CN113050329A - Polyimide type reworking liquid for alignment film - Google Patents
Polyimide type reworking liquid for alignment film Download PDFInfo
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- CN113050329A CN113050329A CN201911378599.1A CN201911378599A CN113050329A CN 113050329 A CN113050329 A CN 113050329A CN 201911378599 A CN201911378599 A CN 201911378599A CN 113050329 A CN113050329 A CN 113050329A
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- alignment film
- type alignment
- polyimide
- rework
- liquid
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- 239000007788 liquid Substances 0.000 title claims abstract description 67
- 239000004642 Polyimide Substances 0.000 title claims abstract description 33
- 229920001721 polyimide Polymers 0.000 title claims abstract description 33
- 150000001412 amines Chemical class 0.000 claims abstract description 19
- 239000000654 additive Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims abstract description 11
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 9
- XRIBIDPMFSLGFS-UHFFFAOYSA-N 2-(dimethylamino)-2-methylpropan-1-ol Chemical compound CN(C)C(C)(C)CO XRIBIDPMFSLGFS-UHFFFAOYSA-N 0.000 claims abstract description 7
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims abstract description 7
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims abstract description 5
- BFSVOASYOCHEOV-UHFFFAOYSA-N 2-diethylaminoethanol Chemical compound CCN(CC)CCO BFSVOASYOCHEOV-UHFFFAOYSA-N 0.000 claims abstract description 5
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 claims abstract description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000003960 organic solvent Substances 0.000 claims description 15
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 14
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 9
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims description 7
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 7
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 7
- 150000001408 amides Chemical class 0.000 claims description 7
- 239000000174 gluconic acid Substances 0.000 claims description 7
- 235000012208 gluconic acid Nutrition 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- SUHOOTKUPISOBE-UHFFFAOYSA-N O-phosphoethanolamine Chemical compound NCCOP(O)(O)=O SUHOOTKUPISOBE-UHFFFAOYSA-N 0.000 claims description 5
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 3
- XIPFMBOWZXULIA-UHFFFAOYSA-N pivalamide Chemical compound CC(C)(C)C(N)=O XIPFMBOWZXULIA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 159000000000 sodium salts Chemical class 0.000 claims description 3
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 abstract description 36
- 230000000694 effects Effects 0.000 abstract description 15
- 230000007797 corrosion Effects 0.000 abstract description 14
- 238000005260 corrosion Methods 0.000 abstract description 14
- 230000001988 toxicity Effects 0.000 abstract description 3
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 56
- 239000011521 glass Substances 0.000 description 44
- 238000000034 method Methods 0.000 description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 238000002386 leaching Methods 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 238000007664 blowing Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 5
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 239000012964 benzotriazole Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical class [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
- G02F1/133711—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by organic films, e.g. polymeric films
- G02F1/133723—Polyimide, polyamide-imide
Abstract
In order to overcome the problems of insufficient treatment of a TMAH system on PI residues, strong corrosion on Cu, PS and ITO and short service life in a PI type alignment film in the prior art, the invention provides a polyimide type alignment film reworking liquid, which comprises organic amine, a solvent and an additive, wherein the organic amine is selected from one or more of 2-dimethylamino-2-methylpropanol, diethylaminoethanol, 2-amino-2-methyl-propanol, 1-amino-2-propanol, 3-diethylaminopropylamine, triisopropanolamine and diethylenetriamine. The polyimide type alignment film reworking liquid provided by the invention has an excellent effect of PI residue dropping treatment on a PI type alignment film, has low corrosivity on Cu, PS and ITO, and is low in toxicity, small in harm and longer in service life.
Description
Technical Field
The invention belongs to the field of reworking of TFT-LCD (thin film transistor-liquid crystal display) coating films, and particularly relates to a reworking liquid for a polyimide type alignment film.
Background
As a key material and structure for realizing liquid crystal alignment in a thin film transistor liquid crystal display (TFT-LCD), the yield of an alignment film is an important parameter in a CELL process and even a whole Liquid Crystal Display (LCD) production line. If the alignment film has an unqualified quality, such as an uneven thickness of the alignment film and an unqualified baking, the whole panel is directly scrapped. Since the front-end process structures of the alignment films are all qualified, the direct scrapping of the panel causes great waste, and the production cost is increased.
