Surface residue detection method

Abstract

The invention discloses a surface residue detection method, which is used for detecting organic pollutants and inorganic pollutants on the surface of a to-be-detected product, and comprises the following steps: dispersing a modified silane coupling agent solution on the surface of the to-be-detected product, and heating the to-be-detected product; placing the to-be-detected product in the ultraviolet fluorescence detection equipment, and detecting to obtain the total fluorescence intensity of the to-be-detected product; and comparing the total fluorescence intensity with a preset highest fluorescence intensity value, and judging whether the residual quantity of the surface residues of the to-be-detected product is qualified or not. The modified silane coupling agent solution is dispersed on the surface of the to-be-detected product, so that the modified silane coupling agent solution and the inorganic residues on the surface of the to-be-detected product form a fluorescent complex, and simultaneous detection of the organic pollutants and the inorganic residues is realized.

Description

Technical Field

[0001] The present application relates to the field of detection, and in particular to a method for detecting surface residues. Background Art

[0002] In current technology, methods for detecting surface cleanliness based on the principle of fluorescence effect include: X-ray fluorescence analysis, ultraviolet fluorescence analysis, etc. However, X-ray fluorescence analysis requires X-ray excitation, which is difficult to use on the production site. Ultraviolet fluorescence analysis can only detect organic dirt on the surface, but cannot detect inorganic dirt. Therefore, it is urgent to develop a method that can be applied to the production site and can detect both organic and inorganic dirt, so as to realize the detection of residues on the product surface. Summary of the invention

[0003] In view of this, the present application provides a method for detecting surface residues that can solve the above-mentioned technical problems.

[0004] A method for detecting surface residues, used for detecting organic pollutants and inorganic pollutants on the surface of a product to be tested, comprising: Dispersing a modified silane coupling agent solution on the surface of the product to be tested, and heating the product to be tested; Placing the product to be tested in an ultraviolet fluorescence detection device to detect and obtain the total fluorescence intensity of the product to be tested; The total fluorescence intensity is compared with a preset maximum fluorescence intensity value to determine whether the residual amount of the surface residue of the product to be tested is qualified.

[0005] In some embodiments, the modified silane coupling agent solution comprises, by weight: 3 to 25 parts of conjugated molecule modified silane coupling agent; 60 to 80 parts of organic solvent; 5 to 15 parts of inorganic solvent.

[0006] In some embodiments, the structural formula of the conjugated molecule modified silane coupling agent is: , Wherein, X1, X2, X3 are each independently one of methoxy, ethoxy, propoxy, isopropoxy, hydroxyl, chlorine or bromine, and Y is one of vinyl, propenyl, butenyl, butadienyl, phenyl, phenol, benzyl or anthracenyl.

[0007] In some embodiments, at least one of X1, X2, and X3 is methoxy, and Y is butadiene.

[0008] In some embodiments, the heating temperature is 40° C. to 80° C., and the heating time is 2 min to 15 min.

[0009] In some embodiments, the organic solvent includes one or more of methanol, ethanol, propanol, isopropanol, or acetic acid.

[0010] In some embodiments, before the step of "dispersing the modified silane coupling agent solution on the surface of the product to be tested", the method further includes: placing the product to be tested in an ultraviolet fluorescence detection device to detect the fluorescence intensity of the organic pollutants on the surface of the product to be tested; After the step of "placing the product to be tested in an ultraviolet fluorescence detection device to detect the total fluorescence intensity of the product to be tested", the method also includes: in the surface residue of the product to be tested, the quantified fluorescence intensity corresponding to the inorganic pollutant is the difference between the total fluorescence intensity and the fluorescence intensity of the organic pollutant.

[0011] In some embodiments, the material of the product to be tested is metal, and the inorganic pollutant includes inorganic silicon.

[0012] In some embodiments, the method comprises: obtaining a plurality of products having residues on their surfaces, and measuring the total fluorescence intensity of each product; covering the surface of each of the products with an adhesive tape, and measuring the pull-out force P of each of the adhesive tapes, and establishing a standard curve equation between the pull-out force P and the total fluorescence intensity of each of the products, and obtaining a standard curve equation between the pull-out force P of the adhesive tape and the total fluorescence intensity of each of the products through data fitting.

