CN104795497B - A kind of insulating barrier method of modifying for inkjet printing OTFT - Google Patents
A kind of insulating barrier method of modifying for inkjet printing OTFT Download PDFInfo
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- CN104795497B CN104795497B CN201410796448.9A CN201410796448A CN104795497B CN 104795497 B CN104795497 B CN 104795497B CN 201410796448 A CN201410796448 A CN 201410796448A CN 104795497 B CN104795497 B CN 104795497B
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Abstract
The invention discloses a kind of insulating barrier method of modifying for inkjet printing OTFT, including：Hydrophilic region is formed on the gate insulation layer of substrate；Synthesize ATRP（ATRP）Above ATRP silane end initiators are grown on the insulating barrier of substrate by silane end initiator, solwution method, form ATRP initiator monolayers.ATRP initiators monolayer triggers monomer that ATRP occurs in substrate surface, is used as the decorative layer of inkjet printing OTFT gate insulation layer in substrate surface formation one layer of polymeric molecular brush by polymerisation；By controlling polymerization time, the thickness of different degrees of change polymer molecule brush decorative layer, to regulate and control size, pattern and the crystal habit of the semiconductor ink droplet single-point film of inkjet printing, so as to regulate and control the electric property of inkjet printing single-point device.
Description
Technical field
The present invention relates to technical field of liquid crystal display, more particularly to a kind of for inkjet printing OTFT
Insulating barrier method of modifying.
Background technology
Because organic semiconductor thin-film generally all has larger body conductance, if film transistor device in integrated circuit
Organic semiconductor thin-film interconnect, on the one hand easily produce crosstalk between adjacent devices, on the other hand can also make device
Leakage current greatly increase, cause switching current than reduce.The presence of these problems seriously hinders OTFT devices in large area
Application in array and integrated circuit, therefore the patterning of active layer is increasingly important.
Inkjet printing patterning process has incomparable advantage in all patterning methods.It can be realized certainly first
Writing in patterning.Only need to be controlled coordinate of the print nozzles on substrate, set the interval between two print points
Distance, it is possible to the film preparation patterned independent of other factors (such as masterplate, design etc.).And ink-jet
Impact system can also prepare the insulating layer material and electrode material of patterning.The mechanization of ink jet printing device and intelligence degree
It is extremely advanced, especially when preparing the organic thin film transistor array of large area, multiple black head cooperatings can be
The preparation of finishing patterns film in the very short time.But ink-jet printing process has the defects of fatal, its method is prepared organic
Film transistor device performance is also poor.It is primarily due to that the film that ink jet printing device prints is uneven, and especially single-point is beaten
Easily there is coffee toroidal effect in the drying process in print, ink droplet, form surrounding thickness, the film of intermediate thin, the interface topography of film
Bad, the very big transmission for influenceing carrier.Single droplet volume is small, and one layer of very thin liquid can be formed after spreading over substrate surface
Body thin film, its drying process and dried semiconductor layer pattern are with crystal habit largely by the surface nature shadow of substrate
Ring.In order to improve single-point film morphology and crystal habit, have at present with more by regulating and controlling substrate surface energy, in substrate surface
The methods of growth organic supramolecular decorative layer, spin-coated polymer layers, changes interfacial property, so as to realizing to film morphology and
The regulation and control of crystallization.
The content of the invention
It is an object of the invention to provide a kind of insulating barrier method of modifying for inkjet printing OTFT, to
Regulate and control the pattern and crystal habit of the semiconductive thin film of printing, to regulate and control the electric property of device.
