Method for chemical analysis of residual cerium oxide of a glass substrate

Abstract

The embodiment of the application discloses a chemical analysis method for residual cerium oxide of a glass substrate, comprising the following steps: placing the peeled glass substrate into an acidic solution and uniformly covering the surface of the glass substrate, taking out the glass substrate after standing and cleaning the surface of the glass substrate with ultrapure water, pouring the cleaned liquid into the original soaking hydrofluoric acid to form a soaking solution; transferring the soaking solution into a polytetrafluoroethylene digestion tank and placing it on an electric heating furnace for heating and drying, adding concentrated hydrochloric acid for multiple times for dissolving after the liquid is completely dried, and cooling and cleaning after dissolving to configure a solution; formulating a standard solution configuration table for the configured solution, measuring the Ce element concentration C Ce of the to-be-measured solution according to the element detection spectral line condition, and measuring the Ce element concentration C Ce0 of the reagent blank solution, wherein the method is used for pre-treating the glass, and the content of the residual cerium oxide on the surface of the glass substrate is rapidly analyzed after grinding.

Description

TECHNICAL FIELD

[0001] The application relates to a chemical analysis method for residual cerium oxide of a glass substrate and belongs to the technical field of detection. BACKGROUND

[0002] New glass is more and more significant for the development of the glass industry. In recent years, with the vigorous development of the liquid crystal panel industry at home and abroad, domestic liquid crystal panel display technology has also developed rapidly, especially high-generation liquid crystal panel display technology. From the existing liquid crystal panel industry, whether TFT-LCD or OLED, glass substrate is one of the important and key materials required for production and is also a basic component of the liquid crystal panel. However, in the face of the demand for high-generation glass substrates in today's society, it is undoubtedly China-made and the mainstream of the development of future high-generation glass to produce high-generation glass substrates by using the float process, although the process has the characteristics of high production capacity and easy expansion of the size of the substrate glass, but due to the inherent characteristics of the float process, the high-generation substrate glass produced needs to be surface ground and processed, and the most important material needed in this process is cerium oxide. For the production process with relatively high cost, how to improve the yield while reducing glass waste is the most effective way to reduce costs and increase efficiency. After the glass substrate is ground, cerium oxide is left on the surface after grinding, so the current method is to directly dispose of this part of the glass, which is not allowed to be recycled. However, how to quantitatively analyze the influence of the residual cerium oxide on the glass recycling production after the surface grinding of the glass substrate is the key problem to be solved by the application.

[0003] To solve such problems, the application designs a chemical analysis method for residual cerium oxide of a glass substrate. The detection method is simple and has strong operability, can quantitatively analyze the residual cerium oxide on the surface of the glass substrate after grinding, can more accurately evaluate the glass substrate processed by cerium oxide, and has great help for reducing glass waste in the glass substrate production process to achieve the purpose of reducing costs and increasing efficiency. SUMMARY

[0004] In view of the problem that there is no reliable method for analyzing the residual cerium oxide on the surface of the glass substrate after grinding in the current process production, and the problem of cost waste caused by directly disposing of the glass substrate with residual cerium oxide after surface grinding. In order to achieve the above purpose, the application designs a chemical analysis method for residual cerium oxide of a glass substrate. The method is used for pretreatment of glass by using a detection method, and the content of residual cerium oxide on the surface of the glass substrate after grinding is rapidly analyzed by using the method, which can more accurately evaluate the glass substrate processed by cerium oxide, and has great help for reducing glass waste in the glass substrate production process to achieve the purpose of reducing costs and increasing efficiency.

[0005] The present application solves the above technical problems by adopting the technical scheme as follows:

[0006] The present application provides a chemical analysis method for residual cerium oxide of a glass substrate, comprising the following steps:

[0007] S1: sample processing:

[0008] The residual cerium oxide after surface grinding is completely stripped from the glass substrate, the stripped glass substrate is placed in an acidic solution, and the acidic solution uniformly covers the surface of the glass substrate, the glass substrate is taken out after standing, and the surface of the glass substrate is cleaned with ultrapure water, the cleaned liquid is poured into the original soaking hydrofluoric acid to form a soaking solution;

[0009] S2: sample dissolution:

[0010] The soaking solution is transferred into a polytetrafluoroethylene digestion tank and placed on an electric heating furnace for heating and drying, when the liquid is completely dried, concentrated hydrochloric acid is added multiple times for dissolution, and after dissolution, cooling and cleaning are performed to configure a solution;

[0011] S3: residual cerium oxide content analysis:

[0012] The prepared solution is subjected to qualitative scanning, a standard solution configuration table is prepared according to the results of qualitative scanning, element detection spectral line conditions are set for the standard solution configuration table, and the Ce element concentration C Ce of the to-be-tested solution and the Ce element concentration C of the reagent blank solution are measured according to the element detection spectral line conditions. Ce0 .

