CN106367755A - Etchant composition and manufacturing method of an array substrate for liquid crystal display - Google Patents

Etchant composition and manufacturing method of an array substrate for liquid crystal display Download PDF

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Publication number
CN106367755A
CN106367755A CN201610121704.3A CN201610121704A CN106367755A CN 106367755 A CN106367755 A CN 106367755A CN 201610121704 A CN201610121704 A CN 201610121704A CN 106367755 A CN106367755 A CN 106367755A
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Prior art keywords
acid
weight
group
copper
surplus
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CN201610121704.3A
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CN106367755B (en
Inventor
鞠仁说
南基龙
崔汉永
刘仁浩
金宝衡
李钟文
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Dongwoo Fine Chem Co Ltd
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Dongwoo Fine Chem Co Ltd
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Priority claimed from KR1020150105157A external-priority patent/KR102400312B1/en
Priority claimed from KR1020150105041A external-priority patent/KR102423605B1/en
Priority claimed from KR1020150105204A external-priority patent/KR102423604B1/en
Application filed by Dongwoo Fine Chem Co Ltd filed Critical Dongwoo Fine Chem Co Ltd
Publication of CN106367755A publication Critical patent/CN106367755A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23F—NON-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
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/18—Acidic compositions for etching copper or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23F—NON-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
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/02—Local etching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23F—NON-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
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/26—Acidic compositions for etching refractory metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H01L21/321—After treatment
    • H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
    • H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
    • H01L21/32134—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by liquid etching only
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/77—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • ing And Chemical Polishing (AREA)
  • Weting (AREA)

Abstract

The invention relates to a etchant composition, method for using the etchant composition to manufacture an array substrate of a liquid crystal display device and an array substrate. When the etchant composition is used to etch a copper-based metal layer, a quality etching profile and abudant processing plates are obtained.

Description

Etching agent composite, the method manufacturing the array base palte of liquid crystal indicator using it And array base palte
Technical field
The present invention relates to etching agent composite, manufacture method and the array base of the array base palte of liquid crystal indicator using it Plate.
Background technology
Thin film transistor (TFT) (tft) is the typical electronic circuit driving semiconductor device and flat faced display.The manufacture of tft Process is typically included in the metal level being formed on substrate as gate line data wire material, and the selected area in described metal level Form photoresist, then by the use of described photoresist as metal level described in mask etching on domain.
Gate line data line uses has good electrical conductivity and low-resistance copper, and in a case of copper, coating Photoresist and to be formed pattern be probably difficult for technique, therefore, copper base metal layer replaces individually recently Layers of copper is used as gate line data line.Among described copper base metal layer, titanium/copper is usually used double-deck.However, ought etch simultaneously When titanium/copper is double-deck, processing after having the shortcomings that to etch section difference and be difficult to, and there is copper eluting with etching progress, this Lead to the quantity processing plate few.In view of above-mentioned, actively studying the etching agent composite for copper base metal layer, and make For an example, Korean patent application publication no.2015-0059800 provides a kind of fluid composition, its comprise maleic acid from Component, copper ion source and fluoride sources, and there is 0 to 7 ph value.However, the shortcoming of described fluid composition is have not Good etching section, and process the quantity minimizing of plate.
Accordingly, it has been required to there is outstanding etching section and processing when etch copper base metal layer such as titanium/copper is double-deck Etching agent composite more than plate quantity.
[prior art literature]
[patent documentation]
Korean patent application publication no.2015-0059800
Content of the invention
It is an object of the invention to provide for the etching agent composite of copper base metal layer, it has outstanding etching section simultaneously And it is many to process the quantity of plate.
