CN104480469B - A kind of TFT copper-molybdenums stacked film etchant and engraving method - Google Patents
A kind of TFT copper-molybdenums stacked film etchant and engraving method Download PDFInfo
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- CN104480469B CN104480469B CN201410759948.5A CN201410759948A CN104480469B CN 104480469 B CN104480469 B CN 104480469B CN 201410759948 A CN201410759948 A CN 201410759948A CN 104480469 B CN104480469 B CN 104480469B
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Abstract
The invention discloses a kind of TFT copper-molybdenums stacked film etchant, the component and percentage by weight of composition are respectively：5~30% hydrogen peroxide, 0.1~5% H2SO4, persulfide, chloride, stabilizer of hydrogen peroxide 0.005~0.3%, metal chelating agent 0.005~0.3%, surfactant 0.005~0.2%, 0.001 ~ 1% azole additive and excess water, the percentage by weight sum of persulfide and chloride is 0.01~0.5%.The TFT copper-molybdenum stacked film etchants are uniform to the etching of copper-molybdenum stacked film, etch-rate is moderate and service life is grown.
Description
Technical field
The present invention relates to thin film transistor (TFT) copper-molybdenum stacked film etching technique field, and in particular to a kind of TFT copper-molybdenums stacked film
Etchant.
Background technology
Thin film transistor (TFT)（TFT）Liquid crystal display be in twisted nematic liquid crystal display introduce thin film transistor switch and
The Active Matrix LCD At of formation.In thin film transistor (TFT), non-crystalline silicon is used in usual TFT layer, molybdenum, aluminium are used in wiring material
Or aluminium alloy.Research finds that molybdenum, aluminium and aluminium alloy resistance are high, and with display maximization and high resolution, due to field
The problem of signal delay occurs in effect mobility, uneven so as to cause picture to show.Improved technical scheme uses resistance
The less copper of rate is as wiring material, but the associativity of copper and glass substrate or silicon substrate is bad, it is necessary to draw between the two layers
Enter molybdenum as binder course.Therefore copper/molybdenum laminate film turns into the primary structure of thin film transistor (TFT) plain conductor development.
Copper-molybdenum stacked film etchant of the prior art mainly includes：Hydrogen peroxide, organic acid or inorganic acid are such as
Hydrofluoric acid and aqueous medium.Such as CN101418449A discloses a kind of Etchant composition and engraving method of copper/molybdenum,
Consisting of hydrogen peroxide, amino acid, pH stable agent, fluoric-containing acid, acid ph value stabilizer and aqueous medium.
But there is technological deficiency in above-mentioned hydrogen peroxide system etching solution when being used in TFT metal chips：Firstth, lose
Carve liquid can constantly decompose in use, decomposing hydrogen dioxide solution can caused by oxygen bubble be inevitably attached to copper surface or
Person is etched at the side oblique angle to be formed, and can influence further to etch, so as to cause the figure for occurring etching uneven, copper and molybdenum to cut open
Face and the poor phenomenon of glacing flatness, and the control to etching angle is undesirable；Secondth, hydrogen peroxide system etching solution is to copper metal
The etching of film can produce the copper ion being free in etching solution, and decomposition of the copper ion to hydrogen peroxide has catalytic action, can entered
One step accelerates the decomposition of hydrogen peroxide, therefore copper-molybdenum stacked film etching process is unstable, while shortens the etching solution life-span；3rd,
Difference is compared in rate selection at the time of copper/molybdenum stacked film；4th, the activity of fluorine ion is stronger, can be to operation using fluorine-containing etching solution
Environment causes certain pollution, is unfavorable for the health of operating personnel, and if failure etching solution without correctly processing, also
Serious pollution can be caused to environment.Therefore, it is necessary to TFT copper-molybdenums stacked film etchant of the prior art is carried out
Formula improves.
The content of the invention
It is an object of the invention to overcome defect present in prior art, there is provided a kind of that copper-molybdenum stacked film is etched
Even, etch-rate is moderate and the TFT copper-molybdenum stacked film etchants of service life length.
