Detection methods for surface residues
By reacting a modified silane coupling agent solution with the product surface and combining it with ultraviolet fluorescence detection, the problem of the inability to detect organic and inorganic residues on the product surface in existing technologies has been solved, enabling accurate quantification and quality control of surface residues.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SHENZHENSHI YUZHAN PRECISION TECH CO LTD
- Filing Date
- 2024-12-31
- Publication Date
- 2026-08-04
AI Technical Summary
Existing technologies cannot effectively detect organic and inorganic residues on the surface of products at the production site. In particular, X-ray fluorescence analysis cannot detect inorganic substances, while ultraviolet fluorescence analysis can only detect organic substances.
A modified silane coupling agent solution is dispersed on the surface of the product to be tested, and the total fluorescence intensity is detected by an ultraviolet fluorescence detection device. Combined with the reaction of the conjugated silane coupling agent with inorganic residues, a fluorescent complex is formed, and the fluorescence intensity of organic and inorganic pollutants is quantified.
It enables quantitative detection of organic and inorganic contaminants on product surfaces at the production site, improving the accuracy and efficiency of detection and ensuring product quality compliance.
Smart Images
Figure CN119985411B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of testing, and more particularly to a method for detecting surface residues. Background Technology
[0002] Current technologies for detecting surface cleanliness based on the fluorescence effect include X-ray fluorescence analysis and ultraviolet fluorescence analysis. However, X-ray fluorescence analysis requires X-ray excitation, making it difficult to use in production environments. Ultraviolet fluorescence analysis can only detect organic contaminants on surfaces and cannot detect inorganic substances. Therefore, there is an urgent need to develop a method that can be applied in production environments and can detect both organic and inorganic substances, thereby enabling the detection of residues on product surfaces. Summary of the Invention
[0003] In view of this, this application provides a method for detecting surface residues that can solve the above-mentioned technical problems.
[0004] A method for detecting surface residues, used to detect organic and inorganic contaminants on the surface of a product to be tested, comprising:
[0005] The modified silane coupling agent solution is dispersed on the surface of the product to be tested, and the product to be tested is heated.
[0006] The product to be tested is placed in an ultraviolet fluorescence detection device, and the total fluorescence intensity of the product to be tested is detected.
[0007] The total fluorescence intensity is compared with the preset maximum fluorescence intensity value to determine whether the residual amount of the surface residue of the product under test is qualified.
[0008] In some embodiments, the modified silane coupling agent solution comprises, by weight, the following components:
[0009] 3 to 25 parts of conjugated molecule modified silane coupling agent;
[0010] 60-80 parts organic solvent;
[0011] 5 to 15 parts of inorganic solvent.
[0012] In some embodiments, the structural formula of the conjugated molecule modified silane coupling agent is:
[0013] ,
[0014] Wherein, X1, X2, and X3 are each independently one of methoxy, ethoxy, propoxy, isopropoxy, hydroxy, chlorine, or bromine, and Y is one of vinyl, propenyl, butenyl, butadienyl, phenyl, phenolic, benzyl, or anthracene.
[0015] In some embodiments, at least one of X1, X2, and X3 is a methoxy group, and Y is butadiene.
[0016] In some embodiments, the heating temperature is 40°C to 80°C, and the heating time is 2 min to 15 min.
[0017] In some embodiments, the organic solvent includes one or more of methanol, ethanol, propanol, isopropanol, or acetic acid.
[0018] 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;
[0019] After the step of "placing the product to be tested in an ultraviolet fluorescence detection device and detecting the total fluorescence intensity of the product to be tested", the method further 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.
[0020] In some embodiments, the material of the product to be tested is metal, and the inorganic contaminant includes inorganic silicon.
[0021] In some embodiments, the method includes: acquiring multiple products with residues on their surfaces, measuring the total fluorescence intensity of each product; covering the surface of each product with an adhesive tape, measuring the pull-out force P of each adhesive tape, establishing a standard curve equation between the pull-out force P and the total fluorescence intensity of each product, and obtaining the standard curve equation between the pull-out force P of the adhesive tape and the total fluorescence intensity of each product through data fitting.
[0022] In some implementations, the method includes: determining the maximum fluorescence intensity value based on a 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 determining that the residual amount of surface residue of the product under test is qualified; if the total fluorescence intensity is higher than the maximum fluorescence intensity value, then determining that the residual amount of surface residue of the product under test is unqualified.