In order to reduce the cost, some manufacturers propose to Rework Thin Film Transistor (TFT) glass or Color Filter (CF) glass with unqualified alignment film by polyimide alignment film Rework (PI Rework) liquid, remove the unqualified alignment film, and put the unqualified alignment film into the alignment film manufacturing process in the CELL process again to keep the front-end process, thereby saving the production cost.
At present, a tetramethyl ammonium hydroxide (TMAH) system is mostly used in the PIRework liquid. TMAH is organic base with very strong alkalinity, and can be reduced to ppb (part per billion) level due to low metal ion content, and the TMAH has wider application in the electronic field. The PI reworking liquid of the system has a good reworking effect on the alignment film, but the problem of precipitation caused by the interaction of TMAH and N-Methyl pyrrolidone (NMP) used in the production process of the PI type alignment film is solved, and the PI reworking liquid has strong corrosivity on a Cu substrate, Polystyrene (PS) and nano Indium Tin Oxides (ITO). Moreover, due to the strong hygroscopicity of TMAH, the liquid medicine is easy to lose efficacy, and the service life is short. In addition, TMAH is highly toxic, and is poisoned and killed by TMAH sputtering in korea, japan, and the like, and the TMAH is relatively expensive.
Disclosure of Invention
The invention aims to solve the technical problems that in the prior art, a TMAH system in a PI type alignment film cannot treat PI residues sufficiently, and the polyimide type alignment film has strong corrosivity on Cu, PS and ITO and short service life.
The technical scheme adopted by the invention for solving the problems is as follows:
the invention provides a polyimide type alignment film reworking liquid, which comprises the following components:
organic amine, solvent and additive, wherein the organic amine comprises one or more of 2-dimethylamino-2-methylpropanol, diethylaminoethanol, 2-amino-2-methyl-propanol, 1-amino-2-propanol, 3-diethylaminopropylamine, triisopropanolamine and diethylenetriamine.
Optionally, the content of the organic amine is 5% to 30% by taking the total weight of the polyimide type alignment film reworking liquid as 100%. More preferably, the organic amine content is 8% to 20%.
Optionally, the additive comprises one or more of gluconic acid and potassium or sodium salt thereof, ethanolamine phosphate, 2-mercaptobenzothiazole, methylbenzotriazole, benzotriazole and polyethylene glycol PEG 400-PEG 2000.
Optionally, the content of the additive is 0.1-1% by taking the total weight of the polyimide type alignment film reworking liquid as 100%.
Optionally, the content of the solvent is 69% -94.9% by taking the total weight of the polyimide type alignment film reworking liquid as 100%.
Optionally, the solvent includes water and an organic solvent that is miscible with water, and the content of the organic solvent is 10% to 40% and the content of the water is 29% to 84.9% based on 100% of the total weight of the rework liquid of the polyimide-type alignment film.
Optionally, the organic solvent includes one or both of an amide substance and an alcohol substance.
Optionally, the amide-based substance comprises one or more of dimethylformamide, dimethylacetamide, N-methylformamide and dimethylpropionamide, and the alcohol-based substance comprises one or more of diethylene glycol, dipropylene glycol, diethylene glycol, ethylene glycol, glycerol, diethylene glycol monomethyl ether and diethylene glycol monobutyl ether.
The polyimide type alignment film reworking liquid provided by the invention is prepared by organic amine, solvent and additive with optimized formula, the problem of precipitation caused by interaction of TMAH and NMP in the PI type alignment film process can be effectively avoided by replacing TMAH, the PI residue of the PI type alignment film is subjected to falling treatment by the reworking liquid, the PI residue of the PI type alignment film is subjected to falling treatment, the corrosion to Cu, PS and ITO is low, the toxicity is low, the hazard is small, and the service life is longer.
