CN113388836B - Method for thinning FeNi alloy foil strip by chemical etching - Google Patents
Method for thinning FeNi alloy foil strip by chemical etching Download PDFInfo
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- CN113388836B CN113388836B CN202110847470.1A CN202110847470A CN113388836B CN 113388836 B CN113388836 B CN 113388836B CN 202110847470 A CN202110847470 A CN 202110847470A CN 113388836 B CN113388836 B CN 113388836B
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- feni alloy
- alloy foil
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- feni
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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
- C23F1/28—Acidic compositions for etching iron group metals
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/19—Iron or steel
Abstract
The invention discloses a method for chemically etching and thinning FeNi alloy foil strips, which comprises the following steps: pretreating FeNi alloy sheetUniformly spraying the FeNi alloy sheet by using etching liquid to etch and thin the FeNi alloy sheet to form a FeNi alloy foil strip, and performing post-treatment on the FeNi alloy foil strip; wherein the etching solution comprises FeCl 3 HCl and water. The method has simple process and easy operation, can further quickly and uniformly reduce the thickness of the FeNi alloy sheet, can remove the rolling hardening layer on the surface of the FeNi alloy sheet, and reduces the internal plastic strain and residual stress of the FeNi alloy sheet, thereby inhibiting the deformation during etching material reduction, effectively improving the flexibility of the FeNi alloy foil belt, remarkably improving the yield of mask manufacturing, and does not need post treatment. The method is suitable for FeNi alloy thin plates with various components, sizes and thicknesses, and the obtained FeNi alloy foil strip has uniform thickness and low surface roughness.
Description
Technical Field
The invention relates to a method for thinning a FeNi alloy foil strip, in particular to a method for chemically etching and thinning a FeNi alloy foil strip, and belongs to the field of nonferrous metal foil processing.
Background
The FeNi alloy foil strip is a preferred material for preparing the mask plate for OLED evaporation due to good processability and extremely low thermal expansion coefficient. As OLED resolution increases, smaller hole sizes and spacings on the reticle are required, and thus smaller thicknesses of reticle material are required, with a minimum thickness of 15 μm currently desired. However, with the current precision rolling process, it is limited to obtain a sheet with a thickness of 20-30 μm, and the rolling process is easy to form defects such as stripes on the surface of the sheet, and internal stress is generated in the strip, so that the sheet is easy to deform during further material reduction, and the subsequent etching process is affected.
Disclosure of Invention
The invention mainly aims to provide a method for chemically etching and thinning FeNi alloy foil strips so as to overcome the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the method for chemically etching and thinning the FeNi alloy foil belt provided by the embodiment of the invention comprises the following steps: pretreating a FeNi alloy sheet, uniformly spraying etching liquid on the FeNi alloy sheet to etch and thin the FeNi alloy sheet to form a FeNi alloy foil strip, and performing post-treatment on the FeNi alloy foil strip; wherein the etching solution comprises FeCl 3 HCl and water
Compared with the prior art, the method for thinning the FeNi alloy foil strip by chemical etching provided by the invention realizes uniform thinning of the FeNi alloy sheet by integral non-protective uniform spray etching, has a simple process and is easy to operate, not only can further quickly and uniformly reduce the thickness of the FeNi alloy sheet, but also can remove a rolling hardening layer on the surface of the FeNi alloy sheet and reduce the internal plastic strain and residual stress of the FeNi alloy sheet, thereby inhibiting deformation during material reduction by etching, effectively improving the flexibility of the FeNi alloy foil strip, remarkably improving the manufacturing yield of a mask, and needing no post treatment. The method is suitable for FeNi alloy thin plates with various components, sizes and thicknesses, particularly for large-area FeNi alloy thin plates, and the obtained FeNi alloy foil strip has uniform thickness, can be as low as 10 mu m and has low surface roughness (Ra is 0.15-0.3).
