CN115679219A - Iron-nickel alloy foil for precise metal mask plate and preparation method thereof - Google Patents
Iron-nickel alloy foil for precise metal mask plate and preparation method thereof Download PDFInfo
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- CN115679219A CN115679219A CN202211426255.5A CN202211426255A CN115679219A CN 115679219 A CN115679219 A CN 115679219A CN 202211426255 A CN202211426255 A CN 202211426255A CN 115679219 A CN115679219 A CN 115679219A
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Abstract
The invention discloses an iron-nickel alloy foil for a precise metal mask plate, which is characterized by comprising the following components in parts by weight: the iron-nickel alloy comprises 28-45 wt% of Ni and 0.1-19 wt% of M, wherein M is selected from at least one of Mn, cr, co, ti, al, mo, cu, V, sc, zn and Si, and the balance of iron and inevitable impurity elements; in the iron-nickel alloy crystal grains, the volume percentage of crystal grains in the crystal direction (200) is 5-99%, the volume percentage of crystal grains in the crystal direction (220) is 0.3-65%, the volume percentage of crystal grains in the crystal direction (311) is 0.1-30%, and the volume percentage of crystal grains in the crystal direction (111) is less than or equal to 10%. The method has the advantages of high flatness, low residual stress and uniform performance of all parts of the foil, so that the quality and the performance of the foil are improved, the uniformity of the performance of the etched material is also improved, and the yield of the mask plates are improved.
Description
Technical Field
The invention belongs to the technical field of metal material preparation, and particularly relates to an iron-nickel alloy foil for manufacturing a precise metal mask plate for an AMOLED display screen and a preparation method thereof.
Background
AMOLED (Active Matrix Organic Light Emitting Diode) is an Organic Light Emitting Diode, and has the advantages of Light weight, wide viewing angle, fast response time, low temperature resistance, high luminous efficiency, and the like, compared with a liquid crystal display, and is considered as a next-generation novel display technology. Generally, a vacuum evaporation technology is adopted to prepare an organic electroluminescent thin film, namely, an organic semiconductor material is heated in a vacuum environment, the material is heated and sublimated, an organic thin film device stack with a designed shape is formed on the surface of a substrate through a metal mask plate with a special sub-pixel pattern, continuous deposition and film formation of various materials are carried out, and an anode and a cathode are respectively plated at two ends of the stack to form an OLED (organic light emitting diode) light emitting device structure with multiple layers of thin films.
In the AMOLED display industry at present, a thermal evaporation process is used for manufacturing a sub-pixel OLED light-emitting device of a display screen; the light emitting layer of the OLED device in the sub-pixel region is deposited using a Fine Metal Mask (FMM) as a shadow Mask during evaporation. In order to manufacture a high-resolution AMOLED screen product, a precise metal mask plate must be used, and at present, three manufacturing methods of the precise metal mask plate are provided: 1. etching to form precise mask; 2. precision mask plate by electroforming method; 3. the mixed type precise mask plate does not need to be stretched. At present, the precision mask plate of the etching method can only realize the products of the OLED screen of 400-600 ppi, and products (the OLED screen of 400-800 ppi) which need to be manufactured with higher resolution need to use the precision mask plate of the electroforming method or the mixed mask plate. However, since the maturity of the two products is still insufficient, the AMOLED product is limited to 600ppi or less.
The etching method Metal Mask (FMM) is the most widely used at present, and the etching method Metal Mask is an ultrathin Metal sheet which is made of a smelted Metal plate through multi-section traditional hot rolling, heat treatment and cold rolling to the required thickness, wherein the ultrathin Metal sheet is usually an iron-nickel alloy and has the thickness of 20-40 mu m. The metal foil is subjected to yellow (photolithography), wet etching (wet etching) of the semiconductor, forming a pattern of numerous micro-holes in the ultra-thin metal foil, corresponding to the areas where the OLED light emitting devices of the light emitting sub-pixels in the desired AMOLED display are designed on the driving backplane.
With the improvement of the resolution of the AMOLED, the size of the pixel is reduced due to the improvement of the density of the pixel, the thickness of a precise metal mask used as a shadow mask in the patterning manufacture of the thermal evaporation OLED light emitting device is also reduced, and precise micropores corresponding to the positions and the sizes of the sub-pixels of the AMOLED display are manufactured on the mask. This also places higher demands on the properties of the thin metal foil as a starting material (e.g., high flatness, low residual stress, and high uniformity, high homogeneity, etc.) so that high yield precision metal reticles can be fabricated. If the metal foil is not flat or has too large residual stress, the problems of warping, deformation, micro-displacement and the like are easily generated when manufacturing the precise metal mask. The problem that the internal stress of the foil is unevenly distributed after etching, and further the FMM is not flat and deformed, so that the defects of the FMM finished product are caused and the like is easily caused.