Drawings
Fig. 1 is a view of an Optical Microscope (OM) before reworking of a PI alignment film in example 1 provided by the present invention;
fig. 2 is a microscope image of OM after rework of the PI alignment film in example 1 provided by the present invention;
FIG. 3 is a microscope image of OM before soaking CF glass in example 1 provided by the present invention;
FIG. 4 is a microscope image of OM of example 1, wherein the CF glass has been treated with a rework fluid;
FIG. 5 is a microscope image of an OM of a CF glass provided by the present invention treated with deionized water;
FIG. 6 is a microscope image of OM before soaking TFT glass in example 1 provided by the present invention;
FIG. 7 is a microscope image of OM of example 1, processed with rework fluid;
fig. 8 is a microscope image of OM of a TFT glass treated with deionized water provided by the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a polyimide type alignment film reworking liquid, which comprises the following components:
organic amine, solvent and additive, wherein the organic amine comprises one or more of 2-dimethylamino-2-methylpropanol, diethylaminoethanol, 2-amino-2-methyl-propanol, 1-amino-2-propanol, 3-diethylaminopropylamine triisopropanolamine and diethylenetriamine.
The polyimide type alignment film reworking liquid provided by the invention is prepared by organic amine, solvent and additive with optimized formula, the problem of precipitation caused by interaction of TMAH and NMP in the PI type alignment film process can be effectively avoided by replacing TMAH, the PI residue of the PI type alignment film is excellent in dropping effect, the corrosivity to Cu, PS and ITO is low, the toxicity is low, the hazard is small, and the service life is longer.
In some embodiments of the invention, the organic amine is selected from one or more of 2-dimethylamino-2-methylpropanol, diethylaminoethanol, 2-amino-2-methyl-propanol, 1-amino-2-propanol, 3-diethylaminopropylamine, triisopropanolamine, and diethylenetriamine.
In some embodiments of the present invention, the content of the organic amine is 5% to 30% based on 100% of the total weight of the rework liquid of the polyimide-type alignment film. More preferably, the organic amine content is 8% to 20%.
Through a large number of experiments, the content of the organic amine influences the reworking performance. The content of organic amine is too high, so that the metal layer is corroded or falls off, and the content is too low, so that the PI residue falling effect is poor, and the reworking is unqualified. Therefore, the proper content of the organic amine is selected, the corrosion to Cu, PS and ITO can be prevented, and the reworking performance can be improved.
In order to optimize the reworking performance of the invention, the reworking liquid also contains additives, the additives mainly prevent the corrosion or the falling off of the metal layer (the Cu layer and the ITO layer), and the selected additives have good wettability and chemical stability, so that the service life of the reworking liquid medicine can be prolonged. And the contact angle of the glass surface is reduced by selecting good additives, so that the hydrophilicity is judged by utilizing the surface contact angle, and the treatment effect or cleaning effect of the surface of the TFT glass or the CF glass is confirmed.
In some embodiments of the present invention, the additive contained in the polyimide type alignment film rework solution includes one or more of gluconic acid and potassium or sodium salt thereof, ethanolamine phosphate, 2-mercaptobenzothiazole, methylbenzotriazole, benzotriazole, and polyethylene glycol PEG400 to PEG 2000.
In some embodiments of the present invention, the content of the additive is 0.1% to 1% based on 100% of the total weight of the rework fluid of the polyimide type alignment film.
Through a large number of experiments, the inventor finds that if the content of the additive is lower than 0.1%, the effect of improving the reworking fluid is not obviously different. If the content of the additive is higher than 1%, compared with the addition of proper additive content, the effect is not obviously improved, and the waste is caused.
In some embodiments of the present invention, the content of the solvent is 69% to 94.9% based on 100% of the total weight of the rework liquid of the polyimide type alignment film.
Specifically, the solvent comprises water and an organic solvent which can be mutually dissolved with the water, the content of the organic solvent is 10% -40% and the content of the water is 29% -84.9% by taking the total weight of the polyimide type alignment film reworking liquid as 100%.
More preferably, the content of the organic solvent is 15% to 25%.
The organic solvent is selected from amides or alcohols which can be mutually dissolved with water, the higher the content of the organic solvent is, the more excellent the reworking effect on the PI type alignment film is theoretically, but the higher the content of the organic solvent can corrode Cu. The content of the organic solvent is selected to prevent the corrosion to Cu, and the reworking performance is excellent.
In some embodiments of the invention, the organic solvent comprises one or both of an amide-based material and an alcohol-based material.