In view of above-mentioned, one aspect of the present invention provides the etching agent composite for copper base metal, and it is with respect to institute State the gross weight of compositionss, comprise,
The copper compound of 0.5 weight % to 10 weight %；
The fluorine compounds of 0.01 weight % to 2 weight %；
One or more type mineral acid of 1 weight % to 10 weight %, it is selected from nitric acid, sulphuric acid, phosphoric acid and high chlorine The group that acid is formed；
One or more type chlorine compound of 0.1 weight % to 10 weight %, it is selected from hydrochloric acid, sodium chloride, chlorination The group that potassium, ammonium chloride, mesyl chloride, ethyl sulfonic chloride, chlorobenzene sulfonyl chloride, benzene sulfonyl chloride and chloro-ethane-sulfonyl chloride are formed；
One or more type organic acid of 1 weight % to 10 weight %, it is selected from acetic acid, butanoic acid, citric acid, first Acid, gluconic acid, glycolic, oxalic acid, valeric acid, sulfosalicylic acid, 2-Sulfosuccinic acid, sulfosalicylic phthalate, salicylic acid, sulfo group water Poplar acid, benzoic acid, lactic acid, glyceric acid, malic acid, tartaric acid, 1-Hydroxy-1,2,3-propanetricarboxylic acid., propanoic acid (profenoic acid), imino-diacetic The group that acetic acid and ethylenediaminetetraacetic acid are formed, or its salt；
One or more type non-metallic inorganic salt of 0.1 weight % to 10 weight %, it is selected from ammonium sulfate, sulphuric acid Sodium, potassium sulfate, calcium sulfate, ammonium hydrogen sulfate, sodium bisulfate, potassium acid sulfate, calcium bisulfate, ammonium nitrate, sodium nitrate, potassium nitrate and nitre The group that sour calcium is formed；
The cyclic amine compound of 0.01 weight % to 5 weight %；
The chelating agen of 0.5 weight % to 10 weight %；With
The water of surplus,
Wherein, described chelating agen is
1) cisoid dicarboxylic acids or its salt,
2) it is selected from maleic acid, citraconic acid, phthalic acid, 1,2,4,5- benzene tertacarbonic acid, mellic acid., 4- sulfo group neighbour's benzene Dioctyl phthalate, quinolinic acid, cis- 5- norborene-outer -2,3- dicarboxylic acids, 1,2,3,4- Tetramethylene. tetrabasic carboxylic acid and suitable, suitable, suitable, cis- One or more of the group that 1,2,3,4- Pentamethylene. tetrabasic carboxylic acid is formed type, or its salt, or
3) it is selected from one or more of the group that malonic acid, succinic acid and 1,3-propanedicarboxylic acid are formed type, or its salt.
In one embodiment, described chelating agen can be selected from one or more of following formed group class Type: maleic anhydride, citraconic anhydride, 2,3- dimethyl maleic anhydrides, 3,4,5,6- tetrabydrophthalic anhydrides, phenyl maleic acid Acid anhydride, 2,3- dihydros-Isosorbide-5-Nitrae-two sulfur [2,3-c] furan -5,7- diketone (2,3-dihydro-1,4-dithino [2,3-c] furan- 5,7-dione), phthalic anhydride, 4- methyl nadic anhydride, PMDA, 3- oxabicyclo [3,1,0]-hex- 2,4- diketone, cis- 1,2,3,4- Pentamethylene. tetracarboxylic dianhydrides, Tetramethylene. -1,2,3,4- tetracarboxylic dianhydrides, cis- 5- norborene - Outward -2,3- dicarboxylic anhydride, cis- 1,2,3,6- tetrabydrophthalic anhydrides, maleic acid, citraconic acid, phthalic acid, 1,2,4,5- Benzene tertacarbonic acid, mellic acid. and 4- sulfosalicylic phthalate；Or its salt.
In another embodiment, described copper base metal layer can be titanium or the bilayer of titanium alloy and copper or copper alloy.
The method that another aspect of the present invention provides the array base palte manufacturing liquid crystal indicator, methods described bag Include,
A) gate line is formed on substrate；
B) form gate insulator on the described substrate including gate line；
C) semiconductor layer is formed on described gate insulator；
D) source electrode and drain electrode are formed on described semiconductor layer；With
E) form the pixel electrode being connected with described drain electrode,
Wherein a) or d) step includes forming copper base metal layer on described substrate or semiconductor layer, and uses described etchant Compositionss etch described copper base metal layer to form gate line or source electrode and drain electrode, and
Described etching agent composite, with respect to the gross weight of described compositionss, comprises, and 0.5 weight % is to 10 weight % Copper compound；The fluorine compounds of 0.01 weight % to 2 weight %；One or more type of 1 weight % to 10 weight % is inorganic Acid, it is selected from the group that nitric acid, sulphuric acid, phosphoric acid and perchloric acid are formed；One or more class of 0.1 weight % to 10 weight % Type chlorine compound, it is selected from hydrochloric acid, sodium chloride, potassium chloride, ammonium chloride, mesyl chloride, ethyl sulfonic chloride, chlorobenzene sulfonyl chloride, benzene The group that sulfonic acid chloride and chloro-ethane-sulfonyl chloride are formed；One or more type organic acid of 1 weight % to 10 weight %, it is selected from Acetic acid, butanoic acid, citric acid, formic acid, gluconic acid, glycolic, oxalic acid, valeric acid, sulfosalicylic acid, 2-Sulfosuccinic acid, sulfo group neighbour's benzene Dioctyl phthalate, salicylic acid, sulfosalicylic acid, benzoic acid, lactic acid, glyceric acid, malic acid, tartaric acid, 1-Hydroxy-1,2,3-propanetricarboxylic acid., propanoic acid, imido The group that base oxalic acid and ethylenediaminetetraacetic acid are formed, or its salt；One or more type of 0.1 weight % to 10 weight % is non- Metal inorganic salt, it is selected from ammonium sulfate, sodium sulfate, potassium sulfate, calcium sulfate, ammonium hydrogen sulfate, sodium bisulfate, potassium acid sulfate, sulfur The group that sour hydrogen calcium, ammonium nitrate, sodium nitrate, potassium nitrate and calcium nitrate are formed；The cyclammonium chemical combination of 0.01 weight % to 5 weight % Thing；The chelating agen of 0.5 weight % to 10 weight %；Water with surplus.