The technical solution adopted by the present invention is：
Insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that comprise the following steps：
（1）Synthesize ATRP ATRP silane end initiators, the conjunction of described silane end initiator
Into comprising the following steps：
Take dry triethylamine 7.2ml and 80ml tetrahydrofuran to mix respectively, be a liquid；The bromo- 2- methyl-propionyl bromides of 2-
5.92ml and 40ml tetrahydrofurans mix, and are b liquid；B liquid is slowly added dropwise in a liquid, reaction is filtered off after 3.8-4.1h is stirred at room temperature
Sediment in liquid, being poured into after tetrahydrofuran is evaporated in 100ml dichloromethane, mixed liquor is extracted with aqueous hydrochloric acid solution, and
Dried with anhydrous magnesium sulfate, finally vacuumize dry oily liquids, i.e. silane end initiator（3- aminopropyls）- triethoxy
Silane；
（2）Above ATRP silane end initiators are grown on the insulating barrier of substrate with solwution method, ATRP is formed and triggers
Agent monolayer, described solwution method comprise the following steps：The above-mentioned silane end initiators of 0.3ml are taken to be dissolved in 60-62ml nothing
In water-toluene, silicon chip is dipped in above-mentioned solution and is heated to 50 DEG C, heated 3.9-4.1h, moved to after stirring at room temperature, by silicon chip
It is dipped in solution and keeps 12-12.5h, is put into ultrasonic 9-10min in 25-26ml toluene after taking out silicon chip, then use acetone successively
With each ultrasonic 4-5min of methanol, finally silicon chip is dried up with nitrogen；
（3）Trigger monomer that ATRP occurs in substrate surface ATRP initiators monolayer, pass through
Polymerisation forms one layer of polymeric molecular brush repairing as inkjet printing OTFT gate insulation layer in substrate surface
Adorn layer；Concrete technology step is：Surface A TRP will be prepared above by solwution method（ATRP）Initiator list
The silicon chip of molecular layer is put into the flask with diaphragm of rubber, extraction nitrogen 3 times, nitrogen atmosphere protection；Respectively take 54ml benzene second
Alkene, 220mg copper bromides and 66ml anhydrous anisoles are in another flask with diaphragm of rubber, and inflated with nitrogen 1h；Take 628 μ L's
PMDETA is added in the mixed system, and mixed liquor is stirred at 100 DEG C until become uniform, is injected mixed liquor with syringe previous
It is placed with the flask of initiator silicon chip, 12h is polymerize at 100 DEG C, and add 92 μ L radical initiator ethyl -2- bromo acids
Ester, polymerization with dichloromethane rinse silicon chip and ATRP crystal grain after terminating, then by silicon chip tetrahydrofuran surname extraction 24H；
（4）By controlling polymerization time, the thickness of different degrees of change polymer molecule brush decorative layer, to regulate and control ink-jet
Size, pattern and the crystal habit of the semiconductor ink droplet single-point film of printing, so as to regulate and control the electricity of inkjet printing single-point device
Performance.
2nd, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that described
Substrate is silicon chip and glass substrate.
3rd, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that described
Polymerization is ATRP polymerization.
4th, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that polymer
The thickness of insulating barrier can be controlled by polymerization time, and described polymerization time is 6-24h, and described polymer insulation layer thickness is 4-
16nm。
6th, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that described
Insulating polymer molecule brush material is polystyrene, gathered（Methyl）Esters of acrylic acid, polyacrylonitrile, polydiene hydrocarbon rubbers, with
And the block copolymer of above polymer, preferred polystyrene.
7th, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that described
The solvent of semiconductor ink droplet solution is dichloro-benzenes, tetrahydronaphthalene or methyl phenyl ethers anisole.
8th, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that including according to
Gate electrode, gate insulation layer, polymer molecule brush decorative layer, source-drain electrode and the organic semiconductor layer of secondary arrangement, wherein, it is described poly-
Adduct molecule brush decorative layer is prepared by claim 1 methods described, and organic semiconductor layer is made by inkjet printing.
9th, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that described
The semi-conducting material of organic semiconductor layer is small molecule type semiconductor, and preferably 6,13- is double（Tri isopropyl silane ethyl-acetylene base）And
Pentaphene (TIPS- pentacenes), 2,7- didecyls-[1] benzothiophene [3,2-b] [1]-benzothiophene (BTBT).