Specifically, the amide substances comprise one or more of dimethylformamide, dimethylacetamide, N-methylformamide and dimethylpropionamide, and the alcohol substances comprise one or more of diethylene glycol, dipropylene glycol, diethylene glycol, ethylene glycol, glycerol, diethylene glycol monomethyl ether and diethylene glycol monobutyl ether.
The reworking performance of the PI alignment film is controlled by taking TFT and CF glass in the TFT-LCD manufacturing process as objects and adjusting the types and contents of organic amine, organic solvent, additives and the like. Setting the rework temperature to be 45-55 ℃, setting the rework time to be 3-6 min, leaching with pure water, and then purging with nitrogen. PI residues, Cu and ITO corrosion were evaluated under an OM microscope.
The present invention will be further illustrated by the following examples. It is to be understood that the present invention is not limited to the following embodiments, and methods are regarded as conventional methods unless otherwise specified. Materials are commercially available from the open literature unless otherwise specified.
Example 1
This example is provided to illustrate the rework liquid of polyimide type alignment film and the preparation and application methods thereof.
The reworking liquid for the polyimide type alignment film comprises the following components in percentage by weight:
2-dimethylamino-2-methylpropanol 8%
12 percent of diethylenetriamine
Diethylene glycol monomethyl ether 20%
Diethylene glycol 13%
Gluconic acid 0.5%
PEG400 0.3％
46.2 percent of water
The preparation and use method comprises the following steps:
(1) dissolving 2-dimethylamino-2-methylpropanol, diethylenetriamine, gluconic acid and PEG400 in a solvent of diethylene glycol monomethyl ether, diethylene glycol and water according to the weight percentage to prepare a reworking liquid;
(2) and (4) coating the reworking liquid on TFT or CF glass, setting the reworking temperature to be 50 ℃, setting the reworking time to be 4min, leaching with pure water, and then blowing with nitrogen, wherein the mark is S1.
Example 2
This example is provided to illustrate the rework liquid of polyimide type alignment film and the preparation and application methods thereof.
The reworking liquid for the polyimide type alignment film comprises the following components in percentage by weight:
3-diethylaminopropylamine 15%
Diethylene glycol monobutyl ether 20%
Diethylene glycol 20%
0.5 percent of 2-mercaptobenzothiazole
PEG600 0.2％
44.3 percent of water
The preparation and use method comprises the following steps:
(1) dissolving 3-diethylaminopropylamine, 2-mercaptobenzothiazole and PEG600 in a solvent of diethylene glycol monobutyl ether, diethylene glycol and water according to the weight percentage to prepare a rework liquid;
(2) and (4) coating the reworking liquid on TFT or CF glass, setting the reworking temperature to be 50 ℃, setting the reworking time to be 4min, leaching with pure water, and then blowing with nitrogen, wherein the mark is S2.
Example 3
This example is provided to illustrate the rework liquid of polyimide type alignment film and the preparation and application methods thereof.
The reworking liquid for the polyimide type alignment film comprises the following components in percentage by weight:
3-diethylaminopropylamine 30%
N-methylformamide 10%
Diethylene glycol 15%
Ethanolamine phosphate 0.5%
0.3 percent of methylbenzotriazole
44.2 percent of water
The preparation and use method comprises the following steps:
(1) dissolving 3-diethylaminopropylamine, ethanolamine phosphate and methylbenzotriazole in a solvent of N-methylformamide, diethylene glycol and water according to the weight percentage to prepare a reworking liquid;
(2) and (4) coating the reworking liquid on TFT or CF glass, setting the reworking temperature to be 50 ℃, setting the reworking time to be 4min, leaching with pure water, and then blowing with nitrogen, wherein the mark is S3.
Example 4
This example is provided to illustrate the rework liquid of polyimide type alignment film and the preparation and application methods thereof.
