Detection method for inclusion of OLED metal mask plate material

Abstract

The invention provides a method for detecting impurities in an OLED (Organic Light Emitting Diode) metal mask plate material, and relates to the technical field of mask plates. The detection method for the inclusion of the OLED metal mask plate material comprises the following steps: sampling at different stages in a production process; cleaning and weighing the sample; preparing an acid dissolving liquid medicine, and dissolving the sample in an acid solution; carrying out vacuum filtration on the dissolved solution and drying filter paper; and analyzing the inclusions on the dried filter paper by adopting a scanning electron microscope and an energy dispersive spectrometer. And the technical effect of better detecting the inclusions of the metal mask plate material is achieved.

Description

Technical Field

[0001] The present invention relates to the technical field of mask plates, and in particular to a method for detecting inclusions in metal mask plate materials for OLEDs. Background Art

[0002] Ultra-thin stainless steel precision strip has ultra-thin thickness, light weight, high strength and good processing formability. It is a key material in the high-end electronics industry, such as the production of fine metal mask plates. Ultra-thin stainless steel precision strip has very high requirements for inclusions, and the size and number of inclusions need to be strictly controlled. Currently, metallographic microscopic rating method and electrolytic extraction-energy spectrum analysis method are generally used.

[0003] The metallographic microscopic rating method can qualitatively observe and rate the inclusions in the field of view in terms of type and shape, but it is difficult to use for quantitative detection of inclusions in multiple fields of view in larger samples, especially it is impossible to quickly obtain accurate information such as the number and size of inclusions. In particular, it is difficult to find inclusions in samples of high-purity materials at the ingot and forging stages using the metallographic method, and the surface area of ​​the material is constantly changing in different process sections, so it is impossible to compare and analyze the inclusion data of different process sections.

[0004] The electrolytic extraction-energy spectrum analysis method can obtain the type, shape and statistical quantity of inclusions, but its analysis cycle is long, the efficiency is low, the human error is large, and some material matrices are difficult to dissolve into the electrolyte and the inclusions are dissolved in the electrolyte during the long electrolysis process, which makes it difficult to accurately quantify the inclusions and cannot compare the number and type of inclusions of different materials. Summary of the invention

[0005] The object of the present invention is to provide a method for detecting inclusions in an OLED metal mask material, so as to alleviate the technical problem that the inclusions in the metal mask material cannot be detected well in the prior art.

[0006] In a first aspect, an embodiment of the present invention provides a method for detecting inclusions in an OLED metal mask material, comprising the following steps:

[0007] Taking samples at different stages of the production process;

[0008] The samples were cleaned and weighed;

[0009] Prepare an acid dissolving solution and place the sample in the acid solution to dissolve;

[0010] The dissolved solution was vacuum filtered and the filter paper was dried;

[0011] The inclusions on the dried filter paper were analyzed using scanning electron microscopy and energy dispersive spectrometer.

[0012] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein samples are taken during the ingot, forging, hot rolled strip, rough rolled strip and finished thin strip process stages of the material production process, and the sample weight is between 6g and 50g.

[0013] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein the sample is cleaned with alcohol or a low-concentration acid reagent.

[0014] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein the low-concentration acid reagent includes hydrochloric acid with a concentration of 0.05%-1%.

[0015] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein the acid dissolving liquid includes hydrogen peroxide, sulfuric acid and purified water;

[0016] The proportion of the hydrogen peroxide is between 1% and 3%, the proportion of the sulfuric acid is between 10% and 15%, and the proportion of the pure water is between 82% and 89%.

[0017] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein, after the sample is completely dissolved, vacuum filtration is performed using a vacuum filter and acid-resistant filter paper, and the pore size of the acid-resistant filter paper does not exceed 2 microns;

[0018] After vacuum filtration, place the acid-resistant filter paper in a drying oven and dry it at low temperature.

[0019] In combination with the first aspect, the embodiment of the present invention provides a possible implementation of the first aspect, wherein the temperature in the drying box is set between 40-60 degrees Celsius.

[0020] In combination with the first aspect, an embodiment of the present invention provides a possible implementation method of the first aspect, wherein, after the acid-resistant filter paper is dried, a scanning electron microscope is used to observe the inclusions on the acid-resistant filter paper, and the field of view of the scanning electron microscope is selected from the 0° position, 90° position, 180° position and 270° position on the circular acid-resistant filter paper, and at least two fields of view are photographed and analyzed at each position.