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those skilled in the art from this disclosure that the drawings described below are merely exemplary and that other embodiments may be derived from the drawings provided without undue effort.
FIG. 1 is an etched surface topography of a 50 μm thick FeNi alloy foil strip in example 1;
FIG. 2 is an etched surface topography of a FeNi alloy foil strip with a thickness of 25 μm in example 2;
FIG. 3 is an etched surface topography of a 20 μm thick FeNi alloy foil strip in example 3;
FIG. 4 is an etched surface topography of a FeNi alloy foil strip of 15 μm thickness in example 4;
FIG. 5 is an etched surface topography of a 10 μm thick FeNi alloy foil strip in example 5;
FIG. 6 is a cross-sectional profile of a 10 μm thick FeNi alloy foil strip etched in example 5.
Detailed Description
In view of the shortcomings of the prior art, the inventor of the present invention has long studied and practiced to propose a technical solution of the present invention, namely, a method for chemically etching and thinning a FeNi alloy foil strip, comprising: pretreating a FeNi alloy sheet, uniformly spraying etching liquid on the FeNi alloy sheet to etch and thin the FeNi alloy sheet to form a FeNi alloy foil strip, and performing post-treatment on the FeNi alloy foil strip; wherein the etching solution comprises FeCl 3 HCl and water.
Further, the thickness of the FeNi alloy sheet is 30-100 μm.
Further, the preprocessing includes: and sequentially performing first alkali washing treatment and first drying treatment on the FeNi alloy sheet.
Further, the cleaning liquid adopted in the first alkali cleaning treatment comprises KOH or NaOH aqueous solution with the concentration of 0.5-1 mol/L.
Further, the etching solution comprises 8 to 10mol/L hydrochloric acid and 10 to 30g/L FeCl 3 。
Further, the etching solution is composed of FeCl 3 HCl and water.
Further, the temperature of the etching solution is 25-35 ℃.
Further, the pressure of the spraying is 0.05-0.2 MPa.
Further, the spraying time is 5-20 minutes.
Further, the post-processing includes: and sequentially carrying out second alkaline washing treatment and second drying treatment on the FeNi alloy foil belt.
Further, the second alkaline washing treatment comprises: and spraying and cleaning the FeNi alloy foil strip by using an alkali solution.
Further, the alkali solution comprises KOH or NaOH aqueous solution with concentration of 0.2-0.5 mol/L.
Further, the first drying treatment and the second drying treatment adopt a drying mode, and the drying temperature is 40-60 ℃.
Further, the method for chemically etching and thinning the FeNi alloy foil strip further comprises the following steps: after the finishing, the surface yield of the FeNi alloy foil tape was checked.
In some more specific embodiments, the method of chemically etching a thin FeNi alloy foil strip comprises: firstly, alkaline washing is carried out on a FeNi alloy sheet to be thinned by using a KOH or NaOH aqueous solution with the concentration of 0.5-1 mol/L, surface pollutants possibly existing are removed, and the FeNi alloy sheet is dried by hot air; then evenly spraying the film by using etching solution with the temperature of 25-35 ℃ and the spraying pressure of 0.05-0.2 MPa, and determining the spraying time according to the thickness to be thinned, wherein the spraying time is generally 5-20 minutes; and (3) after the FeNi alloy sheet is reduced to the target thickness, taking out the obtained FeNi alloy foil belt, carrying out spray cleaning by using KOH or NaOH aqueous solution with the concentration of 0.2-0.5 mol/L, drying in a drying oven at the temperature of 40-60 ℃, and checking the surface yield.
In the embodiment, on the basis of the conventional etching technology, the uniform thinning of the FeNi alloy sheet is realized by an integral non-protection uniform spray etching method, the residual internal stress can be reduced, the flexibility of the foil belt is improved, the thickness is uniform (can be as low as 10 mu m), and the surface roughness (R) a 0.15 to 0.3) and no post-treatment is required.