The reworking liquid for the polyimide type alignment film comprises the following components in percentage by weight:
2-amino-2-methyl-propanol 2%
6 percent of diethylenetriamine
Diethylene glycol monomethyl ether 20%
Diethylene glycol 19%
Gluconic acid 0.5%
PEG400 0.2％
52.3 percent of water
The preparation and use method comprises the following steps:
(1) dissolving 2-amino-2-methyl-propanol, diethylenetriamine, gluconic acid and PEG400 in a solvent of diethylene glycol monomethyl ether, diethylene glycol and water according to the weight percentage to prepare a reworking liquid;
(2) and (4) coating the reworking liquid on TFT or CF glass, setting the reworking temperature to be 50 ℃, setting the reworking time to be 4min, leaching with pure water, and then blowing with nitrogen, wherein the mark is S4.
Example 5
This example is provided to illustrate the rework liquid of polyimide type alignment film and the preparation and application methods thereof.
The reworking liquid for the polyimide type alignment film comprises the following components in percentage by weight:
3-diethylaminopropylamine 25%
Diethylene glycol monobutyl ether 20%
10 percent of diethylene glycol
0.05 percent of 2-mercaptobenzothiazole
PEG600 0.02％
44.3 percent of water
The preparation and use method comprises the following steps:
(1) dissolving 3-diethylaminopropylamine, 2-mercaptobenzothiazole and PEG600 in a solvent of diethylene glycol monobutyl ether, diethylene glycol and water according to the weight percentage to prepare a rework liquid;
(2) and (4) coating the reworking liquid on TFT or CF glass, setting the reworking temperature to be 50 ℃, setting the reworking time to be 4min, leaching with pure water, and then blowing with nitrogen, wherein the mark is S5.
Comparative example 1
This comparative example is used for comparative illustration of the polyimide type alignment film rework fluid and the methods of making and using the same disclosed in the present invention.
The comparative polyimide type alignment film reworking liquid comprises the following components in percentage by weight:
TMAH 8％
diethylene glycol monobutyl ether 25%
Dipropylene glycol 20%
0.5 percent of methylbenzotriazole
46.5 percent of water
The preparation and use method comprises the following steps:
(1) dissolving TMAH and methylbenzotriazole in a solvent of diethylene glycol monobutyl ether, dipropylene glycol and water according to the weight percentage to prepare a rework liquid;
(2) and coating the reworking liquid on TFT or CF glass, setting the reworking temperature to be 50 ℃ and the reworking time to be 4min, leaching with pure water, and then blowing with nitrogen, wherein the label is D1.
Performance testing
1. The performance tests were performed on the S1 to S5 prepared above and the comparative sample D1. The numbers of peeling of PI residues, NMP residues, Cu corrosion and ITO corrosion were observed under an OM microscope for S1 to S5 and comparative sample D1 prepared as described above, and the service life of the rework liquid and the contact angle of TFT or CF glass were tested.
(1) PI residual
The samples S1 to S5 of the TFT or CF glass prepared as described above and the comparative sample D1 were examined for PI remaining under OM microscope. Wherein A represents substantially no residue; b indicates slight residue; c indicates severe residue.
(2) Corrosion of Cu
The above-prepared S1 to S5 and comparative sample D1 of the TFT glass sample were observed for Cu corrosion under an OM microscope. Wherein A represents substantially no corrosion; b represents slight corrosion; c indicates severe corrosion.
(3) Etching of ITO
The numbers of ITO corrosion drops were observed under an OM microscope for S1 to S5 of the TFT or CF glass samples prepared as described above and for a comparative sample D1. Wherein, the percentage ratio represents the ITO falling number to the total ITO number.
(4) NMP residue
The TFT or CF glass samples prepared as described above, S1 to S5, and comparative sample D1 were examined for NMP residue under OM microscope. Wherein A represents substantially no residue; b indicates slight residue; c indicates severe residue.
(5) Service life
The reworking liquids used in S1 to S5 of the TFT or CF glass samples prepared as described above and comparative sample D1 were tested. The service life takes the time from continuous test to performance reduction as the evaluation standard under the condition that the liquid medicine is placed in an open place. The life is represented by a number of days or more.
(6) Contact angle of CF glass
Testing S1-S5 of the CF glass sample soaked by the reworking liquid and a comparison sample D1, obtaining an outline image of the liquid drop through an OM microscope lens and a camera, and calculating the contact angle of the liquid drop in the image by using digital image processing and an algorithm.
The test results obtained are filled in Table 1.