[0021] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein the field of view of the scanning electron microscope is evenly distributed on the circular acid-resistant filter paper.

[0022] In combination with the first aspect, an embodiment of the present invention provides a possible implementation of the first aspect, wherein the inclusion composition is analyzed using an energy dispersive spectrometer after being observed under a scanning electron microscope.

[0023] Beneficial effects:

[0024] The present invention provides a method for detecting inclusions in OLED metal mask materials, comprising the following steps: sampling at different stages in a production process; cleaning and weighing the samples; preparing an acid dissolving solution and placing the samples in the acid solution to dissolve; vacuum filtering the dissolved solution and drying the filter paper; and analyzing the inclusions on the dried filter paper using a scanning electron microscope and an energy spectrometer.

[0025] Specifically, in the process of inclusion analysis of Fe-Ni alloy or Fe-Ni-Co alloy material, which is the raw material for fine metal mask production, samples are taken at different stages of the production process of the raw materials, and the samples are cleaned. Then, the cleaned samples are weighed, and the samples are put into an acid dissolving agent. The samples are dissolved by the acid dissolving agent, and the inclusions in the samples are left behind. Then, the dissolved solution is vacuum filtered so that the filtered residue is evenly distributed on the filter paper, and the filter paper is dried. Then, the staff uses a scanning electron microscope to directly observe the inclusions on the filter paper to know the number of inclusions, and uses an energy spectrometer to analyze the composition of the inclusions, so as to know the proportion of various inclusions, so as to better feedback the front-end process for adjustment, control raw materials, improve the front-end production process, and improve the quality of raw materials for fine metal mask production. In addition, through acid dissolution, the sample can be quickly dissolved, saving detection time and improving detection efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0027] Figure 1 A schematic diagram of a method for detecting inclusions in an OLED metal mask material provided by an embodiment of the present invention. DETAILED DESCRIPTION

[0028] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0030] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0031] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0032] The present invention is further described in detail below through specific embodiments in conjunction with the accompanying drawings.

[0033] See also Figure 1 As shown, this embodiment provides a method for detecting inclusions in OLED metal mask materials, comprising the following steps: sampling at different stages of the production process; cleaning and weighing the samples; preparing an acid dissolving solution and placing the samples in the acid solution to dissolve; vacuum filtering the dissolving solution and drying the filter paper; and analyzing the inclusions on the dried filter paper using a scanning electron microscope and an energy spectrometer.

[0034] Specifically, in the process of inclusion analysis of Fe-Ni alloy or Fe-Ni-Co alloy material, which is the raw material for fine metal mask production, samples are taken at different stages of the production process of the raw materials, and the samples are cleaned. Then, the cleaned samples are weighed, and the samples are put into an acid dissolving agent. The samples are dissolved by the acid dissolving agent, and the inclusions in the samples are left behind. Then, the dissolved solution is vacuum filtered so that the filtered residue is evenly distributed on the filter paper, and the filter paper is dried. Then, the staff uses a scanning electron microscope to directly observe the inclusions on the filter paper to know the number of inclusions, and uses an energy spectrometer to analyze the composition of the inclusions, so as to know the proportion of various inclusions, so as to better feedback the front-end process for adjustment, control raw materials, improve the front-end production process, and improve the quality of raw materials for fine metal mask production. In addition, through acid dissolution, the sample can be quickly dissolved, saving detection time and improving detection efficiency.

[0035] It should be pointed out that the electrolytic extraction-energy spectrum analysis method in the prior art has a long electrolysis time and will completely decompose the inclusions, making it difficult to accurately quantify the inclusions and unable to conduct comparative analysis on the number and type of inclusions in different materials.

[0036] It should also be pointed out that although the phase microscopic rating method can qualitatively observe and rate the inclusions in the field of view in terms of type and shape, it is difficult to use for quantitative detection of inclusions in multiple fields of view in larger samples, especially the inability to quickly obtain accurate information such as the number and size of inclusions. In particular, it is difficult to find inclusions in samples of high-purity materials at the ingot and forging stages using the metallographic method, and the surface area of ​​the material is constantly changing in different process sections. Therefore, it is impossible to compare and analyze the inclusion data of different process sections.

[0037] The method for detecting inclusions in OLED metal mask materials provided in this embodiment can detect different production stages of raw materials for fine metal mask plates, and has high detection efficiency and high precision.

