Detection method for evaluating high-temperature structural stability of quartz crucible

Abstract

A detection method for evaluating the high-temperature structural stability of a quartz crucible comprises the steps of experimental sampling, experimental detection and result judgment, performance indexes of the high-temperature structural stability of the position of a sample block of the quartz crucible at a crystal pulling high temperature are obtained through the hardness, density and transparent layer thickness of the sample block, and the method is used for detecting the quartz crucible to ensure the stable product quality and improve the quality of the quartz crucible. According to the method, whether the high-temperature structural stability is sufficient or not can be determined before the crucible is used, so that the abnormality of the crucible in use is reduced, the product stability is improved, the abnormality of a customer during crystal pulling is reduced, and the customer satisfaction is greatly improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high-temperature structure stability testing methods for quartz crucibles used for drawing single crystal silicon rods, and particularly relates to a detection method for evaluating the high-temperature structure stability of a quartz crucible. BACKGROUND

[0002] The high-temperature structure stability of a quartz crucible is one of the core factors that determine the success or failure of a single crystal drawing process and the quality of the final crystal. In crystal drawing, there are quite high requirements for the high-temperature structure stability of a quartz crucible. In the pursuit of higher efficiency, larger size, and higher quality of single crystal silicon production processes, the drawing time of single crystal is getting longer and longer, and the high-temperature section time in the drawing process is also getting longer and longer, which requires higher high-temperature structure stability of the quartz crucible. It is directly related to the safety, stability, yield, and economic benefits of production. If the high-temperature structure stability of the quartz crucible is low, it is easy to cause bulging, deformation, and edge collapse during crystal drawing, which may affect the qualified rate of crystal drawing, contaminate the heat shield, and even cause silicon leakage, damage the heat field, and even cause safety accidents.

[0003] Currently, the high-temperature structure stability of a quartz crucible is mainly evaluated by high-temperature viscosity measurement. The high-temperature viscosity detection method of a quartz crucible is to randomly select one quartz crucible sample from each batch of quartz crucibles, cut it to a specified size, and prepare it for 8 hours according to the requirements. The sample preparation process must be strictly operated, and the sample size must be accurately measured, otherwise the detection result will be affected. Then, the prepared sample is sent to a special detection unit for queuing and detection. The detection fee is 5,000 yuan per sample, and the result is obtained at least 4 days later. High-temperature viscosity detection is a process of collecting data and calculating viscosity during high-temperature heating of the sample. The higher the viscosity, the better the high-temperature structure stability in theory.

[0004] High-temperature viscosity measurement is expensive and has a long detection period, which delays the speed of leaving the factory and further causes customers to complain about the long waiting time. SUMMARY

[0005] In view of this, the present application provides a detection method for evaluating the high-temperature structure stability of a quartz crucible, which can quickly and efficiently complete the factory detection of the high-temperature structure stability of a quartz crucible.

[0006] A detection method for evaluating the high-temperature structure stability of a quartz crucible, comprising the following steps:

[0007] Experimental sampling: randomly selecting one quartz crucible sample from each batch of quartz crucibles, obtaining a sample block from the quartz crucible sample, and the thickness of the sample block being the thickness of the corresponding position of the crucible; cutting the sample block into three groups of equal-sized detection sample blocks, and the thickness of each group of detection sample blocks being the thickness of the corresponding position of the crucible;

[0008] Experimental detection: the hardness of the first group of test samples is detected, and the hardness value of the sample is obtained;

[0009] The density of the second group of test samples is tested, and the density value of the sample is obtained;

[0010] The transparent layer thickness of the third group of test samples is tested, and the transparent layer thickness value of the sample is obtained;

[0011] Result determination: the sample hardness value, sample density value and sample transparent layer thickness value measured by the test sample are brought into the following formula to calculate the Y value of the sample, and the obtained Y value is taken as the performance index for evaluating the high temperature structural stability of the quartz crucible;

[0012] X= (sample hardness value / 520) * sample density value * (sample transparent layer thickness value / 25)

[0013] Y=2.9X 2 -172X+3031

[0014] Wherein, X is the relationship coefficient between the sample hardness value, the sample density value and the sample transparent layer thickness value; Y is the performance index for evaluating the high temperature structural stability of the quartz crucible.