TABLE 1
From the test results in table 1, it can be seen that the rework liquid for polyimide type alignment films of the present invention has excellent peeling effect on PI residues, low corrosivity on Cu and ITO, long service life, and significantly reduced contact angle on the glass surface after being soaked in the rework liquid. In comparative example 1, the reworking using TMAH has strong corrosivity to ITO, NMP residue exists, the service life of the reworking liquid is short, and the contact angle of the glass surface is large.
2. (1) appearance
The PI type alignment films before and after reworking of sample S1 were observed with an OM microscope, respectively.
Fig. 1 shows the PI alignment film before the PI alignment film is reworked in example 1, and fig. 2 shows the PI alignment film after the PI alignment film is reworked in example 1, according to the comparison, the PI residues are already clearly dropped off.
(2) Contact angle of CF glass
The CF glass of sample S1 was observed with an OM microscope before immersion, after treatment with rework solution, and after treatment with only deionized water, respectively, and the contact angle of the glass surface was tested.
Fig. 3 shows the CF glass before immersion in example 1, and the contact angle is 74.1 °.
FIG. 4 shows the CF glass treated with the rework liquid of example 1, the contact angle being 28.5 °.
Fig. 5 is a CF glass treated with deionized water and having a contact angle of 70.2 °.
Comparing fig. 3, fig. 4 and fig. 5, it is found that the CF glass treated by the reworking liquid has a smaller contact angle, which indicates that the CF glass treated by the reworking liquid has a good wetting effect and a good PI residual treatment effect.
(3) Contact angle of TFT glass
The TFT glass of sample S1 was observed with an OM microscope before immersion, after treatment with rework solution, and after treatment with only deionized water, and the contact angle of the glass surface was tested.
FIG. 6 shows the TFT glass before immersion in example 1, in which the contact angle is 75.3 °.
FIG. 7 shows the TFT glass treated with the rework liquid of example 1, with a contact angle of 40.6 deg..
Fig. 8 is a TFT glass treated with deionized water and the contact angle is 72.4 °.
Comparing fig. 6, fig. 7 and fig. 8, it is found that the TFT glass treated by the rework liquid has a smaller contact angle, which indicates that the TFT glass treated by the rework liquid has a good wetting effect and the TFT glass has a good PI residual treatment effect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. The reworking liquid for the polyimide type alignment film is characterized by comprising the following components:
the organic amine comprises one or more of 2-dimethylamino-2-methylpropanol, diethylaminoethanol, 2-amino-2-methyl-propanol, 1-amino-2-propanol, 3-diethylaminopropylamine, triisopropanolamine and diethylenetriamine.
2. The polyimide-type alignment film rework fluid of claim 1, wherein the organic amine is present in an amount of 5% to 30% based on 100% of the total weight of the polyimide-type alignment film rework fluid.
3. The reworking liquid of a polyimide-type alignment film according to claim 1, wherein the additive comprises one or more of gluconic acid and potassium or sodium salt thereof, ethanolamine phosphate, 2-mercaptobenzothiazole, methylbenzotriazole, benzotriazol and polyethylene glycol PEG 400-PEG 2000.
4. The polyimide-type alignment film rework fluid of claim 1 or 3, wherein the additive is present in an amount of 0.1% to 1% based on 100% of the total weight of the polyimide-type alignment film rework fluid.
5. The polyimide-type alignment film rework fluid of claim 1, wherein the content of the solvent is 69% to 94.9% based on 100% of the total weight of the polyimide-type alignment film rework fluid.
6. The rework liquid of claim 5, wherein the solvent comprises water and an organic solvent miscible with water, and the content of the organic solvent is 10% to 40% and the content of the water is 29% to 84.9% based on 100% of the total weight of the rework liquid of polyimide type alignment film.
7. The rework liquid of claim 6, wherein the organic solvent comprises one or both of an amide-based substance and an alcohol-based substance.
8. The polyimide-type alignment film rework fluid of claim 7, wherein the amide-based substance comprises one or more of dimethylformamide, dimethylacetamide, N-methylformamide, and dimethylpropionamide;
the alcohol substance comprises one or more of diethylene glycol, dipropylene glycol, diethylene glycol, ethylene glycol, glycerol, diethylene glycol monomethyl ether and diethylene glycol monobutyl ether.
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