The array base palte of described liquid crystal indicator can be thin film transistor (TFT) (tft) array base in one embodiment Plate.
In another embodiment, described chelating agen can be selected from one or more of following formed group class Type: maleic anhydride, citraconic anhydride, 2,3- dimethyl maleic anhydrides, 3,4,5,6- tetrabydrophthalic anhydrides, phenyl maleic acid Acid anhydride, 2,3- dihydros-Isosorbide-5-Nitrae-two sulfur [2,3-c] furan -5,7- diketone, phthalic anhydride, 4- methyl nadic anhydride, benzene four Formic acid dianhydride, 3- oxabicyclo [3,1,0]-hex- 2,4- diketone, cis- 1,2,3,4- Pentamethylene. tetracarboxylic dianhydrides, Tetramethylene. -1, 2,3,4- tetracarboxylic dianhydrides, cis- 5- norborene-outer -2,3- dicarboxylic anhydride, cis- 1,2,3,6- tetrabydrophthalic anhydrides, horse Come sour, citraconic acid, phthalic acid, 1,2,4,5- benzene tertacarbonic acid, mellic acid. and 4- sulfosalicylic phthalate；Or its salt.
In another embodiment, described copper base metal layer can be titanium or the bilayer of titanium alloy and copper or copper alloy.
An additional aspect of the present invention provides the array base palte of the liquid crystal indicator manufacturing using said method.
Brief description
According to the description of the embodiment being given below in conjunction with the accompanying drawings, the purpose of the present invention and property will become aobvious and easy See, in described accompanying drawing:
Fig. 1 shows the section when the etching agent composite using embodiment 1 and comparative example 12 etches titanium/copper bilayer；
Fig. 2 shows the section when the etching agent composite using embodiment 17 and comparative example 27 etches titanium/copper bilayer； With
Fig. 3 shows the section when the etching agent composite using embodiment 32 and comparative example 42 etches titanium/copper bilayer.
Specific embodiment
The present invention relates to etching agent composite, and the method manufacturing the array base palte of liquid crystal indicator.
The etching agent composite of the present invention, when the specific chelating agen etch copper base metal layer by comprising certain content, has Have outstanding etching section and process plate quantity many.
Hereinafter, will be described in detail the present invention.
Etch combination
In the present invention, copper compound plays the effect of oxidant and keeps when etchant etching metal level cd to offset not Become, and account for 0.5 weight % to 10 weight % preferably with respect to the gross weight of described etchant.When described content is less than 0.5 weight Measure during % the etching it is impossible to realizing copper or comprising the metal level of copper, or etch-rate is very low and initial etch is uneven.When The effect of the quantity of processing plate when described content is more than 10 weight %, cannot be increased.Described copper compound preferably uses and is selected from One or more of the group being made up of copper sulfate, copper chloride and copper nitrate type.
Fluorine compounds are the key components of etching titanium or the metal level comprising titanium, concurrently fling to and remove may go out during etching The effect of existing residue.Described fluorine compounds account for 0.01 weight % to 2 weights preferably with respect to the gross weight of described etchant Amount %.When the content of described fluorine compounds is less than 0.01 weight %, the etch-rate of titanium or the metal level comprising titanium is reduced, Cause residue, and when described content is more than 2.0 weight %, can occur for example to be formed on metal wire to substrate The infringement of glass and to comprising the infringement of the insulating barrier of silicon that formed with it.Described fluorine compounds can using wherein fluorion or The compound that polyatom fluorion dissociates in the solution, and preferably use selected from ammonium fluoride, sodium fluoride, potassium fluoride, fluohydric acid gas One or more type of ammonium, sodium bifluoride and potassium hydrogen fluoride.
One or more of group being formed selected from nitric acid, sulphuric acid, phosphoric acid and perchloric acid type mineral acid be for Etch copper or the metal level comprising copper and titanium or comprise titanium metal level cooxidant, and preferably with respect to described etchant Gross weight account for 1 weight % to 10 weight %.When the content of described mineral acid is less than 1 weight %, to copper or the gold that comprises copper The etch-rate belonging to layer and titanium or comprising the metal level of titanium reduces, and this can cause etching section defect and residue, and works as institute When stating content more than 10 weight %, overetch and photoresist is occurred to split, this can be drawn due to liquid chemical infiltration Initial line short circuit.