10th, the described insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that described
Source-drain electrode is made by gold, silver, aluminium or graphene.
11st, the described insulating barrier method of modifying for inkjet printing OTFT, semiconductive small molecule/ink droplet
The solution quality percentage concentration of solvent is 2%.
It is an advantage of the invention that：
Using technical solution of the present invention, polymer insulation layer surface uniform ground, inside is the different polymer chain of chain length
Segment structure, prepare organic thin film transistor device with the substrate for being grafted PS insulating barriers improves substrate with having within the specific limits
Interfacial property and the size of semiconductor single-point and film, the pattern and crystal habit of machine semiconductor layer, improve organic film
The electric property of transistor device.
Brief description of the drawings
Fig. 1 is the synthesis equation of ATRP silane end initiators.
Fig. 2 is the synthesis equation of substrate surface initiator monolayer.
Fig. 3 is the synthesis equation of substrate surface polystyrene molecular brush decorative layer.
In Fig. 4（a）Scheme for silicon chip surface ATRP initiator monolayers XPS,（b）Scheme for XPS after grafting PS.
In Fig. 5（a）Change for the contact angle of silicon chip surface initiator monolayer water,（b）For the contact of water after grafting PS
Angle changes.
Fig. 6 is the TIPS-BEN single-point and UV/O3 printed on silicon chip surface PS molecular brush decorative layers（UV ozone is cleaned
Instrument）, HMDS（HMDS）, ODTS（Octadecyl trichlorosilane alkane）The TIPS-BEN single-points printed on processing surface
Petrographic microscope figure, a) b) be wherein the single-point array and single-point of the lower printing of UV/O3 processing, c) d) be respectively HMDS processing
The single-point array and single-point of lower printing, e) f) be respectively the lower printing of ODTS processing single-point array and single-point, g) h) i) respectively
For the single-point printed under PS thickness 4nm, 10nm, 16nm.
Fig. 7 is the TIPS-BEN single-points array and UV/O3, HMDS, ODTS printed on silicon chip surface PS molecular brush decorative layers
The XRD of the TIPS-BEN single-point arrays printed on processing surface characterizes comparison diagram.
Fig. 8 is the TIPS- printed on silicon chip surface PS molecular brush decorative layer and UV/O3, HMDS, ODTS processing surface
BEN single-points machine film transistor device optics and petrographic microscope figure, a) be wherein UV/O3 processing, b) it is HMDS processing, c) be
ODTS processing, d) it is PS thickness 16nm.
Fig. 9 is the PS molecular brush decorative layer in silicon chip surface difference thickness 4-16nm with being printed on UV/O3 processing surface
TIPS-BEN single-point machine film transistor device performance maps, the device performance figure under wherein a) being handled for UV/O3, b) it is PS films
Thick 4nm device performance figure, c) be PS thickness 10nm device performance figure, d) be PS thickness 16nm device performance figure.
Embodiment
（1）Synthesize ATRP（ATRP）Silane end initiator；
（2）Above ATRP silane end initiators are grown on the insulating barrier of substrate by solwution method, form ATRP initiators
Monolayer.
（3）ATRP initiators monolayer triggers monomer that ATRP occurs in substrate surface, by poly-
Close reaction and form modification of the one layer of polymeric molecular brush as inkjet printing OTFT gate insulation layer in substrate surface
Layer；
（4）By controlling polymerization time, the thickness of different degrees of change polymer molecule brush decorative layer, to regulate and control ink-jet
Size, pattern and the crystal habit of the semiconductor ink droplet single-point film of printing, so as to regulate and control the electricity of inkjet printing single-point device
Performance.