[0015] Preferably, when the sample is obtained from one position of the quartz crucible sample, a Y value is obtained by bringing the formula into calculation, and the Y value is the performance index for evaluating the high temperature structural stability of the quartz crucible sample;

[0016] When the sample is obtained from two or more positions of the quartz crucible sample, two or more Y values are obtained by bringing the formula into calculation, the size of the obtained Y values is compared, and the smallest Y value is taken as the performance index for evaluating the high temperature structural stability of the quartz crucible sample.

[0017] Preferably, in the experimental sampling step, at least one sample is obtained from the straight wall of the quartz crucible sample, at least one sample is obtained from the R corner of the quartz crucible sample, and at least one sample is obtained from the bottom of the quartz crucible sample.

[0018] Preferably, in the experimental sampling step, the pattern center of the sample on the outer surface of the straight wall of the quartz crucible sample coincides with the center of the developed rectangle of the outer surface of the straight wall;

[0019] The center of the pattern of the sample on the outer surface of the R corner of the quartz crucible sample coincides with the midpoint of the circular arc formed by the outer surface of the R corner;

[0020] The center of the pattern of the sample on the outer surface of the bottom of the quartz crucible sample coincides with the center of the outer surface of the bottom.

[0021] Preferably, in the experimental sampling step,

[0022] The pattern of the straight wall position sample block of the quartz crucible sample on the outer surface of the straight wall is a square with a length of 50 mm and a width of 50 mm; that is, the straight wall position sample block of the quartz crucible sample has a length of 50 mm, a width of 50 mm, and a thickness equal to the thickness of the corresponding position of the crucible;

[0023] The straight wall position sample block of the quartz crucible sample is cut into three equal groups of detection sample blocks, and the pattern of each straight wall position detection sample block of the quartz crucible sample on the outer surface of the straight wall is a square with a length of 10 mm and a width of 10 mm; that is, the straight wall position detection sample block of the quartz crucible sample has a length of 10 mm, a width of 10 mm, and a thickness equal to the thickness of the corresponding position of the crucible;

[0024] The pattern of the R-angle position sample block of the quartz crucible sample on the outer surface of the R-angle is a square with a length of 50 mm and a width of 50 mm; that is, the R-angle position sample block of the quartz crucible sample has a length of 50 mm, a width of 50 mm, and a thickness equal to the thickness of the corresponding position of the crucible;

[0025] The R-angle position sample block of the quartz crucible sample is cut into three equal groups of detection sample blocks, and the pattern of each R-angle position detection sample block of the quartz crucible sample on the outer surface of the straight wall is a square with a length of 10 mm and a width of 10 mm; that is, the R-angle position detection sample block of the quartz crucible sample has a length of 10 mm, a width of 10 mm, and a thickness equal to the thickness of the corresponding position of the crucible;

[0026] The pattern of the bottom position sample block of the quartz crucible sample on the outer surface of the bottom is a square with a length of 50 mm and a width of 50 mm; that is, the bottom position sample block of the quartz crucible sample has a length of 50 mm, a width of 50 mm, and a thickness equal to the thickness of the corresponding position of the crucible;

[0027] The bottom position sample block of the quartz crucible sample is cut into three equal groups of detection sample blocks, and the pattern of each bottom position detection sample block of the quartz crucible sample on the outer surface of the straight wall is a square with a length of 10 mm and a width of 10 mm; that is, the bottom position detection sample block of the quartz crucible sample has a length of 10 mm, a width of 10 mm, and a thickness equal to the thickness of the corresponding position of the crucible.

[0028] Preferably, in the experimental detection step, a hardness tester is used to detect the hardness of the first group of detection sample blocks to obtain a sample hardness value; a drainage method is used to test the density of the second group of detection sample blocks to obtain a sample density value; and a transparent layer tester is used to test the thickness of the transparent layer of the third group of detection sample blocks to obtain a sample transparent layer thickness value.