Disclosure of Invention
The invention aims to solve the first technical problem of providing the iron-nickel alloy foil for the precise metal mask plate, which has high flatness, low residual stress and uniform performance.
The second technical problem to be solved by the invention is to provide an iron-nickel alloy foil for a precise metal mask plate and a preparation method thereof.
The technical scheme adopted by the invention for solving the first technical problem is as follows: the utility model provides an iron-nickel alloy foil for accurate metal mask board which characterized in that: the iron-nickel alloy comprises 28-45 wt% of Ni and 0.01-19 wt% of M, wherein M is selected from at least one of Mn, cr, co, ti, al, mo, cu, V, sc, zn and Si, and the balance of iron and inevitable impurity elements; in the iron-nickel alloy crystal grains, the volume percentage of crystal grains in the crystal direction (200) is 5-99%, the volume percentage of crystal grains in the crystal direction (220) is 0.3-65%, the volume percentage of crystal grains in the crystal direction (311) is 0.1-30%, and the volume percentage of crystal grains in the crystal direction (111) is less than or equal to 10%.
Preferably, the residual stress of the iron-nickel alloy foil is less than or equal to 140MPa.
Preferably, the iron-nickel alloy foil comprises skirt raised areas positioned on two sides of the foil and a central raised area positioned in the foil; the maximum protruding heights of the skirt edge protruding area and the central protruding area are less than or equal to 1mm; the average three-dimensional flatness of the raised area of the skirt edge is less than or equal to 1.5, and the average three-dimensional flatness of the central raised area is less than or equal to 1.
The raised skirt region, i.e., the bulge on the foil, is not completely contained within the metal foil on both sides of the irregularities.
The central raised area, i.e. the bulge on the foil, is completely contained within the foil.
The technical scheme adopted by the invention for solving the second technical problem is as follows: a preparation method of a multi-element iron-nickel alloy foil for a precise metal mask plate is characterized by comprising the following steps: the preparation process comprises the steps of preparing a foil blank → forming a foil material → tension straightening and/or tension annealing; the tension of the tension straightening and tension annealing is as follows: 10N-1000N/mm 2 The temperature of the tension annealing is 200-800 ℃, the annealing speed is 1-100 m/min, and the protection is carried out by adopting a reducing atmosphere.
Through carrying out tension straightening and/or tension annealing to the foil after the shaping, realize the final required microstructure of foil, realize high roughness when reducing foil residual stress, the tension that tension was annealed is: 10N-1000N/mm 2 If the tension is too low, the unevenness of the internal stress of the foil cannot be adjusted, and the improvement of the flatness and the plate shape cannot be improved; if the applied tension is too high, the yield strength and even tensile strength of the foil are too high, which may cause the foil to be too largeOr even fracture.
The method has the advantages that the microstructure required by the material finally is realized, the residual stress of the foil is further reduced, meanwhile, the high flatness is realized, preferably, the foil is heated in the tension straightening process, the heating temperature is 20-200 ℃, the annealing speed is 1-100 m/min, and the foil is protected by using a reducing atmosphere.
In order to realize the final required microstructure of the foil and finally obtain the foil with required specification, the process flow of foil forming preferably comprises hot forging → hot rolling → first heat treatment → cold rolling, second heat treatment → finish rolling and third heat treatment; the temperature of the first heat treatment, the second heat treatment and the third heat treatment is 670-810 ℃, and the annealing speed is 1-200 m/min; or at 250-400 deg.c and annealing speed of 1-100 m/min; or 60-200 ℃ and the annealing speed is 1-100 m/min.
Further, the hot forging temperature is preferably 800 to 1250 ℃.
Further, the hot rolling temperature is preferably 800 to 1250 ℃, and the single-pass hot rolling reduction ratio is preferably 20 to 80%.
Further, it is preferable that the rolling reduction in the single cold rolling pass is 25 to 60%.
Further, preferably, the foil blank is prepared by a casting process, a powder metallurgy laser melting process or an electroforming process.