Embodiment
1. the synthesis of silane end initiator
Dry triethylamine (7.2ml, 52mmol) and 80ml tetrahydrofurans is taken to mix respectively, the bromo- 2- methyl-propionyl of 2-
Bromine (5.92ml, 48mmol) and the mixing of 40ml tetrahydrofurans, the bromo- 2- methyl-propionyl bromides mixed liquors of 2- are slowly added dropwise previous mixed
Close in liquid, filter off sediment in reaction solution after 4h is stirred at room temperature, 100ml dichloromethane is poured into after tetrahydrofuran is evaporated, mix
Liquid is extracted with aqueous hydrochloric acid solution, and is dried with anhydrous magnesium sulfate, is finally vacuumized dry that oily liquids, i.e. silane end trigger
Agent（3- aminopropyls）- triethoxysilane
2. the cleaning of substrate
By the thermally grown silicon chip for there are 300nm SiO2, successively through each ultrasonic 10min of acetone and ethanol, then rushed with a large amount of pure water
Wash, and after nitrogen dries up, 15min is cleaned with UV-ozone cleaning device.
3.ATRP surface aggregates
Above ATRP silane end initiators are grown on the insulating barrier of substrate with solwution method, form ATRP initiator lists
Molecular layer, described solvent method comprise the following steps：Take 0.3ml initiators to be dissolved in dry toluene 60ml, silicon chip is dipped in solution
In be heated to 50 DEG C, heat 4h, moved to after stirring at room temperature, now silicon chip is still dipped in 12h in solution, is put into after taking out silicon chip
Ultrasonic 10min in 25ml toluene, then acetone and each ultrasonic 5min of methanol are used successively, finally dry up silicon chip with nitrogen.
4. the modification of surface insulation layer
Trigger monomer that ATRP occurs in substrate surface ATRP initiators monolayer, pass through polymerization
React and form decorative layer of the one layer of polymeric molecular brush as inkjet printing OTFT gate insulation layer in substrate surface；
Concrete technology step is：Surface A TRP will be prepared above by solwution method（ATRP）Initiator monolayer
Silicon chip be put into the flask with diaphragm of rubber, extraction nitrogen 3 times, nitrogen atmosphere protection.54ml styrene is respectively taken,
220mg copper bromides and 66ml anhydrous anisoles are in another flask with diaphragm of rubber, nitrogen bubble 1h.Take 628 μ L's
PMDETA is added in the mixed system, and mixed liquor is stirred at 100 DEG C until become uniform, is injected mixed liquor with syringe previous
It is placed with the flask of initiator silicon chip, and adds 92 μ L radical initiator ethyl -2- bromo acid esters, polymerize at 100 DEG C,
Polymerization time is that 6h to 24h is not waited to prepare the polystyrene molecular brush thin layer of different thickness.Polymerization uses dichloromethane after terminating
Rinse silicon chip and ATRP crystal grain, then by silicon chip tetrahydrofuran surname extraction 24h.
5. the preparation of single-point OTFT devices
Hot evaporation 40nm gold electrode is as source, drain electrode, and in electrode position inkjet printing 20mg/mL TIPS and five
Benzene/naphthane ink single-point, the OTFT devices of bottom gate top contact are made.