The method has simple process and easy operation, and is suitable for FeNi alloy thin plates with various components, sizes and thicknesses, in particular for large-area FeNi alloy thin plates.
Other advantages and advantages of the present invention will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment 1 a method for chemically etching a thin FeNi alloy foil strip provided in this embodiment includes:
alkali washing FeNi alloy sheet with thickness of 100 μm with KOH aqueous solution of about 0.5mol/L for 5 min, and drying with hot air of about 40deg.C;
uniformly spraying FeNi alloy sheet with etching solution at 30deg.C containing 10mol/L HCl concentration and 30g/L FeCl 3 And the balance of water, wherein the spraying pressure is 0.2MPa, and the spraying time is 20 minutes;
taking out the obtained FeNi alloy foil belt, spraying and cleaning with NaOH aqueous solution with concentration of 0.5mol/L, and then drying in a drying oven at 40 ℃, wherein the thickness of the obtained FeNi alloy foil belt is 50 mu m, the etched surface morphology is shown in figure 1, and the surface stress value is not more than +/-5 MPa.
Comparative example 1 this comparative example provides a method of chemically etching a thin FeNi alloy foil strip substantially identical to example 1, except that: immersing the FeNi alloy sheet subjected to alkali washing and drying in etching solution at 30 ℃ for 20 minutes to obtain FeNi alloy foil with the thickness of 70 mu m and the surface roughness R a 0.45.
Embodiment 2 a method for chemically etching a thin FeNi alloy foil strip provided in this embodiment includes:
alkali washing FeNi alloy sheet with thickness of 50 μm with KOH aqueous solution of 0.6mol/L concentration for 5 min, and drying with hot air of about 50deg.C;
uniformly spraying FeNi alloy sheet with etching solution at 30deg.C containing 10mol/L HCl concentration and 30g/L FeCl 3 And the balance of water, wherein the spraying pressure is 0.2MPa, and the spraying time is 10 minutes;
the obtained FeNi alloy foil strip was taken out, sprayed and washed with an aqueous NaOH solution having a concentration of 0.5mol/L, and then dried in a drying oven at 60℃to obtain a FeNi alloy foil strip having a thickness of 25. Mu.m, and an etched surface morphology as shown in FIG. 2.
Embodiment 3 a method for chemically etching a thin FeNi alloy foil strip provided in this embodiment includes:
alkali washing FeNi alloy sheet with thickness of 40 μm with KOH aqueous solution of 0.5mol/L concentration for 3 min, and drying with hot air of about 60deg.C;
uniformly spraying FeNi alloy sheet with etching solution at 30deg.C containing 10mol/L HCl concentration and 15g/L FeCl 3 And the balance of water, wherein the spraying pressure is 0.1MPa, and the spraying time is 10 minutes;
the obtained FeNi alloy foil strip was taken out, sprayed and washed with an aqueous NaOH solution having a concentration of 0.5mol/L, and then dried in a drying oven at 50℃to obtain a FeNi alloy foil strip having a thickness of 20. Mu.m, and an etched surface morphology as shown in FIG. 3.
Example 4 the method for seed chemical etching thinning of FeNi alloy foil tape provided in this example comprises:
alkali washing FeNi alloy sheet with thickness of 25 μm with KOH aqueous solution of 0.5mol/L concentration for 5 min, and drying with hot air of about 60deg.C;
uniformly spraying FeNi alloy sheet with etching solution at 30deg.C, wherein the etching solution contains FeCl with HCl concentration of 9mol/L and FeCl concentration of 20g/L 3 And the balance of water, wherein the spraying pressure is 0.1MPa, and the spraying time is 5 minutes;
the obtained FeNi alloy foil strip was taken out, sprayed and washed with an aqueous NaOH solution having a concentration of 0.3mol/L, and then dried in a drying oven at 50℃to obtain a FeNi alloy foil strip having a thickness of 15. Mu.m, and an etched surface morphology as shown in FIG. 4.