To realize above-mentioned technique effect, the technical scheme is that：A kind of TFT copper-molybdenums stacked film etchant,
Characterized in that, the component and percentage by weight of the composition are respectively：Hydrogen peroxide 5~30%, H2SO40.1~5%, over cure
Compound, chloride, stabilizer of hydrogen peroxide 0.005~0.3%, metal chelating agent 0.005~0.3%, surfactant 0.005~
0.2%th, 0.001 ~ 1 % azoles additive and excess water, the percentage by weight sum of the persulfide and chloride for 0.01~
0.5%。
Preferable technical scheme is that the component and percentage by weight of the composition are respectively：Hydrogen peroxide 10~20%,
H2SO40.3~3%, persulfide, chloride, stabilizer of hydrogen peroxide 0.01~0.1%, metal chelating agent 0.01~0.1%, table
Face activating agent 0.01~0.1%, 0.005 ~ 0.5% azole additive and excess water, the weight hundred of the persulfide and chloride
It is 0.03~0.3% to divide than sum.
Wherein, the persulfide be potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate and potassium hydrogen persulfate in one kind, institute
It is potassium chloride or ammonium chloride to state chloride.
Wherein, the stabilizer of hydrogen peroxide is phosphate, glycols compound or aminated compounds.
Wherein, the metal chelating agent is aminocarboxylate metalloid complexing agent.
Preferable technical scheme is that the metal chelating agent is selected from nitrilotriacetic acid salt, edetate, divinyl
In pentacetate, nitrilotriacetic acid, sub- nitrogen base oxalic acid, methyl amimoacetic acid, alanine, glutamic acid, aminobutyric acid and glycine at least
It is a kind of.
Wherein, the surfactant is nonionic surfactant.
Preferable technical scheme is that the surfactant is fatty glyceride, fatty acid sorbitan and polysorbate
At least one of.
Wherein, the azole is selected from 1H- BTAs, 5- methyl isophthalic acids-BTA, 3- amino -1H- triazoles, 1H- tetra-
Azoles, 5- methyl isophthalic acid H- tetrazoliums, at least one of 5- phenyl -1H-TETRAZOLE.
The present invention, which also resides in, provides a kind of copper-molybdenum stacked film etching side suitable for TFT copper-molybdenum stacked film etchants
Method, it is characterised in that engraving method is using above-mentioned TFT copper-molybdenum stacked film etchants to thin film transistor (TFT) copper-molybdenum metal
Laminate film is etched, and the etch temperature of the TFT copper-molybdenums stacked film etchant is 20~50 DEG C.
The advantages of the present invention are：
The TFT copper-molybdenum stacked film etchants are excellent in the selectivity to metallic copper and molybdenum, to glass substrate or silicon
Substrate hardly etches；
The addition of surfactant makes tension force be reduced to 35N/m from original 72N/m, it is ensured that etching solution penetrate into layers of copper and
The trickle gap of Mo layer surface and etching inclination angle, and assign etching solution certain defoaming effect；
Metal chelating agent can be complexed etching solution etching copper metal layer and caused copper ion, avoid because hydrogen peroxide accelerate point
Solve and shorten the etching solution life-span；
Fluoride is substituted using persulfide or chloride, the dirt with caused by operating environment of fluorine containing etchant liquid can be avoided
Dye, ensure the health of operating personnel；
When being etched using the engraving method in the present invention to thin film transistor (TFT) copper-molybdenum stacked film, etch-rate is moderate, etching
Process stabilization, after testing, using the etching solution to TFT metal chips carry out the moment, it is ensured that etching angle 40 °~70 ° it
Between, and bottom molybdenum noresidue.
Embodiment
With reference to embodiment, the embodiment of the present invention is further described.Following examples are only used for more
Add and clearly demonstrate technical scheme, and can not be limited the scope of the invention with this.
Embodiment 1
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 1 be respectively：Hydrogen peroxide
5%、H2SO40.1%th, potassium peroxydisulfate 0.005%, potassium chloride 0.005%, stabilizer of hydrogen peroxide 0.005%, metal chelating agent
0.005%th, surfactant 0.2%, azole additive 1% and excess water.Stabilizer of hydrogen peroxide is phosphate, metal chelating agent
For nitrilotriacetic acid, surfactant is fatty glyceride, and azole additive is 1H- BTAs.
