 DEG C and is disengaged with the speed transmission of 150-250 mm/mins, hot stripping film, graphene is transferred to flexible glass
On glass；
Step 6. so repeatedly, can obtain multi-layer graphene film in same flexible glass；
Step 7. makes a four line touch panels with hollow template and silk-screen printing；Print between silver electrode and point
Every by top panel and lower panel, carefully assembling forms graphene-based flexible touch-screen electronic instrument.
Further, the transparent graphene conductive film for preparing completion is grown in the flexible flexible glass of 25-100 microns
On.
Beneficial effect：The present invention is compared with prior art：
(1) transparent graphene conductive film of flexible glass, the development for flexible electronic device are directly formed；
(2) electric thin formed is flexible and extends；Performance is suitable with the film performance on nonbreakable glass.
(3) this method is applied to the production of large area thin film circuits, and speed is fast, high yield rate.
Embodiment
A kind of transparent graphene conductive film based on flexible glass, transparent graphene conductive film is grown in soft
On the property flexible glass of 25-100 microns rather than on current nonbreakable glass.
A kind of preparation method of the transparent graphene conductive film based on flexible glass, including three parts：
(1) R2R CVD growths copper-base graphite alkene transparent conductive film；
(2) R2R shifts copper-base graphite alkene transparent conductive film to flexible glass；
(3) manufacture of the transparent graphene conductive film touch-screen electronic device based on flexible glass.
In (1) part, R2R CVD growths use R2R CVD stoves, and R2R CVD stoves have concentric biquartz pipe, interior quartz
Pipe is rotation, partly there is gas port therebetween, so that CH4 enters between outer tube wall and outer wall of inner tube, realizes R2R graphite
Alkene film production.
R2R CVD growths graphene film method of the present invention and R2R matrixes transfer film process step are as follows：
Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter by step 1., is led in outer tube
Enter the hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes.
Step 2. is passed through the CH of 30SCCM flows in inner tube simultaneously4With the H of 10SCCM flows2, keep pipe to be pressed in
500mTorr 30 minutes, then pass to hydrogen and be cooled fast to normal temperature in the case where pipe presses 100mTorr with 15 DEG C/sec of cooling rates.
The Copper thin film and hot stripping film that step 3. obtains step 2 processing are also cross rolling surface one group of rolling close to each other
Wheel, the graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers.
Copper-based portion is immersed in plastics pickling basin by step 4. to be removed copper corrosion and falls and clean residual acid with deionized water
Liquid, dry.
Step 5. be put between two rollers 25-100 microns flexible glass and insert post hot stripping film graphene it is slow
It is heated to 85-125 DEG C and is disengaged with the speed transmission of 150-250 mm/mins, hot stripping film, graphene is transferred to flexible glass
On glass.
Step 6. so repeatedly, can obtain multi-layer graphene film in same flexible glass.
Step 7. makes a four line touch panels with hollow template and silk-screen printing；Print between silver electrode and point
Every by top panel and lower panel, carefully assembling forms graphene-based flexible touch-screen electronic instrument.
Embodiment 1
(1) Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter, be passed through in outer tube
The hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes.
(2) H2 of the CH4 and 10SCCM flows of 30SCCM flows while in inner tube is passed through, keeps pipe to be pressed in 500mTorr
30 minutes, then pass to hydrogen and be cooled fast to normal temperature in the case where pipe presses 100mTorr with 15 DEG C/sec of cooling rates.
(3) by the step 2 obtained Copper thin film of processing and hot stripping film also cross rolling surface one group of roller close to each other,
The graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers.
(4) copper-based portion is immersed in plastics pickling basin and removes copper corrosion and fall and clean remaining acid solution with deionized water,
Dry.
(5) 25 microns of flexible glass are put between two rollers and are inserted and posts the graphene of hot stripping film and is heated slowly to
90 DEG C and with the speed transmission of 150 mm/mins, hot stripping film is disengaged, and graphene is transferred in flexible glass.
(6) it is repeated twice in same flexible glass, can obtain two layers of graphene film.
Embodiment 2
(1) Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter, be passed through in outer tube
The hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes.
(2) H2 of the CH4 and 10SCCM flows of 30SCCM flows while in inner tube is passed through, keeps pipe to be pressed in 500mTorr
30 minutes, then pass to hydrogen and be cooled fast to normal temperature in the case where pipe presses 100mTorr with 15 DEG C/sec of cooling rates.
(3) by the step 2 obtained Copper thin film of processing and hot stripping film also cross rolling surface one group of roller close to each other,
The graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers.
(4) copper-based portion is immersed in plastics pickling basin and removes copper corrosion and fall and clean remaining acid solution with deionized water,
Dry.