[0038] Specifically, the detection method for inclusions in OLED metal mask materials provided in this embodiment includes the following steps: sampling in the ingot, forging, hot-rolled strip, rough-rolled strip and fine-rolled thin strip process stages of the material production process, and the sample weight is between 6g and 50g. Then, the sample is cleaned with alcohol or a low-concentration acid reagent, wherein the low-concentration acid can be 0.05%-1% hydrochloric acid, or the low-concentration acid can also be 0.05%-1% nitric acid. Then, an acid dissolving solution mixed with hydrogen peroxide, sulfuric acid and pure water is prepared, and the sample is placed in a beaker containing the acid dissolving solution in the acid fume hood, and the sample is quickly dissolved under the action of a magnetic stirrer. After the sample is dissolved, the acid is filtered using a vacuum filter and an acid-resistant filter paper (where the pore size of the acid-resistant filter paper is within 2 microns), wherein the acid-resistant filter paper is laid flat in the vacuum filter so that the inclusions can be evenly distributed on the filter paper. After the belt filtration is completed, the filter paper is dried at a low temperature in an oven. After drying, the staff used SEM (scanning electron microscope) equipment and EDS (energy dispersive spectrometer) component analysis module to analyze the inclusions on the acid-resistant filter paper, including the number, size, and composition of inclusions within a fixed magnification field of view. The size of a single field of view is specified to be 800 times, and the area of ​​a single field of view is about 0.2637mm 2 , and it is required to shoot and analyze at least 4-12 800x fields of view. The positions of the fields of view can be selected along the 0° position, 90° position, 180° position and 270° position of the circular acid-resistant filter paper, and shoot and analyze more than 1-3 fields of view at each position (multiple fields of view at each position are equally divided along the radius of the filter paper). Finally, the average value of the number and size of inclusions in each field of view is calculated, and the composition of the inclusions is counted and classified to calculate the percentage of each type of inclusions.

[0039] By comparing the number, size and composition of inclusions in different process stages of the same smelting process and in the same process stage of different smelting processes, we can determine the influence of the process on inclusions and improve the process and product quality in a targeted manner, so that the material purity meets the requirements of FMM. Mask, reduce the addition of corresponding elements, control raw materials, and improve purification process.

[0040] Among them, the raw materials for the production of fine metal mask plates are Fe-Ni alloy or Fe-Ni-Co alloy materials, and trace amounts of silicon oxide, aluminum oxide, magnesium oxide and combinations thereof are doped in the raw materials. The detection method for inclusions in OLED metal mask plate materials provided in this embodiment uses an acid dissolving solution mixed with hydrogen peroxide, sulfuric acid and pure water to dissolve the raw materials. The dilute sulfuric acid solution can dissolve the Fe-Ni alloy or Fe-Ni-Co alloy material, so that the inclusions of silicon oxide, aluminum oxide, magnesium oxide and combinations thereof are retained, thereby enabling the staff to accurately detect.

[0041] Among them, for the sample weight, the staff can take 6g sample, or the staff can take 10g sample, or the staff can take 20g sample, or the staff can take 30g sample, or the staff can take 40g sample, or the staff can take 50g sample, or the staff can take 60g sample.

[0042] Among them, in the pharmaceutical ratio of the acid-dissolving solution, hydrogen peroxide accounts for 1%, sulfuric acid accounts for 10%, and pure water accounts for 89%, or hydrogen peroxide accounts for 2%, sulfuric acid accounts for 10%, and pure water accounts for 82%, hydrogen peroxide accounts for 3%, sulfuric acid accounts for 10%, and pure water accounts for 87%, hydrogen peroxide accounts for 1%, sulfuric acid accounts for 12%, and pure water accounts for 86%, hydrogen peroxide accounts for 1%, sulfuric acid accounts for 15%, and pure water accounts for 84%, hydrogen peroxide accounts for 3%, sulfuric acid accounts for 15%, and pure water accounts for 82%.

[0043] Among them, the temperature in the drying box can be set to 40 degrees Celsius, or the temperature in the drying box can be set to 45 degrees Celsius, or the temperature in the drying box can be set to 50 degrees Celsius, or the temperature in the drying box can be set to 55 degrees Celsius, or the temperature in the drying box can be set to 60 degrees Celsius.