[0029] A detection method for evaluating the high-temperature structural stability of a quartz crucible, comprising the following steps:

[0030] Experimental sampling: in the production process of each batch of quartz crucible or in the experimental process, at least one sample is randomly taken from the edge material in the production process of the batch of quartz crucible, one side of the sample in the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible; the sample is cut into three groups of detection samples of equal size, and the thickness of each group of detection samples is the thickness of the corresponding position of the crucible;

[0031] Experimental detection: the hardness of the first group of detection samples is detected to obtain the sample hardness value;

[0032] The second group of detection samples is tested for density to obtain the sample density value;

[0033] The third group of detection samples is tested for transparent layer thickness to obtain the sample transparent layer thickness value;

[0034] Result determination: the sample hardness value, sample density value and sample transparent layer thickness value measured by the detection sample are brought into the following formula to calculate the Y value of the sample, and the obtained Y value is taken as the performance index for evaluating the high-temperature structural stability of the quartz crucible in the sampling time period in the production process or the experimental process;

[0035] X = (sample hardness value / 520) * sample density value * (sample transparent layer thickness value / 25) Y = 2.9X 2 -172X + 3031

[0036] Wherein, X is the relationship coefficient between the sample hardness value, the sample density value and the sample transparent layer thickness value; Y is the performance index for evaluating the high-temperature structural stability of the quartz crucible.

[0037] Preferably, in the experimental sampling step: the sample is 50 mm long, 50 mm wide, one side of the sample in the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible; the sample is cut into three groups of detection samples of equal size, and each group of detection samples is 10 mm long, 10 mm wide, one side of the detection sample in the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.

[0038] Preferably, in the experimental detection step, a hardness tester is used to detect the hardness of the first group of detection samples to obtain the sample hardness value; a drainage method is used to test the density of the second group of detection samples to obtain the sample density value; a transparent layer tester is used to test the transparent layer thickness of the third group of detection samples to obtain the sample transparent layer thickness value.

[0039] Preferably, the above-mentioned quartz crucible is a quartz crucible for drawing a single crystal silicon rod.

[0040] The method for evaluating the high-temperature structural stability of quartz crucibles described in this invention models long-term production data, experimental research data, and customer feedback data. The model shows that the hardness, density, and thickness of the transparent layer of the quartz crucible are significant controlling factors affecting high-temperature structural stability. Based on this, the intrinsic relationship between these three parameters and their mapping relationship with the performance indicators of the high-temperature structural stability of the quartz crucible are analyzed. Finally, a method for predicting the high-temperature structural stability of quartz crucibles using hardness, density, and transparent layer thickness as inputs is obtained. In subsequent production processes, combined with mechanical sensing, data analysis, and feedback data verification, it is proven that the method for predicting the high-temperature structural stability of quartz crucibles described in this invention can accurately predict the high-temperature structural stability of quartz crucibles, with short testing time, high accuracy, high reliability, and low cost.

[0041] The detection method for evaluating the high-temperature structural stability of quartz crucibles described in this invention can be applied to the factory inspection of the high-temperature structural stability of finished quartz crucibles. Using this method to test quartz crucibles ensures stable product quality. It can confirm whether the high-temperature structural stability is sufficient before the crucible is used, reducing abnormalities that occur during use. This not only improves product stability and reduces abnormalities during crystal pulling, but also significantly improves customer satisfaction.

[0042] The detection method for evaluating the high-temperature structural stability of quartz crucibles described in this invention can also be applied to the detection of high-temperature structural stability during the production or experimental process of quartz crucibles. During the production or experimental process of quartz crucibles, the high-temperature structural stability can be confirmed using the scrap material, which effectively helps to determine the effect of process development and process improvement. It can more comprehensively evaluate newly developed products, shorten experimental time, reduce experimental costs, and provide a basis for continuous improvement. Attached Figure Description

[0043] Appendix Figure 1 A schematic diagram of one embodiment of sampling blocks for quartz crucible samples.