Embodiment 2
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 2 be respectively：Hydrogen peroxide
10%、H2SO40.3%th, ammonium persulfate 0.02%, potassium chloride 0.01%, stabilizer of hydrogen peroxide 0.01%, metal chelating agent 0.01%, table
Face activating agent 0.1%, azole additive 0.5% and excess water.Stabilizer of hydrogen peroxide is phosphate, and metal chelating agent is sub- nitrogen base
Oxalic acid, surfactant are fatty acid sorbitan, and azole additive is 5- methyl isophthalic acid H- tetrazoliums.
Embodiment 3
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 3 be respectively：Hydrogen peroxide
15%、H2SO41.5%th, sodium peroxydisulfate 0.015%, potassium chloride 0.015%, stabilizer of hydrogen peroxide 0.05%, metal chelating agent 0.05%,
Surfactant 0.05%, azole additive 0.25% and excess water.Stabilizer of hydrogen peroxide is phosphate, and metal chelating agent is Asia
Nitrogen base oxalic acid, surfactant are fatty acid sorbitan, and azole additive is 5- methyl isophthalic acid H- tetrazoliums.
Embodiment 4
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 4 be respectively：Hydrogen peroxide
20%、H2SO43%th, potassium hydrogen persulfate 0.01%, potassium chloride 0.02%, stabilizer of hydrogen peroxide 0.1%, metal chelating agent 0.1%, surface
Activating agent 0.01%, azole additive 0.005% and excess water.Stabilizer of hydrogen peroxide is phosphate, and metal chelating agent is sub- nitrogen
Base oxalic acid, surfactant are fatty acid sorbitan, and azole additive is 5- methyl isophthalic acid H- tetrazoliums.
Embodiment 5
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 5 be respectively：Hydrogen peroxide
30%、H2SO45%th, potassium peroxydisulfate 0.1%, potassium chloride 0.05%, stabilizer of hydrogen peroxide 0.3%, metal chelating agent 0.3%, surface are lived
Property agent 0.005%, azole additive 0.001% and excess water.Stabilizer of hydrogen peroxide is phosphate, and metal chelating agent is paddy ammonia
Acid, surfactant are fatty glyceride, and azole additive is 1H- BTAs.
Embodiment 6
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 6 be respectively：Hydrogen peroxide
10%、H2SO40.3%th, potassium peroxydisulfate 0.075%, ammonium chloride 0.075%, metal chelating agent 0.01%, surfactant 0.1%, azole
Additive 0.5% and excess water, without stabilizer of hydrogen peroxide.Stabilizer of hydrogen peroxide is phosphate, and metal chelating agent is sub- nitrogen
Base oxalic acid, surfactant are fatty acid sorbitan, and azole additive is 5- methyl isophthalic acid H- tetrazoliums.
Embodiment 7
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 7 be respectively：Hydrogen peroxide
30%、H2SO45%th, sodium peroxydisulfate 0.05%, ammonium chloride 0.1%, stabilizer of hydrogen peroxide 0.3%, metal chelating agent 0.3%, surface are lived
Property agent 0.005% and excess water, not azole additive.Stabilizer of hydrogen peroxide is phosphate, and metal chelating agent is glutamic acid,
Surfactant is fatty glyceride.
Embodiment 8
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 8 be respectively：Hydrogen peroxide
15%、H2SO41.5%th, potassium hydrogen persulfate 0.2%, ammonium chloride 0.1%, stabilizer of hydrogen peroxide 0.05%, surfactant 0.05%, azoles
Class additive 0.25% and excess water, without metal chelating agent.Stabilizer of hydrogen peroxide is phosphate, and surfactant is fat
Acid glyceride, azole additive are 1H- BTAs.
Embodiment 9
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 9 be respectively：Hydrogen peroxide
5%、H2SO40.1%th, ammonium persulfate 0.15%, ammonium chloride 0.15%, stabilizer of hydrogen peroxide 0.005%, metal chelating agent 0.005%,
Azole additive 1% and excess water, without surfactant.Stabilizer of hydrogen peroxide is phosphate, and metal chelating agent is the second of ammonia three
Acid, azole additive are 1H- BTAs.
