CN107164762A - A kind of AMOLED acid etching solution of low surface tension and its preparation technology - Google Patents

A kind of AMOLED acid etching solution of low surface tension and its preparation technology Download PDF

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Publication number
CN107164762A
CN107164762A CN201710354626.6A CN201710354626A CN107164762A CN 107164762 A CN107164762 A CN 107164762A CN 201710354626 A CN201710354626 A CN 201710354626A CN 107164762 A CN107164762 A CN 107164762A
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Prior art keywords
acid
surface tension
low surface
stirring
etching solution
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白航空
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Hefei Huike Precision Mould Co Ltd
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Hefei Huike Precision Mould Co Ltd
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Priority to CN201710354626.6A priority Critical patent/CN107164762A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/16Acidic compositions

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

The invention discloses a kind of AMOLED acid etching solutions of low surface tension, it is made up of the raw material of following percentage by weight:Nitric acid 23 25%, hydrochloric acid 11 13%, acetic acid 7 9%, inorganic salts chloride 1.2 1.8%, ammonium fluoride 8.5 9.4%, surfactant 11.2 14.5%, additive 5 8% and deionized water.Compared with prior art, the present invention adds ammonium fluoride and suitable additive in etching solution, and any metal ion and anion are not introduced, the oxidation layer surface noresidue after etching, and can assign etching solution relatively low surface tension, increases etching solution permeability;Surfactant has the property of high surface hydrophobic oleophobic, compared with the other surfaces activating agent of equivalent, can greatly reduce the surface tension of solution, therefore its consumption is few, and production cost is relatively low.