(5) 50 microns of flexible glass are put between two rollers and are inserted and posts the graphene of hot stripping film and is heated slowly to
100 DEG C and with the speed transmission of 180 mm/mins, hot stripping film is disengaged, and graphene is transferred in flexible glass.
(6) in same flexible glass so in triplicate, three layer graphene films be can obtain.
(7) a four line touch panels are made with hollow template and silk-screen printing；Print silver electrode and point is spaced, will
Carefully assembling forms graphene-based flexible touch-screen electronic instrument for top panel and lower panel
Embodiment 3
(1) Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter, be passed through in outer tube
The hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes.
(2) H2 of the CH4 and 10SCCM flows of 30SCCM flows while in inner tube is passed through, keeps pipe to be pressed in 500mTorr
30 minutes, then pass to hydrogen and be cooled fast to normal temperature in the case where pipe presses 100mTorr with 15 DEG C/sec of cooling rates.
(3) by the step 2 obtained Copper thin film of processing and hot stripping film also cross rolling surface one group of roller close to each other,
The graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers.
(4) copper-based portion is immersed in plastics pickling basin and removes copper corrosion and fall and clean remaining acid solution with deionized water,
Dry.
(5) 100 microns of flexible glass are put between two rollers and are inserted and posts the graphene of hot stripping film and is heated slowly to
120 DEG C and with the speed transmission of 200 mm/mins, hot stripping film is disengaged, and graphene is transferred in flexible glass.
(6) so it is repeated four times in same flexible glass, can obtain four layer graphene films.
(7) a four line touch panels are made with hollow template and silk-screen printing；Print silver electrode and point is spaced, will
Carefully assembling forms graphene-based flexible touch-screen electronic instrument for top panel and lower panel
Embodiment 4
(1) Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter, be passed through in outer tube
The hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes.
(2) H2 of the CH4 and 10SCCM flows of 30SCCM flows while in inner tube is passed through, keeps pipe to be pressed in 500mTorr
30 minutes, then pass to hydrogen and be cooled fast to normal temperature in the case where pipe presses 100mTorr with 15 DEG C/sec of cooling rates.
(3) by the step 2 obtained Copper thin film of processing and hot stripping film also cross rolling surface one group of roller close to each other,
The graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers.
(4) copper-based portion is immersed in plastics pickling basin and removes copper corrosion and fall and clean remaining acid solution with deionized water,
Dry.
(5) 60 microns of flexible glass are put between two rollers and are inserted and posts the graphene of hot stripping film and is heated slowly to
85 DEG C and with the speed transmission of 170 mm/mins, hot stripping film is disengaged, and graphene is transferred in flexible glass.
(6) so repeated five times in same flexible glass, can obtain five layer graphene films.
(7) a four line touch panels are made with hollow template and silk-screen printing；Print silver electrode and point is spaced, will
Carefully assembling forms graphene-based flexible touch-screen electronic instrument for top panel and lower panel
Embodiment 5
(1) Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter, be passed through in outer tube
The hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes.
(2) H2 of the CH4 and 10SCCM flows of 30SCCM flows while in inner tube is passed through, keeps pipe to be pressed in 500mTorr
30 minutes, then pass to hydrogen and be cooled fast to normal temperature in the case where pipe presses 100mTorr with 15 DEG C/sec of cooling rates.
(3) by the step 2 obtained Copper thin film of processing and hot stripping film also cross rolling surface one group of roller close to each other,
The graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers.
(4) copper-based portion is immersed in plastics pickling basin and removes copper corrosion and fall and clean remaining acid solution with deionized water,
Dry.
(5) 25 microns of flexible glass are put between two rollers and are inserted and posts the graphene of hot stripping film and is heated slowly to
125 DEG C and with the speed transmission of 250 mm/mins, hot stripping film is disengaged, and graphene is transferred in flexible glass.
(6) so repeated six times in same flexible glass, can obtain six layer graphene films.
(7) a four line touch panels are made with hollow template and silk-screen printing；Print silver electrode and point is spaced, will
Carefully assembling forms graphene-based flexible touch-screen electronic instrument for top panel and lower panel.
Using TEM, the analysis example 1 such as four probe resistance measuring instruments, UV-vis optical spectrum instrumentations arrives flexibility prepared by example 5
Electronic glass graphene film, specific analysis result are shown in Table 1.
The flexible electronic glass graphite alkene transparent membrane results of performance analysis of table 1
Above-described embodiment is merely to illustrate the present invention, and according to above-described embodiment, the present invention may be better understood, and does not have to
In limitation the scope of the present invention.In addition, this area scientific research technical staff read the present invention after, with equivalent substitution or variable etc. pair
The present invention carries out various modifications, also belongs to claims of the present invention limited range.