[0013] Optionally, in some embodiments of the present application, before the glass substrate is completely stripped of cerium oxide, two glass substrates with a size of 100mm*100mm are cut, dried at 105℃, and the initial weights M1 and M2 of the two glass substrates are recorded;

[0014] The dried glass substrates are respectively placed in a square PP disc with a side length of 200mm or a rectangular PP disc with a short side of 200mm.

[0015] Optionally, in some embodiments of the present application, in the S1, after the surface of the glass substrate is cleaned with ultrapure water, the cleaned glass substrate is dried at 105℃, weighed, and the processing weights M3 and M4 are recorded;

[0016] The difference between the initial masses M1 and M2 and the processing masses M3 and M4 is used to evaluate the corrosion mass, and the corrosion masses of the two glass substrates are obtained respectively.

[0017] Optionally, in some embodiments of the present application, in the S1, the acidic solution comprises one of the following: 36.0%-38.0% of concentrated hydrochloric acid, 40% of hydrofluoric acid, and 36.0%-38.0% of hydrochloric acid with a volume ratio of 1:1 of pure water.

[0018] Optionally, in some embodiments of the present application, in the S1, the glass substrate is placed in the acidic solution for 10 minutes.

[0019] Optionally, in some embodiments of the present application, in the S2, the heating temperature of the electric heating furnace ranges from 250°C to 280°C.

[0020] Optionally, in some embodiments of the present application, in the S2, the process of adding concentrated hydrochloric acid comprises:

[0021] When the liquid is completely evaporated, 20mL of concentrated hydrochloric acid is added for the first time, and the liquid is evaporated, and when the liquid is completely evaporated again, 20mL of concentrated hydrochloric acid is added for the second time for complete dissolution;

[0022] The concentration of the concentrated hydrochloric acid is 36%-38%.

[0023] Optionally, in some embodiments of the present application, in the S2, a blank solution is also configured, which does not undergo the cleaning process of the glass substrate in the acidic solution in the S1 and enters the processing process in the S2.

[0024] Optionally, in some embodiments of the present application, in the S3, the qualitative scanning is performed by an element scanning instrument, and the wavelength range of the element scanning instrument is 180nm-800nm.

[0025] Optionally, in some embodiments of the present application, in the S3, the configuration of the standard solution comprises:

[0026] Four 100mL volumetric flasks are provided, which are numbered 1#, 2#, 3#, and 4# respectively, and reagents are added to the four volumetric flasks according to the qualitative scanning results, and 10mL (1:1) of concentrated hydrochloric acid is added respectively, and ultrapure water is added to the calibration line to complete the configuration, and standby is performed.

[0027] Compared with the prior art, the beneficial effects of the present application are:

[0028] This invention presents a chemical analysis method for residual cerium oxide in glass substrates. This method is simple, highly operable, and can quantitatively analyze the residual cerium oxide on the surface of glass substrates after grinding. It can accurately assess the impact of cerium oxide processing on the glass substrates and their reprocessing. This method is of great help in reducing glass waste during the glass substrate production process, thereby achieving the goal of cost reduction and efficiency improvement. Attached Figure Description

[0029] To more clearly illustrate the technical solutions in the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0030] Figure 1 A schematic diagram of the overall process for chemical analysis of residual cerium oxide on a glass substrate provided in this application embodiment. Detailed Implementation

[0031] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this application. It is understood that the accompanying drawings are provided for reference and illustration only, and are not intended to limit this application. The connection relationships shown in the accompanying drawings are only for clear description and do not limit the connection method.

[0032] Specifically, such as Figure 1 As shown in the embodiments of this application, a chemical analysis method for residual cerium oxide in a glass substrate is provided. This chemical analysis method removes cerium oxide by surface treatment of the glass. The specific operation process is as follows:

[0033] S1: Sample processing:

[0034] The cerium oxide residue remaining after surface grinding is completely peeled off from the glass substrate. The peeled glass substrate is placed in an acidic solution, and the acidic solution is evenly covered on the surface of the glass substrate. After standing for a certain period of time, the glass substrate is removed and the surface of the glass substrate is cleaned with ultrapure water. The cleaned liquid is poured into the original soaking hydrofluoric acid to form a soaking solution.