[0023] This application uses a modified silane coupling agent solution dispersed on the surface of the product to be tested, so that the modified silane coupling agent solution forms a fluorescent complex with the inorganic residues on the surface of the product to be tested. When performing ultraviolet fluorescence detection, 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 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 the fluorescence detection of surface residues. Attached Figure Description
[0024] Figure 1 This is a schematic flowchart of a method for detecting surface residues provided in one embodiment of this application.
[0025] Figure 2 A fitted graph of the second fluorescence intensity versus pull-out force provided for one embodiment of this application. Detailed Implementation
[0026] The embodiments of this application are described in detail below. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this application, and should not be construed as limiting this application. The reagents and materials described in the following embodiments are all commercially available.
[0027] In the anodic masking process, adhesive tape is typically used to mask the product surface. If the surface of the area to be masked is not thoroughly cleaned, residual contaminants (organic and inorganic residues) will reduce the adhesion of the tape, ultimately leading to poor liquid penetration in the masked area. Therefore, controlling the cleanliness of the product surface is crucial to ensuring process stability and yield.
[0028] Small amounts of organic and inorganic residues remaining on product surfaces due to improper cleaning cannot be visually assessed. Therefore, this application provides a method for effectively detecting organic and inorganic contaminants remaining on product surfaces, enabling quantitative detection of surface residues.
[0029] Specifically, please refer to Figure 1 This application provides a method for detecting surface residues, used to detect organic and inorganic contaminants on the surface of a product to be tested, including:
[0030] The modified silane coupling agent solution is dispersed on the surface of the product to be tested, and the product to be tested is heated.
[0031] The product to be tested is placed in an ultraviolet fluorescence detection device, and the total fluorescence intensity of the surface residue of the product to be tested is detected.
[0032] The total fluorescence intensity is compared with the preset maximum fluorescence intensity value to determine whether the residual amount of surface residue of the product under test is qualified.
[0033] The working principle of the above detection method is as follows: After absorbing ultraviolet light, the organic residues on the surface of the product to be tested are excited by photons, and the electrons in the organic residues reach a higher energy level excited state. However, this high-energy excited state is unstable. When the electrons return to the initial energy level, they release energy. The released energy is emitted in the form of fluorescence. Finally, the sensor in the ultraviolet fluorescence detection device detects the fluorescence intensity, thereby quantifying the residual amount of organic residues on the surface of the product to be tested. Since the migration energy of inorganic residues (most of which are inorganic silicon contaminants) is greater than that of organic residues, their fluorescence effect is weak. That is, it is difficult for inorganic residues to release fluorescence after absorbing ultraviolet light, making it difficult to measure by ultraviolet fluorescence detection equipment. This application modifies a silane coupling agent with a conjugated structure molecule that has a strong fluorescence effect to form a conjugated molecule modified silane coupling agent. The conjugated molecule modified silane coupling agent can react and bind with the inorganic residues on the surface of the product to be tested, giving the inorganic residues a fluorescence effect. Therefore, the measured total fluorescence intensity includes the fluorescence intensity of both organic and inorganic contaminants. 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 under test is qualified.
[0034] In some implementations, the material of the product to be tested is metal, and the inorganic contaminants include inorganic silicon.
[0035] In some embodiments, the modified silane coupling agent solution comprises, by weight, the following components:
[0036] 3 to 25 parts of conjugated molecule modified silane coupling agent;
[0037] 60-80 parts organic solvent;
[0038] 5 to 15 parts of inorganic solvent.
[0039] In some embodiments, the amount of conjugated molecular modified silane coupling agent can be 3 parts, 6 parts, 10 parts, 15 parts, 20 parts, 25 parts, or any value within the range of any two of the above values; the amount of organic solvent can be 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, or any value within the range of any two of the above values; and the amount of inorganic solvent can be 5 parts, 8 parts, 10 parts, 13 parts, 15 parts, or any value within the range of any two of the above values. Preparing a solution of the conjugated molecular modified silane coupling agent with organic and inorganic solvents in the above proportions facilitates its dispersion on the surface of the test product, allowing the conjugated molecular modified silane coupling agent to fully bind with inorganic residues on the surface of the test product. Furthermore, an appropriate amount of conjugated molecular modified silane coupling agent can improve the accuracy of detection, thereby enabling more accurate determination of the content of inorganic contaminants.