[0044] Appendix Figure 2 This is a schematic diagram of one implementation of a sampling block on a side view of a quartz crucible sample.

[0045] Appendix Figure 3 This is a schematic diagram of one implementation method for taking a sampling block from the bottom front view of a quartz crucible sample.

[0046] In the figure: 1. Quartz crucible sample; 2. Bottom of quartz crucible sample; 3. Radius of quartz crucible sample; 4. Straight wall of quartz crucible sample; 5. Sampling position at the bottom of quartz crucible sample; 6. Sampling position at the radius of quartz crucible sample; 7. Sampling position at the straight wall of quartz crucible sample. Detailed Implementation

[0047] Example 1

[0048] A detection method for evaluating high-temperature structural stability of a quartz crucible, comprising the following steps:

[0049] (1) Experimental sampling: one quartz crucible sample 1 is randomly selected from each batch of quartz crucibles, two sample blocks are obtained from the straight wall 4 of the quartz crucible sample, two sample blocks are obtained from the R corner 3 of the quartz crucible sample, and two sample blocks are obtained from the bottom 2 of the quartz crucible sample. The thickness of the sample block is the thickness of the corresponding position of the crucible; each sample block is cut into three groups of equal-sized detection sample blocks, and the thickness of each group of detection sample blocks is the thickness of the corresponding position of the crucible.

[0050] Specifically, the centers of the patterns on the two adjacent sample blocks at the straight wall position of the quartz crucible sample on the outer surface of the straight wall coincide with the center of the developed rectangle of the outer surface of the straight wall. The pattern of the two sample blocks at the straight wall 4 position of the quartz crucible sample on the outer surface of the straight wall is a rectangle with a length of 100 mm and a width of 50 mm; that is, the two sample blocks at the straight wall 4 position of the quartz crucible sample have a length of 100 mm, a width of 50 mm, and a thickness that is the thickness of the corresponding position of the crucible, that is, each sample block at the straight wall position of the quartz crucible sample has a length of 50 mm, a width of 50 mm, and a thickness that is the thickness of the corresponding position of the crucible, one side of the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible. Each sample block at the straight wall position of the quartz crucible sample is cut into three groups of equal-sized detection sample blocks, and the pattern of each detection sample block at the straight wall position of the quartz crucible sample on the outer surface of the straight wall is a square with a length of 10 mm and a width of 10 mm; that is, the detection sample block at the straight wall position of the quartz crucible sample has a length of 10 mm, a width of 10 mm, and a thickness that is the thickness of the corresponding position of the crucible, one side of the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.

[0051] The centers of the patterns on the two adjacent sample blocks at the R corner position of the quartz crucible sample on the outer surface of the R corner coincide with the midpoint of the circular arc formed by the outer surface of the R corner. The pattern of the two sample blocks at the R corner position of the quartz crucible sample on the outer surface of the R corner is a rectangle with a length of 100 mm and a width of 50 mm; that is, the two sample blocks at the R corner position of the quartz crucible sample have a length of 100 mm, a width of 50 mm, and a thickness that is the thickness of the corresponding position of the crucible, that is, each sample block at the R corner position of the quartz crucible sample has a length of 50 mm, a width of 50 mm, and a thickness that is the thickness of the corresponding position of the crucible, one side of the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible. Each sample block at the R corner position of the quartz crucible sample is cut into three groups of equal-sized detection sample blocks, and the pattern of each detection sample block at the R corner position of the quartz crucible sample on the outer surface of the R corner is a square with a length of 10 mm and a width of 10 mm; that is, the detection sample block at the R corner position of the quartz crucible sample has a length of 10 mm, a width of 10 mm, and a thickness that is the thickness of the corresponding position of the crucible, one side of the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.