[0035] S2: Sample dissolution:

[0036] The soaking liquid is transferred into a polytetrafluoroethylene digestion tank and placed on an electric heating furnace for drying, and when the liquid is completely dried, concentrated hydrochloric acid is added multiple times for dissolution, and after dissolution, cooling and cleaning are performed to configure a solution;

[0037] S3: residual cerium oxide content analysis:

[0038] The configured solution is subjected to qualitative scanning, a standard solution configuration table is prepared according to the results of the qualitative scanning, element detection spectral line conditions are set for the standard solution configuration table, and the Ce element concentration C of the to-be-measured solution is measured according to the element detection spectral line conditions Ce and the Ce element concentration C Ce0 of the reagent blank solution.

[0039] Specifically:

[0040] 1. Sample processing, i.e., stripping the residual cerium oxide after surface grinding from the glass substrate:

[0041] (1) Accurately cut two glass substrates of 100mm*100mm, dry at 105℃, weigh, and record the initial weight 1# sample m0=11.6998g, 2# sample m0=11.8369g;

[0042] (2) Place the glass substrates in (1) in a square PP dish with a side length of 200mm or a rectangular PP dish with a short side of at least 200mm;

[0043] (3) Accurately add 40mL of hydrofluoric acid to evenly cover the surface of the glass substrate, and after 10 minutes, remove the glass substrate and clean the surface of the glass substrate with ultrapure water, and pour the cleaned liquid into the original soaking hydrofluoric acid;

[0044] (4) Dry the cleaned glass substrate at 105℃, weigh, and record the weight 1# sample m1=11.0035g, 2# sample m1=11.1538g;

[0045] (5) From (1) and (4), the corrosion mass of 1# sample m=0.6963g, and 2# sample m=0.6831g;

[0046] 2. Simulate uniform spraying of cerium oxide powder:

[0047] (1) Add cerium oxide powder to 1# sample and 2# sample of the final corrosion solution in step 1, i.e., add 0.0160g to 1# sample and 0.0154g to 2# sample;

[0048] (2) Convert the added cerium oxide powder to a proportion of 1# sample 2.30%, and 2# sample 2.25%.

[0049] 3. Sample dissolution

[0050] (1) The hydrogen fluoride soaking solution in the PP disc (together with the glass powder corroded off) was transferred into a 200 mL polytetrafluoroethylene digestion tank and placed on an electric heating furnace for heating at 250-280°C for dissolution;

[0051] (2) After 20-30 min, the dissolution in the digestion tank was observed, and after the liquid was completely evaporated, concentrated hydrochloric acid was added twice for dissolution, 20 mL each time, and the second time, the liquid in the digestion tank was completely evaporated before the second concentrated hydrochloric acid was added;

[0052] (3) After complete dissolution, the polytetrafluoroethylene beaker in the digestion tank was removed and cooled, transferred to a 100 mL volumetric flask, and washed with ultrapure water in small amounts multiple times to ensure complete transfer to the volumetric flask;

[0053] (4) The blank solution was prepared according to the same method;

[0054] 4. Analysis of residual cerium oxide content

[0055] (1) The prepared test solution was first qualitatively scanned in the range of 180 nm-800 nm, and the scanning results are shown in Table 1 below:

[0056] Element name to be measured Content / ppm 1#-Ce 23300 2#-Ce 22900

[0057] (2) According to the element composition and semi-quantitative results of the qualitative scanning, a standard solution preparation table was prepared, as shown in Table 2:

[0058]

[0059] The specific configuration requirements are as follows: four 100 mL volumetric flasks were prepared and numbered 1#, 2#, 3#, and 4#, respectively, and the reagents were added in turn according to Table 1, 10 mL of concentrated hydrochloric acid (1:1) was added at the same time, and finally ultrapure water was added to the calibration mark for volume. After configuration, it was ready for use.