The present invention principle be：
Silane end ATRP is prepared by methodology of organic synthesis（ATRP）Initiator（Reaction equation
Such as Fig. 1）, then the silane initiator is chemically bonded to by silicon chip surface by solwution method, prepare silicon chip surface ATRP monolayers
Initiator（Reaction equation such as Fig. 2）, 100 DEG C are triggered styrene silicon chip surface generation ATRP polymerization again, are prepared silicon chip surface and are gathered
Styrene molecules brush（Reaction equation such as Fig. 3）, polystyrene molecular brush thickness can be regulated and controled by polymerization time, in certain limit
Interior polymerization time is longer, and molecular brush thin layer is thicker：A length of 6h upon polymerization, polystyrene molecular brush thickness are 4nm;During polymerization
Long 16h, polystyrene molecular brush thickness are 10nm；A length of 24h during polymerization, molecular brush thickness are 16nm.During with ATRP polymerization
Between growth, obtained PS chain lengths change, and the PS thickness of silicon chip surface grafting is also different.Be grafted PS silicon chip surface compared with
The contact angle of UV/O3 surface treatment water changes, and situation is as shown in Figure 5.There is the silicon chip table of polymerisation molecular brush in synthesis
Face, the ink single-point of the silicon chip inkjet printing after UV/O3, or ODTS, HMDS surface treatment, which does not crystallize, not to be orientated, and situation is as schemed
Shown in 6.It can be seen that from Fig. 6 and 8, in the silicon chip surface ink-jet printing ink single-point of grafting PS chains, hence it is evident that crystalline orientation occurs
Feature, and as the increase of PS thickness, crystallization change with the pattern situation being orientated, the single-point TIPS in certain film thickness range
The crystallinity of pentacene is greatly improved, as there is significantly the single-point that prints on PS molecular brush films that thickness is 4nm and 10nm
Crystalline orientation, the film of printing also have continuous crystalline orientation, and when PS molecular brush thickness is 16nm, serialgram is presented in single-point crystallization
Shape pattern.Such orientation or continuous crystal habit are advantageous to, the transmission of carrier and the raising of device electric property.By
This is visible, regulates and controls PS thickness by regulating and controlling polymerization time, can be achieved to single-point in inkjet printing and film dimensions, pattern and
Crystalline regulation and control.
From fig. 9, it can be seen that forming one layer of polymeric molecular brush in substrate surface by polymerisation is used as inkjet printing
Device average mobility prepared by the silicon chip surface inkjet printing of the decorative layer of OTFT gate insulation layer is in certain film
Apparently higher than the device average mobility 3.76e-4 only printed by the silicon chip of the surface treatments such as UV/O3 in thick scope, thickness
Increase, is advantageous to improve device mobility in right amount, and device average mobility made from when such as PS thickness being 4nm is 1.68e-3, and
When thickness is 16nm, obtained device average mobility is 9.47e-3.
Claims (8)
1. a kind of insulating barrier method of modifying for inkjet printing OTFT, it is characterised in that comprise the following steps：
（1）Synthesize ATRP (ATRP) silane end initiator, the synthesis of described silane end initiator
Comprise the following steps：
Take dry triethylamine 7.2ml and 80ml tetrahydrofuran to mix respectively, be a liquid；The bromo- 2- methyl-propionyl bromides of 2-
5.92ml and 40ml tetrahydrofurans mix, and are b liquid；B liquid is slowly added dropwise in a liquid, reaction is filtered off after 3.8-4.1h is stirred at room temperature
Sediment in liquid, being poured into after tetrahydrofuran is evaporated in 100ml dichloromethane, mixed liquor is extracted with aqueous hydrochloric acid solution, and
Dried with anhydrous magnesium sulfate, finally vacuumize dry oily liquids, i.e. silane end initiator（3- aminopropyls）- triethoxy
Silane；
（2）Above ATRP silane end initiators are grown on the insulating barrier of substrate with solwution method, form ATRP initiator lists
Molecular layer, described solwution method comprise the following steps：Take the above-mentioned silane end initiators of 0.3ml be dissolved in 60-62ml without water beetle
In benzene, silicon chip is dipped in above-mentioned solution and is heated to 50 DEG C, heated 3.9-4.1h, moved to after stirring at room temperature, silicon chip is dipped in
12-12.5h is kept in solution, is put into ultrasonic 9-10min in 25-26ml toluene after taking out silicon chip, then use acetone and first successively
Each ultrasonic 4-5min of alcohol, finally dry up silicon chip with nitrogen；
（3）Trigger monomer that ATRP occurs in substrate surface ATRP initiators monolayer, pass through polymerization
React and form decorative layer of the one layer of polymeric molecular brush as inkjet printing OTFT gate insulation layer in substrate surface；
Concrete technology step is：By the silicon chip that surface A TRP initiator monolayers are prepared above by solwution method be put into rubber every
In the flask of film, extraction nitrogen 3 times, nitrogen atmosphere protection；Respectively take 54ml styrene, 220mg copper bromides and 66ml anhydrous benzenes
Methyl ether is in another flask with diaphragm of rubber, and inflated with nitrogen 1h；Take 628 μ L PMDETA to add in the mixed system, mix
Liquid is stirred at 100 DEG C until become uniform, with syringe by mixed liquor inject it is previous be placed with the flask of initiator silicon chip, 100
It polymerize 12h at DEG C, and adds 92 μ L radical initiator ethyl -2- bromo acid esters, polymerization is rushed after terminating with dichloromethane
Wash silicon chip and ATRP crystal grain, then by silicon chip tetrahydrofuran surname extraction 24H；
（4）By controlling polymerization time, the thickness of different degrees of change polymer molecule brush decorative layer, to regulate and control inkjet printing
Semiconductor ink droplet single-point film size, pattern and crystal habit, so as to regulate and control the electric property of inkjet printing single-point device.