[0052] The pattern of the two adjacent sample blocks at the bottom position of the quartz crucible sample on the outer surface of the bottom is a rectangle with a length of 100 mm and a width of 50 mm; that is, the two sample blocks at the bottom position of the quartz crucible sample have a length of 100 mm, a width of 50 mm and a thickness of the thickness of the corresponding position of the crucible; that is, each sample block at the bottom position of the quartz crucible sample has a length of 50 mm, a width of 50 mm and a thickness of the thickness of the corresponding position of the crucible, one side of the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible. Each sample block at the bottom position of the quartz crucible sample is cut into three groups of detection sample blocks with equal size, and the pattern of each detection sample block at the bottom position of the quartz crucible sample on the outer surface of the bottom is a square with a length of 10 mm and a width of 10 mm; that is, the detection sample block at the bottom position of the quartz crucible sample has a length of 10 mm, a width of 10 mm and a thickness of the thickness of the corresponding position of the crucible, one side of the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.

[0053] (2) Experimental detection: the hardness of the first group of detection sample blocks is detected by using a hardness tester to obtain the hardness value of the sample blocks; the hardness values of the two adjacent sample blocks at the straight wall position of the quartz crucible sample are 314.6 and 316.9 respectively; the hardness values of the two adjacent sample blocks at the R corner position of the quartz crucible sample are 289.5 and 287.8 respectively; and the hardness values of the two adjacent sample blocks at the bottom position of the quartz crucible sample are 320.4 and 321.7 respectively.

[0054] The density of the second group of detection sample blocks is tested by using the drainage method to obtain the density value of the sample blocks; the density values of the two adjacent sample blocks at the straight wall position of the quartz crucible sample are 2.49 and 2.43 respectively; the density values of the two adjacent sample blocks at the R corner position of the quartz crucible sample are 2.39 and 2.34 respectively; and the density values of the two adjacent sample blocks at the bottom position of the quartz crucible sample are 2.40 and 2.43 respectively.

[0055] The transparent layer thickness of the third group of detection sample blocks is tested by using a transparent layer tester to obtain the transparent layer thickness value of the sample blocks. The transparent layer thicknesses of the two adjacent sample blocks at the straight wall position of the quartz crucible sample are 7 and 6 respectively; the transparent layer thicknesses of the two adjacent sample blocks at the R corner position of the quartz crucible sample are 3 and 4 respectively; and the transparent layer thicknesses of the two adjacent sample blocks at the bottom position of the quartz crucible sample are 4 and 5 respectively.

[0056] (3) Result determination: first, the sample block hardness value, sample block density value and sample block transparent layer thickness value measured by the three groups of detection sample blocks divided from one sample block are used to calculate the Y value of the sample block by using the following formula one and formula two.

[0057] Formula one: X = (sample block hardness value / 520) * sample block density value * (sample block transparent layer thickness value / 25)

[0058] Formula two: Y = 2.9X 2 -172X + 3031

[0059] Wherein, X is the relationship coefficient between the sample block hardness value, the sample block density value, and the sample block transparent layer thickness value; Y is the performance index for evaluating the high-temperature structural stability of the quartz crucible.

[0060] Then, the six Y values obtained by bringing the sample blocks obtained from the six positions of the quartz crucible sample 1 into the formula are compared, and the smallest Y value is taken as the performance index for evaluating the high-temperature structural stability of the quartz crucible sample 1.

[0061] The above data is brought into the formula, and Y is calculated, and the results are shown in the following table.

[0062] Serial number Hardness value Density value Transparent layer thickness Y 1 314.6 2.49 7 2958.96 2 316.9 2.43 6 2970.23 3 289.5 2.39 3 3003.61 4 287.8 2.34 4 2995.48 5 320.4 2.40 4 2990.47 6 321.7 2.43 5 2979.55

[0063] It can be seen that the smallest Y value of the six positions of the quartz crucible sample is 2958.96, that is, the performance index for the high-temperature structural stability of the sample block at one of the positions of the straight wall of the quartz crucible is the lowest, and the performance index for the high-temperature structural stability of the quartz crucible in this batch is 2958.96.