Compared with the prior art, the invention has the advantages that: finally, the residual stress of the iron-nickel alloy foil is less than or equal to 140MPa, and the maximum protrusion heights of the skirt edge protrusion area and the central protrusion area are less than or equal to 1mm by controlling the preferred orientation of the iron-nickel alloy crystal grains, namely the volume percentage of the crystal grains in the crystal direction (200) is 5-99%, the volume percentage of the crystal grains in the crystal direction (220) is 0.3-65%, the volume percentage of the crystal grains in the crystal direction (311) is 0.1-30%, and the volume percentage of the crystal grains in the crystal direction (111) is less than or equal to 10%; the average three-dimensional flatness of the raised area of the skirt edge is less than or equal to 1 DEG, the average three-dimensional flatness of the raised area of the central part is less than or equal to 1 DEG, the high flatness, the low residual stress and the uniform performance of each part of the foil are achieved, the quality and the performance of the foil are improved, the uniformity of the performance of the etched material is also improved, and the yield of the precision metal mask manufactured by the method are improved.
Drawings
Fig. 1 is a three-dimensional flatness chart of example 1 of the present invention.
Fig. 2 is a three-dimensional flatness chart of example 2 of the present invention.
Fig. 3 is a three-dimensional flatness diagram of embodiment 3 of the present invention.
Fig. 4 is a three-dimensional flatness map of example 3 of the present invention.
FIG. 5 is a schematic diagram of a mask for thermal evaporation of a sixth generation half-plate size according to the present invention.
FIG. 6 is a process flow diagram of an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
The invention provides 19 example foils with the specific compositions shown in table 1.
The preparation steps of the examples are as follows:
1) The casting process comprises the following steps: burdening according to required components, and carrying out vacuum melting under the following conditions: 350-1700 ℃, vacuum degree: 0.01 to 10 4 Pa, then casting a cylindrical ingot with the diameter of 200-400 mm.
2) Hot forging: and forging the cast ingot at high temperature, wherein the large cylindrical cast ingot is forged into a square metal block for subsequent high-temperature forming processing, the hot forging temperature is 800-1250 ℃, and the thickness range of the hot forged metal block is 60-80 mm.
3) Hot rolling: and (3) carrying out hot rolling after the surface treatment of the hot-forged metal block, wherein the hot rolling temperature is 800-1250 ℃, and the hot rolling rate of a single pass is 20-80%. The metal block can be hot-rolled into a coil stock with the thickness of 4-8 mm by adopting a plurality of hot rolling processes.
4) First heat treatment: the hot rolled metal coil needs heat treatment, the microstructure is adjusted and the internal stress is removed, so that the subsequent cold rolling is carried out;
5) Cold rolling and secondary heat treatment: and (3) carrying out surface treatment on the hot-rolled coil stock to remove a surface oxide layer, cutting edges, cleaning, and then carrying out cold rolling, wherein the rolling rate of a single cold rolling pass is 25-60%, so that the metal coil stock with the thickness of less than 4mm is obtained. Because of the work hardening properties of metals, a second heat treatment is required to adjust the microstructure of the material and reduce internal stresses during cold rolling. In the embodiment, the cold rolling is performed in multiple passes, and the final cold rolled coil is obtained by combining the second heat treatment.
6) Finish rolling and third heat treatment: the precision rolling can control the thickness uniformity of the foil and the plate shape of the foil more accurately, the foil after cold rolling is used as a feed, the precision rolling rate is 20-70%, and the metal foil with the thickness of 10-100 mu m can be obtained after the precision rolling. Similar to cold rolling, to obtain a thin foil material, finish rolling is performed in multiple passes, and a final metal foil is obtained by combining a third heat treatment.
7) Tension straightening and/or tension annealing: the residual stress in the metal foil is eliminated through a tension leveling machine, and the tension of tension straightening and tension annealing is as follows: 10N-1000N/mm 2 The temperature of the tension annealing is 200-600 ℃, the annealing speed is 1-100 m/min, and the protection is carried out by adopting a reducing atmosphere. The tension straightening can be carried out at room temperature or simultaneously heating the foil, wherein the heating temperature is 20-200 ℃, the annealing speed is 1-100 m/min, and the foil is protected by adopting a reducing atmosphere.
The temperature of the first heat treatment, the second heat treatment and the third heat treatment is 670 ℃ to 810 ℃, and the annealing speed is 1 m/min to 200m/min; or at 250-400 deg.c and annealing speed of 1-100 m/min; or 60-200 ℃ and the annealing speed is 1-100 m/min.