2. the insulating barrier method of modifying according to claim 1 for inkjet printing OTFT, its feature exists
In described substrate is silicon chip and glass substrate.
3. the insulating barrier method of modifying according to claim 1 for inkjet printing OTFT, its feature exists
In the thickness of polymer insulation layer can be controlled by polymerization time, and described polymerization time is 6-24h, described polymer insulation
Tunic thickness is 4-16nm.
4. the insulating barrier method of modifying according to claim 1 for inkjet printing OTFT, its feature exists
In described insulating polymer molecule brush material is polystyrene, gathered（Methyl）Esters of acrylic acid, polyacrylonitrile, polydiene
The block copolymer of class rubber and above polymer.
5. the insulating barrier method of modifying according to claim 1 for inkjet printing OTFT, its feature exists
In the solvent of described semiconductor ink droplet solution is dichloro-benzenes, tetrahydronaphthalene or methyl phenyl ethers anisole.
6. a kind of OTFT, it is characterised in that including the gate electrode, gate insulation layer, polymer molecule being arranged in order
Brush decorative layer, source-drain electrode and organic semiconductor layer, wherein, the polymer molecule brush decorative layer passes through claim 1 institute
Method preparation is stated, organic semiconductor layer is made by inkjet printing.
7. OTFT according to claim 6, it is characterised in that the semiconductor of described organic semiconductor layer
Material is small molecule type semiconductor, double comprising 6,13-（Tri isopropyl silane ethyl-acetylene base）Pentacene (TIPS- pentacenes), 2,
7- didecyls-[1] benzothiophene [3,2-b] [1]-benzothiophene (BTBT).
8. OTFT according to claim 6, it is characterised in that described source-drain electrode by gold, silver, aluminium or
Person's graphene is made.
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| CN107195781B (en) * | 2017-05-24 | 2020-07-07 | 华南师范大学 | PMMA-doped small molecule-based high-mobility transistor and preparation method thereof |
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| CN101267020A (en) * | 2008-04-29 | 2008-09-17 | 友达光电股份有限公司 | Organic film transistor and its making method |
| CN102623639A (en) * | 2012-04-10 | 2012-08-01 | 合肥工业大学 | Method for manufacturing organic thin film transistor realizing patterning and automatic-modification interface in one step |
| CN103762314A (en) * | 2013-12-31 | 2014-04-30 | 合肥工业大学 | Insulating layer decorating method for printing organic thin-film transistor in ink jet mode |
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| TW201034269A (en) * | 2009-03-13 | 2010-09-16 | Nat Univ Tsing Hua | Organic thin film transistor which contains azole complex to dielectric insulating layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101267020A (en) * | 2008-04-29 | 2008-09-17 | 友达光电股份有限公司 | Organic film transistor and its making method |
| CN102623639A (en) * | 2012-04-10 | 2012-08-01 | 合肥工业大学 | Method for manufacturing organic thin film transistor realizing patterning and automatic-modification interface in one step |
| CN103762314A (en) * | 2013-12-31 | 2014-04-30 | 合肥工业大学 | Insulating layer decorating method for printing organic thin-film transistor in ink jet mode |
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