Selected from hydrochloric acid, sodium chloride, potassium chloride, ammonium chloride, mesyl chloride, ethyl sulfonic chloride, chlorobenzene sulfonyl chloride, benzene sulfonyl chloride One or more of group being formed with chloro-ethane-sulfonyl chloride type chlorine compound plays the effect of the cooxidant of metal level, And control etch-rate and metal level angle, and have the advantages that to prevent line exposed (wire opening).Described chlorine compound Gross weight preferably with respect to described compositionss accounts for 0.1 weight % to 10 weight %.When the content of described chlorine compound is less than 0.1 During weight %, the etch-rate of copper is reduced, the etching period during causing increases, and this can cause the problem of productivity ratio.Separately Outward, when described content is more than 10 weight %, because the etch-rate to copper can not be controlled, overetch can occur.
One or more type organic acid, it is selected from acetic acid, butanoic acid, citric acid, formic acid, gluconic acid, glycolic, grass Acid, valeric acid, sulfosalicylic acid, 2-Sulfosuccinic acid, sulfosalicylic phthalate, salicylic acid, sulfosalicylic acid, benzoic acid, lactic acid, sweet Group or its salt that Oleic acid, malic acid, tartaric acid, 1-Hydroxy-1,2,3-propanetricarboxylic acid., propanoic acid, iminodiacetic acid and ethylenediaminetetraacetic acid are formed, Effect and the chelating agen controlling etch-rate is played by the dissolubility improving the copper ion occurring during precipitating, and reduces ph.Described organic acid or its salt account for 1 weight % to 10% weight preferably with respect to the gross weight of described etchant.When described organic The effect of processing plate quantity when the content of sour or described acylate is less than 1 weight %, cannot be increased, and it is big to work as described content When 10 weight %, there is overetch, may result in line short circuit.
Selected from ammonium sulfate, sodium sulfate, potassium sulfate, calcium sulfate, ammonium hydrogen sulfate, sodium bisulfate, potassium acid sulfate, hydrogen sulfate One or more of group that calcium, ammonium nitrate, sodium nitrate, potassium nitrate and calcium nitrate are formed type non-metallic inorganic salt, plays The effect of the assisted etch controlling agent of metal level, and there is the effect improving bad etching section, bad etching section is The shortcoming comprising the etchant of chlorine compound.Described non-metallic inorganic salt accounts for 0.1 preferably with respect to the gross weight of described compositionss Weight % is to 10 weight %.When described content is less than 0.1 weight % it is impossible to realize effect and the improvement of assisted etch controlling agent The effect of etching section, and when described content is more than 10 weight %, overetch can occur.
Cyclic amine compound is the etching control agent of the angle of metal level controlling etching in batches and copper or comprising copper.Described Cyclic amine compound accounts for 0.01 weight % to 5 weight % preferably with respect to the gross weight of described compositionss.When described content is less than During 0.01 weight %, cannot to the uniform etching of metal level, and when described content be more than 5 weight % when, it is possible to decrease etching speed Rate.Described cyclic amine compound preferably use selected from 5- Aminotetrazole, triazole, phenyltetrazole, imidazoles, indole, purine, pyrazoles, One or more of the group that pyridine, pyrimidine, pyrroles, pyrrolidine, pyrrolin and 5- methyl tetrazolium are formed type.
Water refers to deionized water, and using the water for semiconductor machining, preferably uses the water of 18m ω/cm or higher.Relatively In total content of described etchant, water accounts for surplus, so that the gross weight of described etchant becomes 100 weight %.
The chelating agen of the present invention plays the effect of the key component for increasing processing plate quantity.
Specifically, described chelating agen can be
1) cisoid dicarboxylic acids or its salt,
2) it is selected from maleic acid, citraconic acid, phthalic acid, 1,2,4,5- benzene tertacarbonic acid, mellic acid., 4- sulfo group neighbour's benzene Dioctyl phthalate, quinolinic acid, cis- 5- norborene-outer -2,3- dicarboxylic acids, 1,2,3,4- Tetramethylene. tetrabasic carboxylic acid and suitable, suitable, suitable, cis- One or more of the group that 1,2,3,4- Pentamethylene. tetrabasic carboxylic acid is formed type, or its salt, or
3) it is selected from one or more of the group that malonic acid, succinic acid and 1,3-propanedicarboxylic acid are formed type, or its salt.