Embodiment 10
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 10 be respectively：Hydrogen peroxide
15%、H2SO40.1%th, potassium peroxydisulfate 0.05%, ammonium chloride 0.15%, stabilizer of hydrogen peroxide 0.05%, metal chelating agent 0.1%, table
Face activating agent 0.2%, azole additive 0.25% and excess water.Stabilizer of hydrogen peroxide is phosphate, and surfactant is fat
Acid glyceride, metal chelating agent are sub- nitrogen base oxalic acid, and azole additive is 1H- BTAs.
Embodiment 11
The component and percentage by weight of the TFT copper-molybdenum stacked film etchants of embodiment 10 be respectively：Hydrogen peroxide
15%、H2SO43%th, ammonium persulfate 0.25%, ammonium chloride 0.25%, stabilizer of hydrogen peroxide 0.05%, metal chelating agent 0.05%, surface
Activating agent 0.05%, azole additive 0.25% and excess water.Stabilizer of hydrogen peroxide is phosphate, and surfactant is aliphatic acid
Glyceride, metal chelating agent are sub- nitrogen base oxalic acid, and azole additive is 1H- BTAs.
Etching experiment
Using glass as substrate, sputter molybdenum and form a layer thickness 500A molybdenum layer, then sputter copper and form a layer thickness
Pattern is formed figuratum copper/molybdenum plural layers, utilizes etching solution by 6000A layers of copper, coating circuit after exposure imaging
Progress is etched at 35 DEG C by shower spray, the copper-molybdenum plural layers being made to.Afterwards by scanning electron microscopy
Viewing film transistor copper-molybdenum is laminated film layer angle and etching situation under 20KV, 40000 multiplying powers under mirror.
Concentration be 30% hydrogen peroxide percentage be less than 10%, thin film transistor (TFT) copper-molybdenum stacked film etch-rate substantially compared with
It is low；Can be too fast with thin film transistor (TFT) copper-molybdenum stacked film etch-rate when the percentage for the hydrogen peroxide that concentration is 30% is higher than 40%,
Etch uniformity is poor, is difficult to control.
Inverted dip phenomenon can be formed by not adding the etching of azole additive, and azole additive etches when being preferably 0.005 ~ 0.5%
Inclination angle can be more stably controlled at 40 ~ 70 °, and nitric acid content is preferably that 0.3% ~ 3% etching CD losses are less than 1um, metal chelating agent
Molybdenum does not have residue completely when preferably 0.005 ~ 0.3%.
Hydrogen peroxide and H2SO4Added in the form of hydrogen peroxide and sulfuric acid, hydrogen peroxide and H2SO4Percentage by weight
It is hydrogen peroxide and sulfuric acid weight through conversion gained.
Persulfide in TFT copper-molybdenum stacked film etchants directly can react with copper, and the addition of chloride
Help lend some impetus to the etching to molybdenum layer.Persulfide must be present in copper-molybdenum stacked film etchant simultaneously with chloride
In, proportioning needs to be determined according to the thickness of layers of copper and molybdenum layer between the two.
Specifically, metal chelating agent can be sub- nitrogen base oxalic acid, nitrilotriacetic acid, ethylenediamine tetra-acetic acid, diethylenetriamine
Pentaacetic acid, aminotrimethylene phosphoric acid, 1- hydroxy ethylene -1,1- diphosphonic acid, ethylenediamine tetraacetic methylene phosphoric acid, diethylenetriamines
Pentamethylene phosphoric acid, methyl amimoacetic acid, alanine, paddy nitronic acid, aminobutyric acid and sweet nitronic acid etc..
Surfactant selects the reasons why nonionic surfactant：Nonionic surfactant has not to be occurred in water
Ionization, low foaming feature, there is preferable dissolubility in water and in organic solvent, stability is high in the solution, be not easy by
Strong electrolyte inorganic salts and acid, the influence of alkali.