Description

A kind of AMOLED acid etching solution of low surface tension and its preparation technology
Technical field
The present invention relates to etching solution technical field, and in particular to a kind of AMOLED with the acid etching solution of low surface tension and its Preparation technology.
Background technology
Substantial amounts of film, thin layer are provided with AMOLED substrates, so in order to prevent undesirable electricity between these Short circuit, is that etching outline is equably tilted preferably by the cut-out side of the substrate after etching, and lower section is wider than top, is blunted cone shape Shape.This is due to that the difference in height between the film layer of more than 2 formed can subtract in the case that etching outline is blunted cone shape It is few.Engraving method has the dry-etching using gas and the Wet-type etching using etching solution, although Wet-type etching has the disadvantage in that, It is equal to mask and substrate without etching environment is maintained into high vacuum state but the equipment investment expense needed for its process is low There is excellent etching selectivity.Existing etching solution complicated components, for main component nitric acid and ammonium fluoride, surfactant Active amount is larger, and production cost is higher;In addition, in etching solution nitric acid and fluorination ammonium concentration it is higher when, general non-ionic surface Activating agent is difficult to dissolve, it is impossible to which the surface tension to etching solution is adjusted, and permeability is relatively weak, it is difficult to be etched into very small Aperture.
The content of the invention
The present invention is intended to provide a kind of the AMOLED acid etching solution of low surface tension and its preparation technology.
The present invention provides following technical scheme:
A kind of AMOLED acid etching solutions of low surface tension, it is made up of the raw material of following percentage by weight:Nitric acid 23-25%, hydrochloric acid 11-13%, acetic acid 7-9%, inorganic salts chloride 1.2-1.8%, ammonium fluoride 8.5-9.4%, surface-active Agent 11.2-14.5%, additive 5-8% and deionized water.
The surfactant is N- alkyl glucose amides, polyisobutene/maleic anhydride derivative, N- aryloxy group polyhydroxys One or more of mixtures in base-fatty acid amide.
The inorganic salts chloride is potassium chloride, and the purity of the potassium chloride is higher than 95%.
The additive is that polyethyleneglycol perfluorinated nonene base ether, perfluoro hexyl sulfonic acid polyglycerol ester, octylame, polyglycereol are complete One or more in fluorine nonenyl ether, polyethylene glycol perfluorinated nonene ylmethyl ether, perfluoro hexyl sulfonic acid macrogol ester.
The deionized water is at least 22 megaohms in 25 DEG C of resistivity.
A kind of AMOLED preparation technologies of the acid etching solution of low surface tension, comprise the following steps:
(1) strong-acid ion exchange resin is added separately in nitric acid, hydrochloric acid and acetic acid, then stirring mixing filters out Strong-acid ion exchange resin, removes the foreign ion in nitric acid, hydrochloric acid and acetic acid;
(2) 1/2 deionized water is added in material-compound tank, stirring is lower to add nitric acid, hydrochloric acid and acetic acid that above-mentioned steps are obtained, After being mixed evenly, the lower addition inorganic salts chloride of stirring and ammonium fluoride are well mixed;
(3) toward addition surfactant and additive in the mixed solution mixed, remaining deionized water is then added, is stirred Mix well mixed;
(4) mixture obtained above is passed through into filter to be filtered, obtains the etching solution.
It is in the state of normal temperature, normal pressure that the strong-acid ion exchange resin is mixed with nitric acid, hydrochloric acid and acetic acid Carry out, the speed of stirring is 60-85r/min, and the time of stirring is 10min.
The stirring is mechanical agitation or magnetic agitation.
The number of times of the filtering is more than twice, and the micro-filtration membrane aperture of the filter is 0.05-0.10 μm.
Compared with prior art, the beneficial effects of the invention are as follows:The present invention adds ammonium fluoride and suitable in etching solution Additive, any metal ion and anion are not introduced, the oxidation layer surface noresidue after etching, and it is relatively low to assign etching solution Surface tension, increase etching solution permeability;Surfactant has the property of high surface hydrophobic oleophobic, with equivalent its He compares surfactant, can greatly reduce the surface tension of solution, therefore its consumption is few, and production cost is relatively low.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all Belong to the scope of protection of the invention.
A kind of AMOLED of the embodiment 1 acid etching solutions of low surface tension, it is the raw material group by following percentage by weight Into:Nitric acid 23%, hydrochloric acid 11%, acetic acid 7%, inorganic salts chloride 1.2%, ammonium fluoride 8.5%, surfactant 11.2%, Additive 5% and deionized water.
The surfactant is N- alkyl glucose amides, polyisobutene/maleic anhydride derivative, N- aryloxy group polyhydroxys One or more of mixtures in base-fatty acid amide.
The inorganic salts chloride is potassium chloride, and the purity of the potassium chloride is higher than 95%.
The additive is that polyethyleneglycol perfluorinated nonene base ether, perfluoro hexyl sulfonic acid polyglycerol ester, octylame, polyglycereol are complete One or more in fluorine nonenyl ether, polyethylene glycol perfluorinated nonene ylmethyl ether, perfluoro hexyl sulfonic acid macrogol ester.
The deionized water is at least 22 megaohms in 25 DEG C of resistivity.
A kind of AMOLED preparation technologies of the acid etching solution of low surface tension, comprise the following steps:
(1) strong-acid ion exchange resin is added separately in nitric acid, hydrochloric acid and acetic acid, then stirring mixing filters out Strong-acid ion exchange resin, removes the foreign ion in nitric acid, hydrochloric acid and acetic acid;