[0040] In some embodiments, the structural formula of the conjugated molecule modified silane coupling agent is as follows:
[0041] ,
[0042] In this system, X1, X2, and X3 are each independently one of methoxy, ethoxy, propoxy, isopropoxy, hydroxy, chlorine, or bromine, while Y is one of vinyl, propenyl, butenyl, butadieneyl, phenyl, phenolic, benzoyl, or anthraceneyl groups. X1, X2, and X3 are hydrolyzable groups, capable of hydrolysis upon contact with water adsorbed on inorganic surfaces, exhibiting good reactivity with inorganic surfaces and the ability to bind to them. Y is a conjugated molecular group with a fluorescent effect, detectable by ultraviolet fluorescence equipment. Specifically, with the silicon atom of the conjugated molecule-modified silane coupling agent at its center, the group at one end of the silicon atom can bind to inorganic residues, while the group at the other end exhibits a fluorescent effect. After ultraviolet light irradiation, the fluorescence intensity can be detected using ultraviolet fluorescence detection equipment, thus achieving the standardization and quantification of inorganic residues.
[0043] In some embodiments, X1, X2, and X3 are preferably groups with good volatility, such as methoxy or chlorine, and Y is preferably a group with high fluorescence intensity, such as benzene, butadiene, anthracene, or phenol.
[0044] In some embodiments, it is preferred that at least one of X1, X2, and X3 is methoxy, and Y is butadiene. Methoxy groups have a smaller molecular weight and lower degree of polymerization, making them more volatile and reducing detection errors. Butadiene groups exhibit strong fluorescence, clearly indicating even small amounts of inorganic silicon residues, thus improving detection accuracy.
[0045] 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 combination of organic and inorganic solvents as described above not only effectively dissolves the conjugated molecule modified silane coupling agent, but also ensures that the resulting modified silane coupling agent solution has good fluidity, can be dispersed on the surface of the test product, and exhibits good volatility under relatively low heating conditions, thereby improving the accuracy of detection.
[0046] 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 of any two of the above values, and the heating time can be 2 min, 4 min, 6 min, 8 min, 10 min, 12 min, 14 min, 15 min, or any value within the range of any two of the above values. Heating the test product after the modified silane coupling agent solution is dispersed on the surface of the test product allows the modified silane coupling agent solution that has not bound to inorganic residues to volatilize, reducing measurement error. Heating within the above-mentioned temperature and time range allows excess modified silane coupling agent solution to fully volatilize, improving the accuracy of the detection.
[0047] 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;
[0048] In the surface residues of the product under test, the quantified fluorescence intensity of inorganic pollutants is the difference between the total fluorescence intensity and the fluorescence intensity of organic pollutants. This application enables rapid detection of the residual amount of inorganic pollutants on the surface of the product under test using this method.
[0049] In some embodiments, multiple products with residues on their surfaces are obtained, and the total fluorescence intensity of each product is measured; an adhesive tape is applied to the surface of each product, and the pull-out force P of each tape is measured. A standard curve equation is established between the pull-out force P and the total fluorescence intensity of each product, and the 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.
[0050] In some implementations, the maximum fluorescence intensity value is determined based on a set minimum pull-out force and a standard curve equation. If the total fluorescence intensity is less than or equal to the maximum fluorescence intensity value, the residual amount of surface residue on the test product is deemed acceptable; if the total fluorescence intensity is higher than the maximum fluorescence intensity value, the residual amount of surface residue on the test product is deemed unacceptable.
[0051] The present application will be specifically described below through specific embodiments.
[0052] Example
[0053] S1: Taking a product as an example, first place the product in the ultraviolet fluorescence detection setting and measure the first fluorescence intensity F1 corresponding to the organic matter in the residue on its surface;
[0054] S2: Take 15 parts of a methoxy-based and butadiene-based conjugated silane coupling agent (X1, X2, and X3 are all methoxy groups, Y is 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.
[0055] S3: Send the product back into the ultraviolet fluorescence detection equipment and measure the second fluorescence intensity F2;
[0056] S4: Calculate the quantized fluorescence intensity F corresponding to inorganic silicon. si F si For F2-F1;
[0057] S5: Apply tape to the area of the product to be covered and measure the pull-out force of the tape.