Described cisoid dicarboxylic acids or its salt can be selected from one or more of following formed group type: maleic acid Acid anhydride, citraconic anhydride, 2,3- dimethyl maleic anhydrides, 3,4,5,6- tetrabydrophthalic anhydrides, phenylmaleic anhydride, 2,3- bis- Hydrogen-Isosorbide-5-Nitrae-two sulfur [2,3-c] furan -5,7- diketone, phthalic anhydride, 4- methyl nadic anhydride, PMDA, 3- oxabicyclo [3,1,0]-hex- 2,4- diketone, cis- 1,2,3,4- Pentamethylene. tetracarboxylic dianhydrides, Tetramethylene. -1,2,3,4- tetracarboxylic acids Acid dianhydride, cis- 5- norborene-outer -2,3- dicarboxylic anhydride, cis- 1,2,3,6- tetrabydrophthalic anhydrides, maleic acid, lemon health Acid, phthalic acid, 1,2,4,5- benzene tertacarbonic acid, mellic acid. and 4- sulfosalicylic phthalate；Or its salt.
Described chelating agen accounts for 0.5 weight % to 10 weight % preferably with respect to the gross weight of described compositionss.Contain when described The effect of processing plate quantity when amount is less than 0.5 weight %, cannot be increased, and when described content is more than 10 weight %, to gold The etch-rate belonging to layer increases, and can cause overetch.
In the present invention, described etching agent composite can also comprise metal ion chelation agent, corrosion inhibitor etc..
The method manufacturing the array base palte of liquid crystal indicator
The method manufacturing the array base palte of liquid crystal indicator, methods described includes,
A) gate line is formed on substrate；
B) form gate insulator on the described substrate including gate line；
C) semiconductor layer is formed on described gate insulator；
D) source electrode and drain electrode are formed on described semiconductor layer；With
E) form the pixel electrode being connected with described drain electrode,
Wherein a) or d) step includes forming copper base metal layer on described substrate or semiconductor layer, and the institute with the present invention State etching agent composite and etch described copper base metal layer to form gate line or source electrode and drain electrode.
The array base palte of liquid crystal indicator can be thin film transistor (TFT) (tft) array base palte, but not limited to this, and Can be used for manufacturing other electronic devices of the metal wire comprising to be formed with copper base metal layer, for example, be used for manufacturing memorizer and partly lead Body display floater.
Hereinafter, reference implementation example, comparative example and test example are more fully described the present invention.However, following enforcement , only for illustrative purpose, the scope of the present invention is not limited to the following example, comparative example and test for example, comparative example and test example Example, and can changeful ground modifications and changes.
Embodiment 1 to 48 and the preparation of comparative example 1 to 46. etching agent composite
Etching agent composite is prepared with the composition and content (unit: weight %) listed in table 1 below, table 2 and table 3.
[table 1]
Classification (a) (b) (c) (d) (e) (f) (g) (h) (i) (j) (k) Water
Embodiment 1 3 0.5 5 6 2 3 1 2 - - - Surplus
Embodiment 2 0.5 0.5 5 6 2 3 1 2 - - - Surplus
Embodiment 3 10 0.5 5 6 2 3 1 2 - - - Surplus
Embodiment 4 3 0.5 1 6 2 3 1 2 - - - Surplus
Embodiment 5 3 0.5 10 6 2 3 1 2 - - - Surplus
Embodiment 6 3 0.5 5 1 2 3 1 2 - - - Surplus