(2) 1/2 deionized water is added in material-compound tank, stirring is lower to add nitric acid, hydrochloric acid and acetic acid that above-mentioned steps are obtained, After being mixed evenly, the lower addition inorganic salts chloride of stirring and ammonium fluoride are well mixed;
(3) toward addition surfactant and additive in the mixed solution mixed, remaining deionized water is then added, is stirred Mix well mixed;
(4) mixture obtained above is passed through into filter to be filtered, obtains the etching solution.
It is in the state of normal temperature, normal pressure that the strong-acid ion exchange resin is mixed with nitric acid, hydrochloric acid and acetic acid Carry out, the speed of stirring is 60-85r/min, and the time of stirring is 10min.
The stirring is mechanical agitation or magnetic agitation.
The number of times of the filtering is more than twice, and the micro-filtration membrane aperture of the filter is 0.05-0.10 μm.
A kind of AMOLED of the embodiment 2 acid etching solutions of low surface tension, it is the raw material group by following percentage by weight Into:Nitric acid 25%, hydrochloric acid 13%, acetic acid 9%, inorganic salts chloride 1.8%, ammonium fluoride 9.4%, surfactant 14.5%, Additive 8% and deionized water.
The surfactant is N- alkyl glucose amides, polyisobutene/maleic anhydride derivative, N- aryloxy group polyhydroxys One or more of mixtures in base-fatty acid amide.
The inorganic salts chloride is potassium chloride, and the purity of the potassium chloride is higher than 95%.
The additive is that polyethyleneglycol perfluorinated nonene base ether, perfluoro hexyl sulfonic acid polyglycerol ester, octylame, polyglycereol are complete One or more in fluorine nonenyl ether, polyethylene glycol perfluorinated nonene ylmethyl ether, perfluoro hexyl sulfonic acid macrogol ester.
The deionized water is at least 22 megaohms in 25 DEG C of resistivity.
A kind of AMOLED preparation technologies of the acid etching solution of low surface tension, comprise the following steps:
(1) strong-acid ion exchange resin is added separately in nitric acid, hydrochloric acid and acetic acid, then stirring mixing filters out Strong-acid ion exchange resin, removes the foreign ion in nitric acid, hydrochloric acid and acetic acid;
(2) 1/2 deionized water is added in material-compound tank, stirring is lower to add nitric acid, hydrochloric acid and acetic acid that above-mentioned steps are obtained, After being mixed evenly, the lower addition inorganic salts chloride of stirring and ammonium fluoride are well mixed;
(3) toward addition surfactant and additive in the mixed solution mixed, remaining deionized water is then added, is stirred Mix well mixed;
(4) mixture obtained above is passed through into filter to be filtered, obtains the etching solution.
It is in the state of normal temperature, normal pressure that the strong-acid ion exchange resin is mixed with nitric acid, hydrochloric acid and acetic acid Carry out, the speed of stirring is 60-85r/min, and the time of stirring is 10min.
The stirring is mechanical agitation or magnetic agitation.
The number of times of the filtering is more than twice, and the micro-filtration membrane aperture of the filter is 0.05-0.10 μm.
A kind of AMOLED of the embodiment 3 acid etching solutions of low surface tension, it is the raw material group by following percentage by weight Into:Nitric acid 24%, hydrochloric acid 12%, acetic acid 8%, inorganic salts chloride 1.5%, ammonium fluoride 8.8%, surfactant 12.6%, Additive 7% and deionized water.
The surfactant is N- alkyl glucose amides, polyisobutene/maleic anhydride derivative, N- aryloxy group polyhydroxys One or more of mixtures in base-fatty acid amide.
The inorganic salts chloride is potassium chloride, and the purity of the potassium chloride is higher than 95%.
The additive is that polyethyleneglycol perfluorinated nonene base ether, perfluoro hexyl sulfonic acid polyglycerol ester, octylame, polyglycereol are complete One or more in fluorine nonenyl ether, polyethylene glycol perfluorinated nonene ylmethyl ether, perfluoro hexyl sulfonic acid macrogol ester.
The deionized water is at least 22 megaohms in 25 DEG C of resistivity.
A kind of AMOLED preparation technologies of the acid etching solution of low surface tension, comprise the following steps:
(1) strong-acid ion exchange resin is added separately in nitric acid, hydrochloric acid and acetic acid, then stirring mixing filters out Strong-acid ion exchange resin, removes the foreign ion in nitric acid, hydrochloric acid and acetic acid;
(2) 1/2 deionized water is added in material-compound tank, stirring is lower to add nitric acid, hydrochloric acid and acetic acid that above-mentioned steps are obtained, After being mixed evenly, the lower addition inorganic salts chloride of stirring and ammonium fluoride are well mixed;
(3) toward addition surfactant and additive in the mixed solution mixed, remaining deionized water is then added, is stirred Mix well mixed;
(4) mixture obtained above is passed through into filter to be filtered, obtains the etching solution.
It is in the state of normal temperature, normal pressure that the strong-acid ion exchange resin is mixed with nitric acid, hydrochloric acid and acetic acid Carry out, the speed of stirring is 60-85r/min, and the time of stirring is 10min.
The stirring is mechanical agitation or magnetic agitation.
The number of times of the filtering is more than twice, and the micro-filtration membrane aperture of the filter is 0.05-0.10 μm.
It is obvious to a person skilled in the art that the invention is not restricted to the details of the one exemplary embodiment, Er Qie In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit is required rather than the explanation is limited, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.Although not each moreover, it will be appreciated that the present specification is described in terms of embodiments Embodiment is only comprising an independent technical scheme, and this narrating mode of specification is only this area for clarity Technical staff should be using specification as an entirety, and the technical solutions in the various embodiments may also be suitably combined, forms this Art personnel may be appreciated other embodiment.