The reasons why stabilizer of hydrogen peroxide selection phosphate, glycols compound or aminated compounds：The stabilizer oxytolerant
The property changed is strong, and stable complex compound can be formed with metal ion, and general impurity energy strong bonded, and reaches with temperature resistant capability
200 DEG C, protect the decomposition of hydrogen peroxide.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of TFT copper-molybdenums stacked film etchant, it is characterised in that the component of the composition and weight percent score
It is not：Hydrogen peroxide 10~20%, H2SO40.3~3%, persulfide, chloride, stabilizer of hydrogen peroxide 0.01~0.1%,
Metal chelating agent 0.01~0.1%, surfactant 0.01~0.1%, 0.005~0.5% azole additive and excess water, institute
Persulfide is stated as one kind in potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate and potassium hydrogen persulfate, the persulfide and chlorination
The percentage by weight sum of thing is 0.03~0.3%, and the metal chelating agent is aminocarboxylate metalloid complexing agent or is selected from
At least one of nitrilotriacetic acid, methyl amimoacetic acid, alanine, glutamic acid, aminobutyric acid and glycine.
2. TFT copper-molybdenums stacked film etchant according to claim 1, it is characterised in that the chloride is chlorine
Change potassium or ammonium chloride.
3. TFT copper-molybdenums stacked film etchant according to claim 1, it is characterised in that the hydrogen peroxide is steady
It is phosphate, glycols compound or aminated compounds to determine agent.
4. TFT copper-molybdenums stacked film etchant according to claim 3, it is characterised in that the metal chelating agent
For selected from least one of nitrilotriacetic acid salt, edetate.
5. TFT copper-molybdenums stacked film etchant according to claim 1, it is characterised in that the surfactant
For nonionic surfactant.
6. TFT copper-molybdenums stacked film etchant according to claim 5, it is characterised in that the surfactant
For at least one of fatty glyceride, fatty acid sorbitan and polysorbate.
7. TFT copper-molybdenums stacked film etchant according to claim 1, it is characterised in that the azole be selected from
1H- BTAs, 3- amino -1H- triazoles, 1H-TETRAZOLE, 5- methyl isophthalic acid H- tetrazoliums, at least one of 5- phenyl -1H-TETRAZOLE.
8. a kind of engraving method of TFT copper-molybdenums stacked film etchant, it is characterised in that appoint using in claim 1 to 7
TFT copper-molybdenum stacked film etchants described in meaning one are etched to thin film transistor (TFT) copper-molybdenum metal stacking film, institute
The etch temperature for stating TFT copper-molybdenum stacked film etchants is 20~50 DEG C.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106637209A (en) * | 2016-12-29 | 2017-05-10 | 深圳市华星光电技术有限公司 | Etching solution composition and metal film etching method using same |
| CN107119278A (en) * | 2017-05-19 | 2017-09-01 | 合肥市惠科精密模具有限公司 | The ITO Ag ITO etching solutions of concave point after a kind of suppression TFT LCDs is thinned |
| CN107151795A (en) * | 2017-06-02 | 2017-09-12 | 苏州晶瑞化学股份有限公司 | A kind of copper-molybdenum alloy film etching solution |
| CN109112545A (en) * | 2018-09-25 | 2019-01-01 | 惠州市宙邦化工有限公司 | A kind of chemical etching composition of copper-molybdenum alloy film |
| CN109972144A (en) * | 2019-04-10 | 2019-07-05 | 深圳市松柏实业发展有限公司 | The regeneration method and recycling system of copper etchant solution and its waste liquid |
| CN109930153B (en) * | 2019-04-24 | 2021-01-01 | 深圳市华星光电技术有限公司 | Etching liquid and etching device |
| CN111270237B (en) * | 2020-02-26 | 2022-04-26 | 江阴润玛电子材料股份有限公司 | Copper-molybdenum etching solution for advanced plate |
| CN111472000B (en) * | 2020-04-15 | 2021-07-27 | 苏州华星光电技术有限公司 | Etching method of copper-molybdenum film layer and array substrate |
| CN112064032B (en) * | 2020-09-11 | 2022-04-01 | 武汉迪赛新材料有限公司 | Supplementary liquid capable of prolonging service life of hydrogen peroxide etching liquid |
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