Embodiment 7 3 0.5 5 10 2 3 1 2 - - - Surplus
Embodiment 8 3 0.5 5 6 0.3 3 1 2 - - - Surplus
Embodiment 9 3 0.5 5 6 10 3 1 2 - - - Surplus
Embodiment 10 3 0.5 5 6 2 1 1 2 - - - Surplus
Embodiment 11 3 0.5 5 6 2 10 1 2 - - - Surplus
Embodiment 12 3 0.5 5 6 2 3 0.05 2 - - - Surplus
Embodiment 13 3 0.5 5 6 2 3 5 2 - - - Surplus
Embodiment 14 3 0.5 5 6 2 3 1 1 - - - Surplus
Embodiment 15 3 0.5 5 6 2 3 1 10 - - - Surplus
Embodiment 16 3 0.5 5 6 2 3 1 - 2 - - Surplus
Comparative example 1 3 0.5 5 6 2 3 1 - - - - Surplus
Comparative example 2 3 0.5 5 6 2 3 1 - - - 2 Surplus
Comparative example 3 3 0.5 5 6 2 3 1 - - 2 - Surplus
Comparative example 4 - 0.5 5 6 2 3 1 2 - - - Surplus
Comparative example 5 13 0.5 5 6 2 3 1 2 - - - Surplus
Comparative example 6 3 0.5 0.5 6 2 3 1 2 - - - Surplus
Comparative example 7 3 0.5 13 6 2 3 1 2 - - - Surplus
Comparative example 8 3 0.5 5 - 2 3 1 2 - - - Surplus
Comparative example 9 3 0.5 5 13 2 3 1 2 - - - Surplus
Comparative example 10 3 0.5 5 6 0 3 1 2 - - - Surplus
Comparative example 11 3 0.5 5 6 13 3 1 2 - - - Surplus
Comparative example 12 3 0.5 5 6 2 0 1 2 - - - Surplus
Comparative example 13 3 0.5 5 6 2 13 1 2 - - - Surplus
Comparative example 14 3 0.5 5 6 2 3 0 2 - - - Surplus
Comparative example 15 3 0.5 5 6 2 3 7 2 - - - Surplus
Comparative example 16 3 0.5 5 6 2 3 1 13 - - - Surplus
[table 2]
Classification (a) (b) (c) (d) (e) (f) (g) (l) (m) Water
Embodiment 17 3 0.5 5 6 2 3 1 2 - Surplus
Embodiment 18 0.5 0.5 5 6 2 3 1 2 - Surplus
Embodiment 19 10 0.5 5 6 2 3 1 2 - Surplus
Embodiment 20 3 0.5 1 6 2 3 1 2 - Surplus
Embodiment 21 3 0.5 10 6 2 3 1 2 - Surplus
Embodiment 22 3 0.5 5 1 2 3 1 2 - Surplus
Embodiment 23 3 0.5 5 10 2 3 1 2 - Surplus
Embodiment 24 3 0.5 5 6 0.3 3 1 2 - Surplus
Embodiment 25 3 0.5 5 6 10 3 1 2 - Surplus
Embodiment 26 3 0.5 5 6 2 1 1 2 - Surplus
Embodiment 27 3 0.5 5 6 2 10 1 2 - Surplus
Embodiment 28 3 0.5 5 6 2 3 0.05 2 - Surplus
Embodiment 29 3 0.5 5 6 2 3 5 2 - Surplus
Embodiment 30 3 0.5 5 6 2 3 1 1 - Surplus
Embodiment 31 3 0.5 5 6 2 3 1 10 - Surplus
Comparative example 17 3 0.5 5 6 2 3 1 - - Surplus
Comparative example 18 3 0.5 5 6 2 3 1 - 2 Surplus
Comparative example 19 - 0.5 5 6 2 3 1 2 - Surplus
Comparative example 20 13 0.5 5 6 2 3 1 2 - Surplus
Comparative example 21 3 0.5 0.5 6 2 3 1 2 - Surplus
Comparative example 22 3 0.5 13 6 2 3 1 2 - Surplus
Comparative example 23 3 0.5 5 - 2 3 1 2 - Surplus
Comparative example 24 3 0.5 5 13 2 3 1 2 - Surplus
Comparative example 25 3 0.5 5 6 0 3 1 2 - Surplus
Comparative example 26 3 0.5 5 6 13 3 1 2 - Surplus
Comparative example 27 3 0.5 5 6 2 0 1 2 - Surplus
Comparative example 28 3 0.5 5 6 2 13 1 2 - Surplus
Comparative example 29 3 0.5 5 6 2 3 0 2 - Surplus
Comparative example 30 3 0.5 5 6 2 3 7 2 - Surplus
Comparative example 31 3 0.5 5 6 2 3 1 13 - Surplus
[table 3]
Classification (a) (b) (c) (d) (e) (f) (g) (n) (o) (p) (q) Water
Embodiment 32 3 0.5 5 6 2 3 1 2 - - - Surplus
Embodiment 33 0.5 0.5 5 6 2 3 1 2 - - - Surplus
Embodiment 34 10 0.5 5 6 2 3 1 2 - - - Surplus
Embodiment 35 3 0.5 1 6 2 3 1 2 - - - Surplus
Embodiment 36 3 0.5 10 6 2 3 1 2 - - - Surplus
Embodiment 37 3 0.5 5 1 2 3 1 2 - - - Surplus
Embodiment 38 3 0.5 5 10 2 3 1 2 - - - Surplus
Embodiment 39 3 0.5 5 6 0.3 3 1 2 - - - Surplus
Embodiment 40 3 0.5 5 6 10 3 1 2 - - - Surplus
Embodiment 41 3 0.5 5 6 2 1 1 2 - - - Surplus
Embodiment 42 3 0.5 5 6 2 10 1 2 - - - Surplus
Embodiment 43 3 0.5 5 6 2 3 0.05 2 - - - Surplus