Claims (9)

1. a kind of AMOLED acid etching solutions of low surface tension, it is characterised in that it is by the raw material of following percentage by weight Composition:Nitric acid 23-25%, hydrochloric acid 11-13%, acetic acid 7-9%, inorganic salts chloride 1.2-1.8%, ammonium fluoride 8.5-9.4%, Surfactant 11.2-14.5%, additive 5-8% and deionized water.
2. a kind of AMOLED according to claim 1 acid etching solutions of low surface tension, it is characterised in that:The surface Activating agent is in N- alkyl glucose amides, polyisobutene/maleic anhydride derivative, N- aryloxy polyhydroxies-fatty acid amide One or more of mixtures.
3. a kind of AMOLED according to claim 1 acid etching solutions of low surface tension, it is characterised in that:It is described Inorganic salts chloride is potassium chloride, and the purity of the potassium chloride is higher than 95%.
4. a kind of AMOLED according to claim 1 acid etching solutions of low surface tension, it is characterised in that:The addition Agent is polyethyleneglycol perfluorinated nonene base ether, perfluoro hexyl sulfonic acid polyglycerol ester, octylame, polyglycereol perfluorinated nonene base ether, poly- second One or more in glycol perfluorinated nonene ylmethyl ether, perfluoro hexyl sulfonic acid macrogol ester.
5. a kind of AMOLED according to claim 1 acid copper etchant solutions of low surface tension, it is characterised in that:It is described to go Ionized water is at least 22 megaohms in 25 DEG C of resistivity.
6. a kind of AMOLED as claimed in claim 1 preparation technologies of the acid etching solution of low surface tension, it is characterised in that: Comprise the following steps:
(1) strong-acid ion exchange resin is added separately in nitric acid, hydrochloric acid and acetic acid, then stirring mixing filters out strong acid Property ion exchange resin, remove the foreign ion in nitric acid, hydrochloric acid and acetic acid;
(2) 1/2 deionized water is added in material-compound tank, stirring is lower to add nitric acid, hydrochloric acid and acetic acid that above-mentioned steps are obtained, mixing After stirring, the lower addition inorganic salts chloride of stirring and ammonium fluoride are well mixed;
(3) toward addition surfactant and additive in the mixed solution mixed, remaining deionized water is then added, stirring is mixed Close uniform;
(4) mixture obtained above is passed through into filter to be filtered, obtains the etching solution.
7. a kind of AMOLED according to claim 6 preparation technologies of the acid etching solution of low surface tension, its feature exists In:The strong-acid ion exchange resin is mixed with nitric acid, hydrochloric acid and acetic acid to be carried out in the state of normal temperature, normal pressure, The speed of stirring is 60-85r/min, and the time of stirring is 10min.
8. a kind of AMOLED according to claim 6 preparation technologies of the acid etching solution of low surface tension, its feature exists In:The stirring is mechanical agitation or magnetic agitation.
9. a kind of AMOLED according to claim 6 preparation technologies of the acid etching solution of low surface tension, its feature exists In:The number of times of the filtering is more than twice, and the micro-filtration membrane aperture of the filter is 0.05-0.10 μm.
CN201710354626.6A 2017-05-19 2017-05-19 A kind of AMOLED acid etching solution of low surface tension and its preparation technology Pending CN107164762A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113322072A (en) * 2021-06-25 2021-08-31 江阴润玛电子材料股份有限公司 Compatible ITO etching solution and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732253A (en) * 2012-06-30 2012-10-17 江阴润玛电子材料股份有限公司 Ferric trichloride ITO etching solution and its preparation method
CN102732252A (en) * 2012-06-21 2012-10-17 江阴润玛电子材料股份有限公司 Novel aqua regia system ITO (indium tin oxide) etching solution and its preparation method
CN102925894A (en) * 2012-10-09 2013-02-13 江阴润玛电子材料股份有限公司 Acid copper etching liquid and preparation process thereof
CN103666478A (en) * 2013-12-13 2014-03-26 江阴润玛电子材料股份有限公司 Non-ionic ammonium hydrogen fluoride etching solution with low surface tension
CN105176533A (en) * 2015-09-25 2015-12-23 江阴润玛电子材料股份有限公司 ITO-Ag-ITO etching liquid for AM-OLED display screen and preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732252A (en) * 2012-06-21 2012-10-17 江阴润玛电子材料股份有限公司 Novel aqua regia system ITO (indium tin oxide) etching solution and its preparation method
CN102732253A (en) * 2012-06-30 2012-10-17 江阴润玛电子材料股份有限公司 Ferric trichloride ITO etching solution and its preparation method
CN102925894A (en) * 2012-10-09 2013-02-13 江阴润玛电子材料股份有限公司 Acid copper etching liquid and preparation process thereof
CN103666478A (en) * 2013-12-13 2014-03-26 江阴润玛电子材料股份有限公司 Non-ionic ammonium hydrogen fluoride etching solution with low surface tension
CN105176533A (en) * 2015-09-25 2015-12-23 江阴润玛电子材料股份有限公司 ITO-Ag-ITO etching liquid for AM-OLED display screen and preparation method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113322072A (en) * 2021-06-25 2021-08-31 江阴润玛电子材料股份有限公司 Compatible ITO etching solution and preparation method thereof
CN113322072B (en) * 2021-06-25 2022-06-03 江阴润玛电子材料股份有限公司 Compatible ITO etching solution and preparation method thereof

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Application publication date: 20170915