[0064] The high-temperature structural stability of the quartz crucible is one of the core factors that determine the success or failure of the single crystal pulling process and the final crystal quality. The quality of the quartz crucible in the same batch is very small, so a random sample can reflect the quality of the quartz crucible in the same batch. Because the quartz crucible is a whole, in the high-temperature crystal pulling process, the weakest place, that is, the place with the lowest Y value, is prone to bulging, deformation, and edge collapse. Therefore, multiple sampling is required at the straight wall of the quartz crucible, the R angle of the quartz crucible, and the bottom of the quartz crucible to determine the high-temperature structural stability. After a large amount of detection data, it is found that a straight line formed at the center of the slowly expanding rectangle on the outer surface of the straight wall of the quartz crucible is a position with a higher probability of low high-temperature structural stability of the straight wall of the quartz crucible, a straight line formed at the midpoint of the circular arc on the outer surface of the R angle of the quartz crucible is a position with a higher probability of low high-temperature structural stability of the R angle of the quartz crucible, and the center of the outer surface of the bottom 2 of the quartz crucible sample is a position with a higher probability of low high-temperature structural stability of the bottom of the quartz crucible. Therefore, sampling at the positions with a higher probability of low high-temperature structural stability of the quartz crucible can reflect the high-temperature structural stability of the quartz crucible in this batch.

[0065] Example 2

[0066] A detection method for evaluating the high-temperature structural stability of a quartz crucible, comprising the following steps:

[0067] (1) Experimental sampling: randomly select one quartz crucible sample 1 from each batch of quartz crucibles, obtain a sample block from the weakest position of the quartz crucible sample 1, the sample block is 50 mm long, 50 mm wide, and the thickness is the thickness of the corresponding position of the crucible, that is, one side of the thickness direction of the sample block is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible; cut the sample block into three groups of detection sample blocks of equal size, and each group of detection sample blocks is 10 mm long, 10 mm wide, and the thickness is the thickness of the corresponding position of the crucible, one side of the thickness direction of the detection sample block is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.

[0068] (2) Experimental detection: use a hardness tester to detect the hardness of the first group of detection sample blocks, and obtain a sample block hardness value of 290.5; use the drainage method to test the density of the second group of detection sample blocks, and obtain a sample block density value of 2.39; use a transparent layer tester to test the transparent layer thickness of the third group of detection sample blocks, and obtain a sample block transparent layer thickness value of 5.

[0069] (3) Result determination: first, the sample block hardness value, sample block density value, and sample block transparent layer thickness value measured by the detection sample block are brought into the following formula one and formula two to calculate the Y value of the sample block, and the obtained Y value is taken as the performance index for evaluating the high-temperature structural stability of the sampling time period of the quartz crucible in the production process or experimental process.

[0070] Formula one: X = (sample block hardness value / 520) * sample block density value * (sample block transparent layer thickness value / 25)

[0071] Formula two: Y = 2.9X 2 -172X + 3031

[0072] Wherein, X is the relationship coefficient between the sample block hardness value, the sample block density value, and the sample block transparent layer thickness value; Y is the performance index for evaluating the high-temperature structural stability of the quartz crucible.

[0073] After the numerical value is brought in, the obtained Y value is 2985.28, and the Y value is the performance index for evaluating the high-temperature structural stability of the quartz crucible sample 1 of this batch.

[0074] After a long time of data accumulation, it can be compared that the quartz crucible sample straight wall 4, the quartz crucible sample R angle 3, and the quartz crucible sample bottom 2 have poor high-temperature structural stability, that is, the Y value is the lowest, that is, the weakest position of the quartz crucible, which is prone to bulging, deformation, and edge collapse. Therefore, the sampling quantity can be reduced, and sampling is performed at the position with the highest probability of low high-temperature structural stability of the quartz crucible, and the Y value of the corresponding position is detected, which can reflect the high-temperature structural stability of the quartz crucible of this batch.