The comparative example differs from example 1 in that: tension straightening and/or tension annealing is omitted.
The following performance tests were carried out on the obtained examples and comparative examples:
1) And (3) detecting the height of the bulge: and detecting the surface flatness of the foil by using a surface height measuring instrument, and measuring the maximum protrusion height of the skirt edge protrusion area and the central protrusion area of the foil from the data.
2) Three-dimensional flatness: the surface flatness of the foil is detected by a surface height measuring instrument, and the measured flatness data can obtain the data of three-dimensional flatness (HSR, hump Size Ratio) according to the following equation:
HSR＝(((H*(X+Y))/(X*Y))*100；
wherein H: the height of the raised area on the foil; x: the width of the raised area as measured from the cross-section in the rolling direction (longitudinal direction); y: the width of the raised area measured from a widthwise (transverse) cross-section, and the data obtained from the surface height measurement of the three-dimensional flatness are represented by three-dimensional contour plots, as shown in fig. 1 to 4. The three-dimensional flatness (HSR) can be measured in three regions, namely the skirt raised regions on both sides of the foil and the central raised region in the foil, the main raised regions in each region are calculated, and the Average three-dimensional flatness (Average HSR) of each region is obtained.
3) Residual stress: detecting by high-precision X-ray diffraction (XRD);
4) The precise metal mask plate for the sixth generation half-plate size thermal evaporation is prepared by wet etching in the embodiments 1 to 4, and as shown in fig. 5, the total longitudinal radiation length (TP) is detected for each sub-pixel point with 8 edges in each screen area of the screen area on the whole mask plate X ) Transverse total width of spoke (TP) Y ) Deviation of measured distance from design distance, total longitudinal spoke length (TP) X ) Transverse total width of spoke (TP) Y ) The definition of (A) is as follows:
TP X1 = (measured distance between points 1-15-design distance between points 1-15);
TP X2 = (measured distance between points 25-16-design distance between points 25-16);
TP X3 = (measured distance between points 26-40-design distance between points 26-40);
TP Y1 = (measured distance between points 1-26-design distance between points 1-26);
TP Y7 = (measured distance between points 7-32-design distance between points 7-32);
TP Y15 = (measured distance between points 15-40-design distance between points 15-40).
Detecting TP X1 And TP X3 Difference of (A) and TP Y The extreme difference between (i.e., TP) Y Maximum value and TP Y Difference of minimum value), shown in Table 3, TP X1 And TP X3 The difference of (D) is within +/-20 mu m, and the total width of TP y The range of the extreme difference is +/-5 mu m, and the AMOLED display screen for the high-quality intelligent mobile phone is met.
In the comparison example, the grain preferred orientation of the foil, the residual stress and the three-dimensional flatness of the obtained foil do not meet the requirements of the invention, and the foil is easy to deform or be uneven after etching, so that a precise metal mask plate (FMM) for thermal evaporation with the size of a half plate in the sixth generation cannot be manufactured.
Table 1 composition/wt.% of inventive examples, comparative examples
TABLE 2 microcrystalline phase structure and foil Properties of inventive and comparative examples
Table 3 properties of the precision metal mask prepared in examples 1 to 4 of the present invention
Claims (10)
1. The utility model provides an iron-nickel alloy foil for accurate metal mask board which characterized in that: the weight percentage of the iron-nickel alloy is 28-45 wt% of Ni, 0.01-19 wt% of M, wherein M is selected from at least one of Mn, cr, co, ti, al, mo, cu, V, sc, zn and Si, and the balance is iron and inevitable impurity elements; in the crystal grains of the iron-nickel alloy foil, the volume percentage of the crystal grains in the crystal direction (200) is 5-99%, the volume percentage of the crystal grains in the crystal direction (220) is 0.3-65%, the volume percentage of the crystal grains in the crystal direction (311) is 0.1-30%, and the volume percentage of the crystal grains in the crystal direction (111) is less than or equal to 10%.
2. The iron-nickel alloy foil for the precise metal mask plate according to claim 1, which is characterized in that: the residual stress of the iron-nickel alloy foil is less than or equal to 140MPa.