[0013] In some embodiments, it includes: determining the maximum fluorescence intensity value based on the set minimum pull-out force and the standard curve equation; if the total fluorescence intensity is less than or equal to the maximum fluorescence intensity value, then judging that the residual amount of the surface residue of the product to be tested is qualified; if the total fluorescence intensity is higher than the maximum fluorescence intensity value, then judging that the residual amount of the surface residue of the product to be tested is unqualified.

[0014] The present application adopts a modified silane coupling agent solution dispersed on the surface of the product to be tested, so that the modified silane coupling agent solution and the inorganic residues on the surface of the product to be tested form a fluorescent complex, and when ultraviolet fluorescence detection is performed, the total fluorescence intensity of the residues on the surface of the product to be tested is obtained. The total fluorescence intensity of the residues on the surface of the product to be tested is the sum of the fluorescence intensity of the inorganic residues on the surface of the product to be tested and the fluorescence intensity of the organic residues on the surface of the product to be tested. The total fluorescence intensity obtained by the detection is compared with the preset maximum fluorescence intensity value to determine whether the residual amount of the surface residues of the product to be tested is qualified, thereby realizing fluorescence detection of the surface residues. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 A schematic flow chart of a method for detecting surface residues provided in accordance with one embodiment of the present application.

[0016] Figure 2 A fitted line graph of the second fluorescence intensity and the pulling force provided in one embodiment of the present application. DETAILED DESCRIPTION

[0017] The embodiments of the present application are described in detail below. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present application, and cannot be understood as limiting the present application. The reagents and materials described in the following embodiments can all be obtained from commercial sources.

[0018] In the anode masking process, tape is usually used to mask the product surface. When the surface of the area to be masked is not cleaned properly, the residual pollutants (organic residues and inorganic residues) will reduce the adhesion of the tape, and eventually lead to poor liquid penetration in the masking area. Therefore, the control of product surface cleanliness is the key to ensuring process stability and yield.

[0019] The small amount of organic and inorganic residues left on the surface of the product due to improper cleaning cannot be judged by human visual inspection. Therefore, the present application provides a method that can effectively detect the organic and inorganic pollutants remaining on the surface of the product to quantitatively detect the surface residues.

[0020] Specifically, see Figure 1 The present application provides a method for detecting surface residues, which is used to detect organic pollutants and inorganic pollutants on the surface of a product to be tested, comprising: Dispersing the modified silane coupling agent solution on the surface of the product to be tested, and heating the product to be tested; The product to be tested is placed in an ultraviolet fluorescence detection device to detect the total fluorescence intensity of the surface residue of the product to be tested; The total fluorescence intensity is compared with a preset maximum fluorescence intensity value to determine whether the residual amount of the surface residue of the product to be tested is qualified.

[0021] The working principle of the above detection method is: after the organic residues on the surface of the product to be tested absorb ultraviolet light, they are excited by photons, and the electrons in the organic residues reach a higher energy level excited state. However, this high energy level excited state is unstable, and when the electrons return to the initial energy level, they will release energy. The released energy is emitted in the form of fluorescence, and finally the sensor in the ultraviolet fluorescence detection equipment detects the fluorescence intensity, and then quantifies the residual amount of organic residues on the surface of the product to be tested. Since the migration energy of inorganic residues (most of the inorganic residues are inorganic silicon pollutants) is greater than that of organic residues, its fluorescence effect is weak, that is, it is difficult for inorganic residues to release fluorescence after absorbing ultraviolet light, and it is difficult to measure by ultraviolet fluorescence detection equipment. The present application modifies a conjugated structure molecule with a strong fluorescence effect on a silane coupling agent to form a conjugated molecule modified silane coupling agent, and the conjugated molecule modified silane coupling agent can react and combine with the inorganic residues on the surface of the product to be tested, so that the inorganic residues have a fluorescence effect, so that the total fluorescence intensity measured includes the fluorescence intensity of organic pollutants and inorganic pollutants. By comparing the total fluorescence intensity with the preset maximum fluorescence intensity value, it can be determined whether the residual amount of the surface residue of the product to be tested is qualified.