[0058] Twelve products with residues on their surfaces were taken and measured in the same manner as described above. The first fluorescence intensity F1, the second fluorescence intensity F2, and the quantized fluorescence intensity F corresponding to inorganic silicon were measured for each product. si The pull-out force of the tape is recorded in Table 1.
[0059] Table 1
[0060]
[0061] 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 inorganic silicon can be obtained. si By performing a linear fit between the second fluorescence intensity F2 in Table 1 and the pull-out force data, the following results were obtained: Figure 2 The linear curve and standard curve equation shown are P = -0.0262 F² + 5.838. (From...) Figure 2 It can be seen that the second fluorescence intensity F2 is inversely proportional to the pull-out force of the tape. The maximum value of the second fluorescence intensity F2 can be obtained according to the minimum pull-out force specified in the process. It can then be determined 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 surface residue of the product to be tested meets the requirements.
[0062] For example, if the process specifies a minimum pull-out force of 2.2 kgf for the tape, then according to... Figure 2The linear curve shown indicates that the second fluorescence intensity on the surface of the test product must be less than or equal to 139 RFU. This forms a quantitative standard. If the second fluorescence intensity on the surface of the test product is greater than 139 RFU, it indicates excessive residue on the surface of the test product, resulting in insufficient pull-out force of the tape, which in turn affects the tape's ability to cover the masked area, leading to problems such as poor liquid seepage in the masked area. This allows for a quick determination of whether the residue on the surface of the test product is acceptable. If it is unacceptable, the test product needs further surface cleaning to ensure that the pull-out force of the tape subsequently applied to its surface meets the requirements, thereby reducing problems such as poor liquid seepage in the masked area.
[0063] The above embodiments are only used to illustrate the technical solutions of this application and are not intended to limit it. Although this application has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions to the technical solutions of this application should not depart from the spirit and scope of the technical solutions of this application.
Claims
1. A method for detecting surface residues, used to detect organic and inorganic silicon contaminants on the surface of a product to be tested, characterized in that, include: The modified silane coupling agent solution is dispersed on the surface of the product to be tested, and the product to be tested is heated. The modified silane coupling agent solution includes a conjugated molecule modified silane coupling agent, and the structural formula of the conjugated molecule modified silane coupling agent is as follows: ， Wherein, X1, X2, and X3 are each independently one of methoxy, propoxy, isopropoxy, hydroxy, chlorine, or bromine, and at least one of X1, X2, and X3 is methoxy, and Y is butadienyl. The product to be tested is placed in an ultraviolet fluorescence detection device, and the total fluorescence intensity of the product to be tested is detected. The total fluorescence intensity is compared with the preset maximum fluorescence intensity value to determine whether the residual amount of the surface residue of the product under test is qualified.
2. The method for detecting surface residues as described in claim 1, characterized in that, The modified silane coupling agent solution comprises, by weight, the following components: 3 to 25 parts of conjugated molecule modified silane coupling agent; 60-80 parts organic solvent; 5 to 15 parts of inorganic solvent.
3. The method for detecting surface residues as described in claim 2, characterized in that, The organic solvent includes one or more of methanol, ethanol, propanol, isopropanol, or acetic acid.
4. The method for detecting surface residues as described in claim 1, characterized in that, The heating temperature is 40℃~80℃, and the heating time is 2min~15min.
5. The method for detecting surface residues as described in 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 and detecting the total fluorescence intensity of the product to be tested", the method further 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.
6. The method for detecting surface residues as described in claim 5, characterized in that, The material of the product to be tested is metal, and the inorganic pollutants include inorganic silicon.
7. The method for detecting surface residues as described in claim 1, characterized in that, include: Multiple products containing residues on their surfaces are obtained, and the total fluorescence intensity of each product is measured. Adhesive tape is applied to the surface of each product, and the pull-out force P of each tape is measured. A standard curve equation is established between the pull-out force P and the total fluorescence intensity of each product. The 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.
8. The method for detecting surface residues as described in claim 7, characterized in that, include: The maximum fluorescence intensity value is determined 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 highest fluorescence intensity value, the residual amount of surface residue of the product under test is deemed to be qualified; if the total fluorescence intensity is higher than the highest fluorescence intensity value, the residual amount of surface residue of the product under test is deemed to be unqualified.