Embodiment 44 3 0.5 5 6 2 3 5 2 - - - Surplus
Embodiment 45 3 0.5 5 6 2 3 1 1 - - - Surplus
Embodiment 46 3 0.5 5 6 2 3 1 10 - - - Surplus
Embodiment 47 3 0.5 5 6 2 3 1 - 2 - - Surplus
Embodiment 48 3 0.5 5 6 2 3 1 - - 2 - Surplus
Comparative example 32 3 0.5 5 6 2 3 1 - - - - Surplus
Comparative example 33 3 0.5 5 6 2 3 1 - - - 4 Surplus
Comparative example 34 - 0.5 5 6 2 3 1 2 - - - Surplus
Comparative example 35 13 0.5 5 6 2 3 1 2 - - - Surplus
Comparative example 36 3 0.5 0.5 6 2 3 1 2 - - - Surplus
Comparative example 37 3 0.5 13 6 2 3 1 2 - - - Surplus
Comparative example 38 3 0.5 5 - 2 3 1 2 - - - Surplus
Comparative example 39 3 0.5 5 13 2 3 1 2 - - - Surplus
Comparative example 40 3 0.5 5 6 0 3 1 2 - - - Surplus
Comparative example 41 3 0.5 5 6 13 3 1 2 - - - Surplus
Comparative example 42 3 0.5 5 6 2 0 1 2 - - - Surplus
Comparative example 43 3 0.5 5 6 2 13 1 2 - - - Surplus
Comparative example 44 3 0.5 5 6 2 3 0 2 - - - Surplus
Comparative example 45 3 0.5 5 6 2 3 7 2 - - - Surplus
Comparative example 46 3 0.5 5 6 2 3 1 13 - - - Surplus
(a): cu (ii) so4
(b): ammonium fluoride
(c): nitric acid
(d): citric acid
(e): ammonium chloride
(f): ammonium sulfate
(g): 5- methyl tetrazolium
(h): cis- Tetramethylene. -1,2- dicarboxylic acids
(i): cis- 1,2,3,4- Pentamethylene. tetracarboxylic dianhydride
(j): trans-cyclobutane -1,2- dicarboxylic acids
(k): trans -4- cyclohexene -1,2- dicarboxylic acids
(l): phthalic acid；Benzene -1,2- dicarboxylic acids
(m): p-phthalic acid；Benzene -1,4- dicarboxylic acids
(n): malonic acid
(o): succinic acid
(p): 1,3-propanedicarboxylic acid
(q): adipic acid
Test example. etching property evaluation
Each etching agent composite using embodiment 1 to 48 and comparative example 1 to 46 is etched.Using spraying etch pattern examination During testing equipment (model: etcher (tft), semes co., ltd.), etching process, the temperature of described etching agent composite sets Put at 30 DEG C about.Etching period is different, however, etch in lcd etching process generally carrying out 30 depending on etch temperature Second was to 80 seconds.In etching process, observed described etched using sem (product of hitachi, ltd., model s-4700) The cross section of double-deck section of the described titanium/copper of journey etching, result table below 4, table 5, table 6, shows in Fig. 1, Fig. 2 and Fig. 3.
[table 4]
[table 5]
[table 6]
Do not etch: do not etch the cu of non-pattern unit and do not form pattern
Etching section defect: refer to the defect in the straight degree defect and tapered plane of the cu line of pattern unit in sem measures
As shown in table 4 is to table 6, embodiment 1 to 48, compared with comparative example 1 to 46, is being processed plate quantity and is being etched in section Show excellent property.
Specifically, as shown in figure 1, embodiment 1, compared with the comparative example 12 not adding inorganic salt (ammonium sulfate), shows Outstanding etching section.
In addition, as shown in Fig. 2 embodiment 17, compared with the comparative example 27 not adding inorganic salt (ammonium sulfate), shows Outstanding etching section.
Additionally, as shown in Figure 3, embodiment 32, compared with the comparative example 42 not adding inorganic salt (ammonium sulfate), shows Go out outstanding etching section.
When the etching agent composite etch copper base metal layer using the present invention, can get outstanding etching section and quantity Many processing plates.