[0022] In some embodiments, the material of the product to be tested is metal, and the inorganic pollutant includes inorganic silicon.

[0023] In some embodiments, the composition of the modified silane coupling agent solution includes, by weight: 3 to 25 parts of conjugated molecule modified silane coupling agent; 60 to 80 parts of organic solvent; 5 to 15 parts of inorganic solvent.

[0024] In some embodiments, the amount of the conjugated molecule modified silane coupling agent can be 3 parts, 6 parts, 10 parts, 15 parts, 20 parts, 25 parts or any value within the range formed by any two of the above values, the amount of the organic solvent can be 60 parts, 65 parts, 70 parts, 75 parts, 80 parts or any value within the range formed by any two of the above values, and the amount of the inorganic solvent can be 5 parts, 8 parts, 10 parts, 13 parts, 15 parts or any value within the range formed by any two of the above values. The conjugated molecule modified silane coupling agent and the organic solvent and the inorganic solvent are prepared into a solution in the above ratio. On the one hand, it is conducive to its dispersion on the surface of the product to be tested, so that the conjugated molecule modified silane coupling agent is fully combined with the inorganic residue on the surface of the product to be tested. On the other hand, the appropriate amount of the conjugated molecule modified silane coupling agent can improve the accuracy of the detection, so that the content of inorganic pollutants can be more accurately calibrated.

[0025] In some embodiments, the structural formula of the conjugated molecule modified silane coupling agent is: , Wherein, X1, X2, X3 are each independently one of methoxy, ethoxy, propoxy, isopropoxy, hydroxyl, chlorine or bromine, and Y is one of vinyl, propenyl, butenyl, butadienyl, phenyl, phenol, benzyl or anthracene. X1, X2, X3 are hydrolyzable groups, which can cause hydrolysis reaction when encountering moisture adsorbed on the surface of inorganic substances, have good reactivity with the surface of inorganic substances, and can be combined with inorganic substances. Y is a conjugated molecular group, which has a fluorescent effect and can be detected by ultraviolet fluorescence equipment. That is, with the silicon atom of the conjugated molecule modified silane coupling agent as the center, the group at one end of the silicon atom can be combined with inorganic residues, and the group at the other end of the silicon atom has a fluorescent effect. After ultraviolet light irradiation, its fluorescence intensity can be detected by ultraviolet fluorescence detection equipment, thereby realizing the calibration and quantification of inorganic residues.

[0026] In some embodiments, X1, X2 and X3 are preferably groups with good volatility, such as methoxy and chlorine, and Y is preferably a group with high fluorescence intensity, such as benzene, butadiene, anthracene, phenol, etc.

[0027] In some embodiments, preferably at least one of X1, X2, and X3 is a methoxy group, and Y is a butadienyl group. The methoxy group has a small molecular weight, a low degree of polymerization, and is easy to volatilize, which can reduce detection errors. The butadienyl group has a strong fluorescence effect, and can clearly calibrate a small amount of inorganic silicon residues, which can improve the accuracy of detection.

[0028] In some embodiments, the organic solvent includes one or more of methanol, ethanol, propanol, isopropanol or acetic acid, and the inorganic solvent can be deionized water. The types of organic solvent and inorganic solvent are matched in the above manner, on the one hand, the conjugated molecule modified silane coupling agent can be well dissolved, and on the other hand, the modified silane coupling agent solution prepared by the combination of the three has good fluidity, can be dispersed on the surface of the product to be tested, and has good volatility under relatively low temperature heating conditions, so as to improve the accuracy of detection.