[0075] The detection method for evaluating the high-temperature structural stability of the quartz crucible provided by the application is modeling the production data, experimental research data and customer feedback data accumulated by the company over a long period of time. The model shows that the hardness, density and transparent layer thickness of the quartz crucible are significant control factors affecting the high-temperature structural stability. On this basis, the internal correlation between the three parameters and the mapping relationship between the three parameters and the performance indicators of the high-temperature structural stability of the quartz crucible are analyzed. Finally, the above formula one and formula two are obtained. The Y value is obtained by inputting the hardness value, density value and transparent layer thickness value into the above formula one and formula two. The high-temperature structural stability of the quartz crucible is predicted by the Y value. At the same time, in the later production process, combined with mechanical sensing, data analysis and feedback data verification, it is proved that the detection method for predicting the high-temperature structural stability of the quartz crucible can accurately predict the high-temperature structural stability of the quartz crucible, has short detection time, high accuracy, strong reliability and low cost.

[0076] The above embodiment 1 and embodiment 2 can be applied to the factory detection of the high-temperature structural stability of the finished quartz crucible. The use of this method for detecting the quartz crucible ensures the stable product quality and can confirm whether the high-temperature structural stability is sufficient before the crucible is used, thereby reducing the abnormality of the crucible in use, improving the product stability and reducing the abnormality of the customer during crystal pulling, and greatly improving the customer satisfaction.

[0077] Embodiment 3

[0078] A detection method for evaluating the high-temperature structural stability of a quartz crucible, comprising the following steps:

[0079] (1) Experimental sampling: during the production process or experimental process of each batch of quartz crucibles, at least one edge material in the production process of the batch of quartz crucibles is randomly taken as a sample block, one side of the sample block in the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible; the sample block is cut into three groups of detection sample blocks with equal size, and the thickness of each group of detection sample blocks is the thickness of the corresponding position of the crucible, that is, one side of the detection sample block in the thickness direction is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.

[0080] (2) In the experimental detection step, a hardness tester is used to detect the hardness of the first group of detection sample blocks, and the hardness value of the sample block is 325.6; a drainage method is used to test the density of the second group of detection sample blocks, and the density value of the sample block is 2.43; a transparent layer tester is used to test the transparent layer thickness of the third group of detection sample blocks, and the transparent layer thickness value of the sample block is 6.

[0081] (3) The sample block hardness value, sample block density value, sample block transparent layer thickness value measured by the detection sample block are brought into the following formula one, formula two to calculate the Y value of the sample block as 2968.58, and the obtained Y value is the performance index for evaluating the high-temperature structural stability of the quartz crucible in the sampling time period in the production process or experimental process;

[0082] Formula one: X=(sample block hardness value / 520)*sample block density value*(sample block transparent layer thickness value / 25) Formula two: Y=2.9X 2 -172X+3031

[0083] Wherein, X is the relationship coefficient among the sample block hardness value, sample block density value and sample block transparent layer thickness value; Y is the performance index for evaluating the high-temperature structural stability of the quartz crucible.

[0084] After a period of practice, it is found that the detection method for evaluating the high-temperature structural stability of the quartz crucible as described in Example 3 can be applied to the detection of the high-temperature structural stability in the production process or experimental process of the quartz crucible. In the production process or experimental process of the quartz crucible, the side material can be used to confirm whether the high-temperature structural stability is sufficient, the process can be adjusted according to the result, the effect of process development and process improvement can be effectively helped to determine, the newly developed product can be more comprehensively evaluated, the experimental time can be shortened, the experimental cost can be reduced, and the basis for continuous improvement and promotion can be provided.

Claims

1. A method for evaluating the high-temperature structural stability of a quartz crucible, characterized in that, Includes the following steps: Experimental sampling: One quartz crucible sample is randomly selected from each batch of quartz crucibles. A sample block is obtained from the quartz crucible sample, and the thickness of the sample block is the thickness of the corresponding position of the crucible. The sample block is cut into three groups of test sample blocks of equal size, and the thickness of each group of test sample blocks is the thickness of the corresponding position of the crucible. Experimental testing: The hardness of the first group of test samples was tested to obtain the hardness values ​​of the samples; The density of the second group of test samples was measured to obtain the sample density values. The thickness of the transparent layer of the third group of test samples was measured to obtain the thickness value of the transparent layer of the sample. Result determination: The hardness value, density value, and transparent layer thickness value of the test sample obtained by measuring the sample block are substituted into the following formula to calculate the Y value of the sample block. The obtained Y value is used as the performance index for evaluating the high-temperature structural stability of this batch of quartz crucibles. X = (sample hardness value / 520) * sample density value * (sample transparent layer thickness value / 25) Y=2.9X 2 -172X+3031 Where X is the relationship coefficient between the sample hardness value, sample density value, and sample transparent layer thickness value; Y is the performance index for evaluating the high-temperature structural stability of the quartz crucible.