Claims (5)
- A kind of 1. transparent graphene conductive film based on flexible glass, it is characterised in that：Graphene electrically conducting transparent is thin Film is grown on the flexible flexible glass of 25-100 microns rather than on current nonbreakable glass.
- 2. a kind of preparation method of transparent graphene conductive film as claimed in claim 1 based on flexible glass, It is characterized in that：Including three parts：(1) R2R CVD growths copper-base graphite alkene transparent conductive film；(2) R2R shifts copper-base graphite alkene transparent conductive film to flexible glass；(3) manufacture of the transparent graphene conductive film touch-screen electronic device based on flexible glass.
- 3. the preparation method of the transparent graphene conductive film according to claim 2 based on flexible glass, its It is characterised by：In described (1) part, R2R CVD growths use R2R CVD stoves, and R2R CVD stoves have concentric biquartz pipe, Interior quartz ampoule is rotation, partly there is gas port therebetween, so that CH4 enters between outer tube wall and outer wall of inner tube, is realized R2R graphene films produce.
- 4. the preparation method of the transparent graphene conductive film based on flexible glass according to Claims 2 or 3, It is characterized in that：What it was prepared comprises the following steps that：Copper thin film is wound up on the quartz inner pipe outer wall of 200 centimetres of 20 centimetre length of diameter by step 1., is passed through in outer tube The hydrogen of 10SCCM flows, it is 95mTorr to keep the pressure in quartz ampoule, is warmed to 1050 DEG C；Insulation 45 minutes；Step 2. step 1 is passed through the CH of 30SCCM flows in quartz inner pipe while implementation4With the H of 10SCCM flows2, keep Pipe is pressed in 500mTorr 30 minutes, then passes to hydrogen and is cooled fast in the case where pipe presses 100mTorr with 15 DEG C/sec of cooling rates Normal temperature；Step 3. by the step 2 obtained Copper thin film of processing and hot stripping film also cross rolling surface one group of roller close to each other, The graphenic surface grown on copper-based is pasted into the hot stripping film of last layer plus micro pressure on two rollers；Copper-based portion is immersed in plastics pickling basin by step 4. to be removed copper corrosion and falls and clean remaining acid solution with deionized water, is dried in the air It is dry；Step 5. is put into 25-100 microns flexible glass between two rollers and inserts the graphene slow heating for posting hot stripping film Disengaged to 85-125 DEG C and with the speed transmission of 150-250 mm/mins, hot stripping film, graphene is transferred in flexible glass；Step 6. so repeatedly, can obtain multi-layer graphene film in same flexible glass；Step 7. makes a four line touch panels with hollow template and silk-screen printing；Print silver electrode and point is spaced, will Carefully assembling forms graphene-based flexible touch-screen electronic instrument for top panel and lower panel.
- 5. the preparation method of the transparent graphene conductive film according to claim 4 based on flexible glass, its It is characterised by：The transparent graphene conductive film completed is prepared to be grown on the flexible flexible glass of 25-100 microns.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110911031A (en) * | 2019-10-21 | 2020-03-24 | 珠海烯蟀科技有限公司 | Device with conducting strip as graphene layer power supply electrode |
| CN112325762A (en) * | 2020-09-14 | 2021-02-05 | 兰州大学 | Graphene multifunctional thin film sensor and preparation method thereof |
| CN114512559A (en) * | 2021-12-28 | 2022-05-17 | 中国建材国际工程集团有限公司 | Flexible large-area laminated solar cell and preparation method thereof |
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| CN202799224U (en) * | 2012-09-28 | 2013-03-13 | 江苏物联网研究发展中心 | Transparent electric heating film based on graphene |
| CN106158144A (en) * | 2016-06-23 | 2016-11-23 | 无锡格菲电子薄膜科技有限公司 | A kind of preparation method of ultra-thin super Flexible graphene conductive film |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202799224U (en) * | 2012-09-28 | 2013-03-13 | 江苏物联网研究发展中心 | Transparent electric heating film based on graphene |
| CN106158144A (en) * | 2016-06-23 | 2016-11-23 | 无锡格菲电子薄膜科技有限公司 | A kind of preparation method of ultra-thin super Flexible graphene conductive film |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110911031A (en) * | 2019-10-21 | 2020-03-24 | 珠海烯蟀科技有限公司 | Device with conducting strip as graphene layer power supply electrode |
| CN112325762A (en) * | 2020-09-14 | 2021-02-05 | 兰州大学 | Graphene multifunctional thin film sensor and preparation method thereof |
| CN112325762B (en) * | 2020-09-14 | 2021-10-01 | 兰州大学 | Graphene multifunctional thin film sensor and preparation method thereof |
| CN114512559A (en) * | 2021-12-28 | 2022-05-17 | 中国建材国际工程集团有限公司 | Flexible large-area laminated solar cell and preparation method thereof |
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Application publication date: 20180109 |