[0044] In Table 1 and Table 2, both Example 1 and Comparative Example 1 use high-purity Fe-36NiInvar materials, which are samples from the same ingot furnace number, the same sampling position, and different processing stages. These samples are compared and analyzed using different inclusion analysis methods, wherein Example 1 is a method for detecting inclusions in OLED metal mask materials provided in this embodiment, and Comparative Example 1 is a prior art SEM metallographic method.

[0045] Table 1

[0046]

[0047]

[0048] Table 2

[0049]

[0050] As shown in Table 1 and Table 2, the detection method for inclusions in OLED metal mask materials provided in this embodiment uses a rapid dissolution method to quantitatively analyze the inclusion levels of materials at different process stages from ingot to thin strip, and can analyze the types and proportions of inclusions, with strong reliability and comparability. The SEM metallographic method is limited to analyzing two-dimensional cross-sections, and the surface area of ​​the material is constantly changing during the process from ingot to thin strip, and cannot accurately quantify and analyze inclusions.

[0051] In Table 3 and Table 4, Example 1 and Comparative Example 2 both use high-purity Fe-36NiInvar materials, which are samples from the same ingot furnace number, the same sampling position, and different processing stages. These samples are compared and analyzed using different inclusion analysis methods. Comparative Example 2 is the prior art electrolysis method.

[0052] Table 3

[0053]

[0054] Table 4

[0055]

[0056] As shown in Table 3 and Table 4, the detection method for inclusions in OLED metal mask materials provided in this embodiment adopts a rapid dissolution method to quantitatively analyze the inclusion levels of materials at different process stages from ingots to thin strips, and can analyze the types and proportions of inclusions, with strong reliability and comparability. The electrolysis method requires a long time for electrolysis, and some inclusions have been dissolved during the electrolysis process, and the remaining part of the matrix material is not dissolved, resulting in a particularly large error in the quantitative analysis of inclusions.

[0057] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for detecting inclusions in OLED metal mask materials, characterized in that: The following steps are involved: Taking samples at different stages of the production process; The samples were cleaned and weighed; Prepare an acid dissolving solution and place the sample in the acid solution to dissolve; The dissolved solution was vacuum filtered and the filter paper was dried; The inclusions on the dried filter paper were analyzed using scanning electron microscopy and energy dispersive spectrometer.

2. The method for detecting inclusions in OLED metal mask materials according to claim 1, characterized in that: Samples are taken during the ingot, forging, hot-rolled strip, rough-rolled strip and finish-rolled thin strip process stages of the material production process, and the sample weight is between 6g and 50g.

3. The method for detecting inclusions in OLED metal mask materials according to claim 2, characterized in that: Use alcohol or low concentration acid reagent to clean the sample.

4. The method for detecting inclusions in OLED metal mask material according to claim 3, characterized in that: Low concentration acid reagents include hydrochloric acid with a concentration of 0.05%-1%.

5. The method for detecting inclusions in OLED metal mask material according to claim 1, characterized in that: The acid dissolving liquid includes hydrogen peroxide, sulfuric acid and purified water; The proportion of the hydrogen peroxide is between 1% and 3%, the proportion of the sulfuric acid is between 10% and 15%, and the proportion of the pure water is between 82% and 89%.

6. The method for detecting inclusions in OLED metal mask materials according to claim 1, characterized in that: When the sample is completely dissolved, vacuum filtration is performed using a vacuum filter and acid-resistant filter paper, the pore size of the acid-resistant filter paper not exceeding 2 microns; After vacuum filtration, place the acid-resistant filter paper in a drying oven and dry it at low temperature.

7. The method for detecting inclusions in OLED metal mask material according to claim 6, characterized in that: The temperature in the drying box is set between 40-60 degrees Celsius.

8. The method for detecting inclusions in OLED metal mask materials according to claim 1, characterized in that: After the acid-resistant filter paper is dried, a scanning electron microscope is used to observe the inclusions on the acid-resistant filter paper. The field of view of the scanning electron microscope is selected from the 0° position, 90° position, 180° position and 270° position on the circular acid-resistant filter paper. At least two fields of view are photographed and analyzed at each position.

9. The method for detecting inclusions in OLED metal mask material according to claim 8, characterized in that: The field of view of the scanning electron microscope is evenly distributed on the circular acid-resistant filter paper.

10. The method for detecting inclusions in OLED metal mask material according to claim 8, characterized in that: After observation under scanning electron microscope, the inclusion composition was analyzed using energy dispersive spectrometer.

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