3. The iron-nickel alloy foil for the precise metal mask plate according to claim 1, which is characterized in that: the iron-nickel alloy foil comprises skirt edge convex areas positioned on two sides of the foil and a central convex area positioned in the foil, wherein the maximum convex heights of the skirt edge convex area and the central convex area are both less than or equal to 1mm; the average three-dimensional flatness of the raised areas of the skirt edges is less than or equal to 1.5, and the average three-dimensional flatness of the raised areas of the central part is less than or equal to 1.
4. The method for preparing the iron-nickel alloy foil for the precise metal mask plate according to claim 1, 2 or 3, which is characterized by comprising the following steps: the preparation process comprises the steps of preparing a foil blank → forming a foil material → tension straightening and/or tension annealing; the tension of tension straightening and tension annealing is as follows: 10N-1000N/mm 2 The temperature of the tension annealing is 200-800 ℃, the annealing speed is 1-100 m/min, and the protection is carried out by adopting a reducing atmosphere.
5. The method for preparing the iron-nickel alloy foil for the precise metal mask plate according to claim 4, wherein the method comprises the following steps: and heating the foil in the tension straightening process, wherein the heating temperature is 20-200 ℃, the annealing speed is 1-100 m/min, and the foil is protected by a reducing atmosphere.
6. The method for preparing the iron-nickel alloy foil for the precise metal mask plate according to claim 4, wherein the method comprises the following steps: the process flow of the foil forming comprises hot forging → hot rolling → first heat treatment → cold rolling, second heat treatment → finish rolling and third heat treatment; the temperature of the first heat treatment, the second heat treatment and the third heat treatment is 670-810 ℃, and the annealing speed is 1-200 m/min; or at 250-400 deg.c and annealing speed of 1-100 m/min; or 60-200 ℃ and the annealing speed is 1-100 m/min.
7. The method for preparing the iron-nickel alloy foil for the precise metal mask plate according to claim 6, which is characterized in that: the hot forging temperature is 800-1250 ℃.
8. The method for preparing the iron-nickel alloy foil for the precise metal mask plate according to claim 6, which is characterized in that: the hot rolling temperature is 800-1250 ℃, and the single-pass hot rolling rate is 20-80%.
9. The method for preparing the iron-nickel alloy foil for the precise metal mask plate according to claim 6, wherein the method comprises the following steps: the rolling rate of the cold rolling single pass is 25-60%.
10. The method for preparing the iron-nickel alloy foil for the precise metal mask plate according to claim 4, wherein the method comprises the following steps: the preparation of the foil blank adopts a casting process, a powder metallurgy laser melting process or an electroforming process.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116197680A (en) * | 2023-03-21 | 2023-06-02 | 寰采星科技(宁波)有限公司 | Manufacturing method of precise metal mask strip |
| CN116237364A (en) * | 2023-03-21 | 2023-06-09 | 寰采星科技(宁波)有限公司 | Preparation method of high-flatness metal foil and metal foil obtained by preparation method |
| CN116377284A (en) * | 2023-03-08 | 2023-07-04 | 北京北冶功能材料有限公司 | Iron-nickel-based soft magnetic alloy foil and preparation method and application thereof |
| CN116445764A (en) * | 2023-03-08 | 2023-07-18 | 北京北冶功能材料有限公司 | Iron-nickel-based soft magnetic alloy foil and preparation method and application thereof |
| CN116511842A (en) * | 2023-04-27 | 2023-08-01 | 寰采星科技(宁波)有限公司 | Manufacturing method of precise metal mask plate and precise metal mask plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116377284A (en) * | 2023-03-08 | 2023-07-04 | 北京北冶功能材料有限公司 | Iron-nickel-based soft magnetic alloy foil and preparation method and application thereof |
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| CN116197680A (en) * | 2023-03-21 | 2023-06-02 | 寰采星科技(宁波)有限公司 | Manufacturing method of precise metal mask strip |
| CN116237364A (en) * | 2023-03-21 | 2023-06-09 | 寰采星科技(宁波)有限公司 | Preparation method of high-flatness metal foil and metal foil obtained by preparation method |
| CN116197680B (en) * | 2023-03-21 | 2023-09-29 | 寰采星科技(宁波)有限公司 | Manufacturing method of precise metal mask strip |
| CN116511842A (en) * | 2023-04-27 | 2023-08-01 | 寰采星科技(宁波)有限公司 | Manufacturing method of precise metal mask plate and precise metal mask plate |
| CN116511842B (en) * | 2023-04-27 | 2023-10-03 | 寰采星科技(宁波)有限公司 | Manufacturing method of precise metal mask plate and precise metal mask plate |
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