[0060] (3) The element detection spectral line and other conditions were set, as shown in Table 3 below:

[0061] Element to be measured Detection spectral line wavelength (nm) Ce 413.38 Ce 413.765 Ce 418.66 Ce 456.236

[0062] (4) Test result processing: the Ce element concentration C Ce of the test solution and the Ce element concentration C Ce0 of the reagent blank solution; using the formula Wce = (C Ce -C Ce0 ) x V / (m x 106 W x 100% wherein, W is the mass percentage content of the element to be detected in the sample, unit %; C Ce C is the Ce element concentration of the solution to be detected, unit μg / mL; C Ce0 C is the Ce element concentration in the reagent blank solution, unit μg / mL; V is the constant volume, unit mL; m is the mass of the sample to be detected, unit g; the final content of the residual cerium oxide after the surface grinding of the glass substrate is calculated and shown in Table 4 below:

[0063] Experiment number Ce content / ppm Converted content / % 1# 23100 2.31％ 2# 22300 2.23％

[0064] (1) The actual detection result is proportional to the added cerium oxide powder, and the maximum error is 0.02%, which proves the reliability of the method of the present application;

[0065] (2) After the determination is completed, the torch flame is first extinguished, the argon valve is closed, and then the power is turned off;

[0066] Through the comparison of the examples and comparative examples and the comparison of comparative example and comparative example 1, the same conclusion is obtained by the method of the present application, which can verify the effectiveness of the present application.

[0067] The above examples are only used to illustrate the technical method of the present application and not to limit it. Although the present application has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical method of the present application can be modified or replaced equivalently without departing from the spirit and scope of the technical method of the present application.

Claims

1. A method for chemical analysis of residual cerium oxide of a glass substrate, characterized by, The method comprises the following steps: S1: sample processing, i.e. completely stripping the cerium oxide remaining after surface grinding from the glass substrate; Two pieces of 100 mm 100 mm glass substrates were dried at 105 °C and the initial weights m0of both glass substrates were recorded; The dried glass substrate is placed in a square PP dish with a side length of 200 mm or a rectangular PP dish with a short side of 200 mm; The glass substrate is placed in a hydrofluoric acid solution which uniformly covers the surface of the glass substrate for etching and stripping, and after standing, the glass substrate is taken out and the surface of the glass substrate is cleaned with ultrapure water, and the cleaned liquid is poured into the original hydrofluoric acid solution to form a soaking solution; After the surface of the glass substrate is cleaned with ultrapure water, the cleaned glass substrate is dried at 105°C, weighed, and the weight m1 is recorded; According to the initial mass m o The corrosion mass is evaluated according to the initial mass m and the weight m1, and the corrosion mass m of the two glass substrates is obtained respectively. S2 Sample dissolution: The soaking solution is transferred to a polytetrafluoroethylene digestion tank and placed on an electric heating furnace for heating and drying, and after the liquid is completely dried, concentrated hydrochloric acid is added multiple times for dissolution, and after dissolution, cooling and cleaning are performed to prepare a solution; A blank solution is also prepared, which does not undergo the cleaning process of the glass substrate with the hydrofluoric acid solution in S1 and enters the processing process in S2. S3: residual cerium oxide content analysis: Qualitative scanning is performed on the prepared solution, a standard solution preparation table is formulated according to the result of the qualitative scanning, element detection spectral line conditions are set for the standard solution preparation table, and the Ce element concentration C of the solution to be measured is measured according to the element detection spectral line conditions Ce and the Ce element concentration C of the blank solution Ce0 ; The content of the residual cerium oxide after polishing the surface of the final glass substrate was calculated by the formula Wce = (C Ce -C Ce0 ) x V / (m x 10 6 x 100%) where V is the constant volume in mL.

2. The method of claim 1, wherein the glass substrate contains cerium oxide. In S1, the standing time of the glass substrate in the hydrofluoric acid solution is 10 minutes.

3. The method of claim 1, wherein the glass substrate contains cerium oxide. In S2, the heating temperature of the electric heating furnace ranges from 250°C to 280°C.

4. The method of claim 1, wherein the glass substrate contains residual cerium oxide. In S2, the concentrated hydrochloric acid addition process includes: After the liquid is completely evaporated, 20 mL of concentrated hydrochloric acid is added for the first time, and the liquid is evaporated, and after the liquid is completely evaporated again, 20 mL of concentrated hydrochloric acid is added for the second time for complete dissolution. The concentration of the concentrated hydrochloric acid is 36%-38%.

5. The method of claim 1, wherein the glass substrate contains residual cerium oxide. In S3, the qualitative scanning is performed by an element scanner, and the wavelength range of the element scanner is 180 nm-800 nm.

6. The method of claim 1, wherein the glass substrate contains residual cerium oxide. In S3, the preparation of the standard solution includes: Four 100 mL volumetric flasks are provided and numbered 1#, 2#, 3#, and 4#, respectively, and reagents are added to the four volumetric flasks according to the qualitative scanning results, 10 mL of concentrated hydrochloric acid is added to each, and ultrapure water is added to the calibration line to complete the preparation, and it is ready for use.

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