Example 5 a method for chemically etching a thin FeNi alloy foil strip provided in this example includes:
alkali washing FeNi alloy sheet with thickness of 20 μm with KOH aqueous solution of 0.2mol/L concentration for 2 min, and drying with hot air of about 60deg.C;
uniformly spraying FeNi alloy sheet with etching solution at 30deg.C containing 8mol/L HCl concentration and 10g/L FeCl 3 And the balance of water, wherein the spraying pressure is 0.05MPa, and the spraying time is 5 minutes;
taking out the obtained FeNi alloy foil belt, spraying and cleaning with 0.2mol/L NaOH aqueous solution, and drying in a drying oven at 40 ℃, wherein the thickness of the obtained FeNi alloy foil belt is 10 μm, the etched surface morphology is shown in figure 5, and the cross section morphology is shown in figure 6.
While the invention has been described in detail with respect to the general description and specific embodiments thereof, it will be apparent to those skilled in the art that various modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (7)
1. A method of chemically etching a thin FeNi alloy foil strip, comprising: the method comprises the steps of carrying out pretreatment on a FeNi alloy sheet, wherein the pretreatment comprises the steps of sequentially carrying out first alkali washing treatment and first drying treatment on the FeNi alloy sheet, and then uniformly spraying the FeNi alloy sheet with etching liquid, wherein the temperature of the etching liquid is 25-35 ℃ and the spraying pressure is 0.05-0.2 MPa, so that the FeNi alloy sheet is etched and thinned to form a FeNi alloy foil strip, and then carrying out post-treatment on the FeNi alloy foil strip, and the post-treatment comprises the steps of sequentially carrying out second alkali washing treatment and second drying treatment on the FeNi alloy foil strip; wherein the etching solution comprises water, 8-10 mol/L hydrochloric acid and 10-30 g/L FeCl 3 Surface roughness R of FeNi alloy foil a 0.15 to 0.3.
2. The method of chemically etching a thin FeNi alloy foil strip according to claim 1, wherein: the thickness of the FeNi alloy sheet is 30-100 mu m.
3. The method of chemically etching a thin FeNi alloy foil strip according to claim 1, wherein: the cleaning solution adopted in the first alkali cleaning treatment comprises KOH or NaOH aqueous solution with the concentration of 0.5-1 mol/L.
4. The method of chemically etching a thin FeNi alloy foil strip according to claim 1, wherein: the spraying time is 5-20 minutes.
5. The method of chemically etching a thin FeNi alloy foil strip according to claim 1 wherein the second alkaline wash treatment comprises: spraying and cleaning the FeNi alloy foil strip by using an alkali solution, wherein the alkali solution comprises KOH or NaOH aqueous solution with the concentration of 0.2-0.5 mol/L.
6. The method of chemically etching a thin FeNi alloy foil strip according to claim 1, wherein: and the first drying treatment and the second drying treatment adopt a drying mode, and the drying temperature is 40-60 ℃.
7. The method of chemically etching a thin FeNi alloy foil strip of claim 1 further comprising: after the finishing, the surface yield of the FeNi alloy foil tape was checked.
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| JP3573303B2 (en) * | 1995-07-25 | 2004-10-06 | 日立金属株式会社 | Method for producing Fe-Ni-based alloy sheet having excellent surface cleanliness |
| JP3144280B2 (en) * | 1995-08-25 | 2001-03-12 | 住友金属工業株式会社 | Pretreatment method for iron-based metal materials for etching |
| JP5885993B2 (en) * | 2011-10-17 | 2016-03-16 | 関東化學株式会社 | Etching solution composition and etching method |
| CN104233302B (en) * | 2014-09-15 | 2016-09-14 | 南通万德科技有限公司 | A kind of etching solution and application thereof |
| JP6804301B2 (en) * | 2015-07-17 | 2020-12-23 | 凸版印刷株式会社 | Method for manufacturing base material for metal mask and method for manufacturing metal mask for vapor deposition |
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