[0029] In some embodiments, the heating temperature is 40°C to 80°C, and the heating time is 2 min to 15 min. For example, the heating temperature can be 40°C, 50°C, 60°C, 70°C, 80°C or any value within the range formed by any two of the above values, and the heating time is 2 min, 4 min, 6 min, 8 min, 10 min, 12 min, 14 min, 15 min or any value within the range formed by any two of the above values. After the modified silane coupling agent solution is dispersed on the surface of the product to be tested, the product to be tested is heated, so that the modified silane coupling agent solution that is not combined with the inorganic residue can be volatilized, thereby reducing the measurement error. The heating temperature and time are within the above range, so that the excess modified silane coupling agent solution can be fully volatilized, thereby improving the accuracy of the detection.

[0030] In some embodiments, before “dispersing the modified silane coupling agent solution on the surface of the product to be tested”, the method further includes: placing the product to be tested in an ultraviolet fluorescence detection device to detect the fluorescence intensity of organic pollutants on the surface of the product to be tested; The quantified fluorescence intensity corresponding to the inorganic pollutants in the surface residues of the product to be tested is the difference between the total fluorescence intensity and the fluorescence intensity of the organic pollutants. The present application can quickly detect the residual amount of inorganic pollutants on the surface of the product to be tested in this way.

[0031] In some embodiments, multiple products with residues on their surfaces are obtained, and the total fluorescence intensity of each product is measured; a tape is covered on the surface of each product, and the pull-out force P of each tape is measured, and a standard curve equation between the pull-out force P and the total fluorescence intensity of each product is established, and a standard curve equation between the pull-out force P of the tape and the total fluorescence intensity of each product is obtained by data fitting.

[0032] In some embodiments, the maximum fluorescence intensity value is determined according to the set minimum pull-out force and the standard curve equation. If the total fluorescence intensity is less than or equal to the maximum fluorescence intensity value, the residual amount of the surface residue of the product to be tested is judged to be qualified; if the total fluorescence intensity is higher than the maximum fluorescence intensity value, the residual amount of the surface residue of the product to be tested is judged to be unqualified.

[0033] The present application is described in detail below through specific embodiments.

[0034] Example S1: Taking a product as an example, the product is first placed in an ultraviolet fluorescence detection device to measure the first fluorescence intensity F1 corresponding to the organic matter in the residue on its surface; S2: Take 15 parts of a conjugated molecule modified silane coupling agent in which X1, X2, and X3 are all methoxy groups and Y is a butadiene group, 70 parts of ethanol, and 10 parts of deionized water to prepare a modified silane coupling agent solution, then disperse the modified silane coupling agent solution on the surface of the product, and heat the product at 60° C. for 10 minutes; S3: Send the product to the ultraviolet fluorescence detection device again to measure the second fluorescence intensity F2; S4: Calculate the quantitative fluorescence intensity F corresponding to inorganic silicon si , F si is F2-F1; S5: Apply tape to the area to be masked on the product and measure the pull-out force of the tape.

[0035] Take 12 products with residues on the surface and measure them in the same way as above. The first fluorescence intensity F1, the second fluorescence intensity F2, and the quantitative fluorescence intensity F corresponding to the inorganic silicon of each product are measured. siAnd the pull-out force of the tape is recorded in Table 1.

[0036] Table 1 As shown in Table 1, by measuring the first fluorescence intensity F1 and the second fluorescence intensity F2, the quantized fluorescence intensity F corresponding to the inorganic silicon can be obtained. si The second fluorescence intensity F2 in Table 1 is linearly fitted with the data of the pulling force to obtain the following: Figure 2 The linear curve and standard curve equation shown are P = -0.0262 F2 + 5.838. Figure 2 It can be seen that the second fluorescence intensity F2 is inversely proportional to the pulling force of the tape. The maximum value of the second fluorescence intensity F2 can be obtained according to the minimum pulling force specified in the process to determine whether the second fluorescence intensity F2 of the product to be tested is less than or equal to the maximum value. If so, it is determined that the residual amount of the surface residue of the product to be tested meets the requirements.