Claims (7)

1. it is used for the etching agent composite of copper base metal layer, it, with respect to the gross weight of described compositionss, comprises,
The copper compound of 0.5 weight % to 10 weight %；
The fluorine compounds of 0.01 weight % to 2 weight %；
One or more type mineral acid of 1 weight % to 10 weight %, it is selected from nitric acid, sulphuric acid, phosphoric acid and perchloric acid institute The group of composition；
One or more type chlorine compound of 0.1 weight % to 10 weight %, it is selected from hydrochloric acid, sodium chloride, potassium chloride, chlorine Change the group that ammonium, mesyl chloride, ethyl sulfonic chloride, chlorobenzene sulfonyl chloride, benzene sulfonyl chloride and chloro-ethane-sulfonyl chloride are formed；
One or more type organic acid of 1 weight % to 10 weight %, it is selected from acetic acid, butanoic acid, citric acid, formic acid, Portugal Saccharic acid, glycolic, oxalic acid, valeric acid, sulfosalicylic acid, 2-Sulfosuccinic acid, sulfosalicylic phthalate, salicylic acid, sulfosalicylic acid, Benzoic acid, lactic acid, glyceric acid, malic acid, tartaric acid, 1-Hydroxy-1,2,3-propanetricarboxylic acid., propanoic acid, iminodiacetic acid and ethylenediaminetetraacetic acid institute group The group becoming, or its salt；
One or more type non-metallic inorganic salt of 0.1 weight % to 10 weight %, it is selected from ammonium sulfate, sodium sulfate, sulfur Sour potassium, calcium sulfate, ammonium hydrogen sulfate, sodium bisulfate, potassium acid sulfate, calcium bisulfate, ammonium nitrate, sodium nitrate, potassium nitrate and calcium nitrate The group being formed；
The cyclic amine compound of 0.01 weight % to 5 weight %；
The chelating agen of 0.5 weight % to 10 weight %；With
The water of surplus,
Wherein, described chelating agen is
1) cisoid dicarboxylic acids or its salt,
2) it is selected from maleic acid, citraconic acid, phthalic acid, 1,2,4,5- benzene tertacarbonic acid, mellic acid., 4- sulfo group O-phthalic Acid, quinolinic acid, cis- 5- norborene-outer -2,3- dicarboxylic acids, 1,2,3,4- Tetramethylene. tetrabasic carboxylic acid and suitable, suitable, suitable, cis- 1,2, The group that one or more type of 3,4- Pentamethylene. tetrabasic carboxylic acids is formed, or its salt, or
3) it is selected from one or more of the group that malonic acid, succinic acid and 1,3-propanedicarboxylic acid are formed type, or its salt.
2. the etching agent composite for copper base metal layer according to claim 1, wherein said chelating agen is
1) it is selected from one or more of following formed group type: by maleic anhydride, citraconic anhydride, 2,3- dimethyl Malaysias Anhydride, 3,4,5,6- tetrabydrophthalic anhydrides, phenylmaleic anhydride, 2,3- dihydros-Isosorbide-5-Nitrae-two sulfur [2,3-c] furan -5,7- Diketone, phthalic anhydride, 4- methyl nadic anhydride, PMDA, 3- oxabicyclo [3,1,0]-hex- 2,4- bis- Ketone, cis- 1,2,3,4- Pentamethylene. tetracarboxylic dianhydrides, Tetramethylene. -1,2,3,4- tetracarboxylic dianhydrides, cis- 5- norborene-outer -2, 3- dicarboxylic anhydride, cis- 1,2,3,6- tetrabydrophthalic anhydrides, maleic acid, citraconic acid, phthalic acid, 1,2,4,5- benzene four The group that carboxylic acid, mellic acid. and 4- sulfosalicylic phthalate are formed；Or its salt,
2) it is selected from maleic acid, citraconic acid, phthalic acid, 1,2,4,5- benzene tertacarbonic acid, mellic acid., 4- sulfo group O-phthalic Acid, quinolinic acid, cis- 5- norborene-outer -2,3- dicarboxylic acids, 1,2,3,4- Tetramethylene. tetrabasic carboxylic acid and suitable, suitable, suitable, cis- 1,2, One or more of the group that 3,4- Pentamethylene. tetrabasic carboxylic acids are formed type, or its salt, or
3) it is selected from one or more of the group that malonic acid, succinic acid and 1,3-propanedicarboxylic acid are formed type, or its salt.
3. the etching agent composite for copper base metal layer according to claim 1, wherein said copper base metal layer is titanium Or the bilayer of titanium alloy and copper or copper alloy.
4. the method manufacturing the array base palte of liquid crystal indicator, methods described includes,
A) gate line is formed on substrate；
B) form gate insulator on the described substrate including gate line；
C) semiconductor layer is formed on described gate insulator；
D) source electrode and drain electrode are formed on described semiconductor layer；With
E) form the pixel electrode being connected with described drain electrode,
Wherein a) or d) step includes forming copper base metal layer on described substrate or semiconductor layer, and with described in claim 1 Etching agent composite etch described copper base metal layer to form gate line or source electrode and drain electrode.
5. the method for the array base palte manufacturing liquid crystal indicator according to claim 4, wherein said liquid crystal display dress The array base palte put is thin-film transistor array base-plate.
6. the method for the array base palte manufacturing liquid crystal indicator according to claim 4, wherein said copper base metal layer It is titanium or the bilayer of titanium alloy and copper or copper alloy.
7. the array base palte of liquid crystal indicator, it utilizes the manufacture method manufacture described in claim 4.
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