[0037] For example, the minimum pull-out force of the tape specified in the process is 2.2kgf. Figure 2 The linear curve shown shows that the second fluorescence intensity on the surface of the product to be tested must be less than or equal to 139RFU. This forms a quantitative standard. If the second fluorescence intensity on the surface of the product to be tested is greater than 139 RFU, it means that there are too many residues on the surface of the product to be tested, resulting in insufficient pull-out force of the tape, which in turn affects the masking ability of the tape to the masking area, which will lead to problems such as poor liquid seepage in the masking area. In this way, it can be quickly determined whether the residue on the surface of the product to be tested is qualified. If it is unqualified, the product to be tested needs to undergo further surface cleaning to ensure that the pull-out force of the tape subsequently covering its surface meets the requirements, so as to reduce problems such as poor liquid seepage in the masking area.

[0038] The above implementation modes are only used to illustrate the technical solutions of the present application and are not intended to limit the present application. Although the present application is described in detail with reference to the above implementation modes, a person skilled in the art should understand that the technical solutions of the present application may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present application.

Claims

1. A method for detecting surface residues, used to detect organic pollutants and inorganic pollutants on the surface of a product to be tested, characterized in that: include: Dispersing a modified silane coupling agent solution on the surface of the product to be tested, and heating the product to be tested; Placing the product to be tested in an ultraviolet fluorescence detection device to detect and obtain the total fluorescence intensity of the product to be tested; The total fluorescence intensity is compared with a preset maximum fluorescence intensity value to determine whether the residual amount of the surface residue of the product to be tested is qualified.

2. The method for detecting surface residues according to claim 1, characterized in that: In parts by weight, the composition of the modified silane coupling agent solution includes: 3 to 25 parts of conjugated molecule modified silane coupling agent; 60 to 80 parts of organic solvent; 5 to 15 parts of inorganic solvent.

3. The method for detecting surface residues as claimed in claim 2, characterized in that: The structural formula of the conjugated molecule modified silane coupling agent is: ， Wherein, X1, X2, X3 are each independently one of methoxy, ethoxy, propoxy, isopropoxy, hydroxyl, chlorine or bromine, and Y is one of vinyl, propenyl, butenyl, butadienyl, phenyl, phenol, benzyl or anthracenyl.

4. The method for detecting surface residues as claimed in claim 3, characterized in that: At least one of X1, X2, and X3 is a methoxy group, and Y is a butadienyl group.

5. The method for detecting surface residues according to claim 2, characterized in that: The organic solvent includes one or more of methanol, ethanol, propanol, isopropanol or acetic acid.

6. The method for detecting surface residues according to claim 1, characterized in that: The heating temperature is 40°C to 80°C, and the heating time is 2min to 15min.

7. The method for detecting surface residues according to claim 1, characterized in that: Before the step of "dispersing the modified silane coupling agent solution on the surface of the product to be tested", the method further includes: placing the product to be tested in an ultraviolet fluorescence detection device to detect the fluorescence intensity of the organic pollutants on the surface of the product to be tested; After the step of "placing the product to be tested in an ultraviolet fluorescence detection device to detect the total fluorescence intensity of the product to be tested", the method also includes: in the surface residue of the product to be tested, the quantified fluorescence intensity corresponding to the inorganic pollutant is the difference between the total fluorescence intensity and the fluorescence intensity of the organic pollutant.

8. The method for detecting surface residues according to claim 7, characterized in that: The material of the product to be tested is metal, and the inorganic pollutants include inorganic silicon.

9. The method for detecting surface residues according to claim 1, characterized in that: include: Acquire multiple products with residues on their surfaces and measure the total fluorescence intensity of each product; cover the surface of each product with a tape, measure the pull-out force P of each tape, establish a standard curve equation between the pull-out force P and the total fluorescence intensity of each product, and obtain a standard curve equation between the pull-out force P of the tape and the total fluorescence intensity of each product through data fitting.

10. The method for detecting surface residues according to claim 9, characterized in that: include: Determining the maximum fluorescence intensity value according to the set minimum pulling force and the standard curve equation; If the total fluorescence intensity is less than or equal to the maximum fluorescence intensity value, the residual amount of the surface residue of the product to be tested is judged to be qualified; if the total fluorescence intensity is higher than the maximum fluorescence intensity value, the residual amount of the surface residue of the product to be tested is judged to be unqualified.

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