2. The method for evaluating the high-temperature structural stability of a quartz crucible as described in claim 1, characterized in that, When a sample block is taken from a location of a quartz crucible sample, a Y value is obtained by substituting it into the formula. The Y value is a performance index for evaluating the high-temperature structural stability of the quartz crucible sample. When samples are taken from two or more locations of a quartz crucible sample, two or more Y values ​​are calculated by substituting them into the formula. The magnitudes of the obtained Y values ​​are compared, and the smallest Y value is used as the performance index for evaluating the high-temperature structural stability of the quartz crucible sample.

3. The method for evaluating the high-temperature structural stability of a quartz crucible as described in claim 2, characterized in that, In the experimental sampling step, at least one sample block is obtained from the straight wall of the quartz crucible sample, at least one sample block is obtained from the radius (R) of the quartz crucible sample, and at least one sample block is obtained from the bottom of the quartz crucible sample.

4. The method for evaluating the high-temperature structural stability of a quartz crucible as described in claim 3, characterized in that, In the experimental sampling step, the center of the pattern on the outer surface of the straight wall of the quartz crucible sample block coincides with the center of the unfolded rectangle on the outer surface of the straight wall. The center of the pattern on the outer surface of the sample block at the R-angle of the quartz crucible coincides with the midpoint of the arc formed by the outer surface of the R-angle. The center of the pattern on the bottom outer surface of the sample block at the bottom of the quartz crucible coincides with the center of the bottom outer surface.

5. The method for evaluating the high-temperature structural stability of a quartz crucible as described in claim 4, characterized in that, In the experimental sampling steps: The pattern on the outer surface of the straight wall of the quartz crucible sample is a square with a length of 50 mm and a width of 50 mm; that is, the straight wall of the quartz crucible sample has a length of 50 mm, a width of 50 mm, and a thickness equal to the thickness of the corresponding position of the crucible. The quartz crucible sample at the straight wall position is cut into three sets of equally sized test blocks. The pattern on the outer surface of the straight wall of each quartz crucible sample at the straight wall position is a square with a length of 10 mm and a width of 10 mm; that is, the quartz crucible sample at the straight wall position is 10 mm long, 10 mm wide, and the thickness is the thickness of the corresponding position of the crucible. The pattern on the outer surface of the sample block at the R-corner of the quartz crucible sample is a square with a length of 50 mm and a width of 50 mm; that is, the sample block at the R-corner of the quartz crucible sample is 50 mm long, 50 mm wide, and has a thickness equal to the thickness of the corresponding position of the crucible. The quartz crucible sample R-corner position sample block is cut into three sets of equally sized test samples. The pattern on the outer surface of the straight wall of each quartz crucible sample R-corner position test sample block is a square with a length of 10 mm and a width of 10 mm; that is, the quartz crucible sample R-corner position test sample block is 10 mm long, 10 mm wide, and the thickness is the thickness of the corresponding position of the crucible. The pattern on the outer surface of the bottom sample block of the quartz crucible sample is a square with a length of 50 mm and a width of 50 mm; that is, the bottom sample block of the quartz crucible sample is 50 mm long, 50 mm wide, and has a thickness equal to the thickness of the corresponding position of the crucible. The bottom sample block of the quartz crucible is cut into three sets of equally sized test blocks. The pattern on the outer surface of the straight wall of each test block is a square with a length of 10 mm and a width of 10 mm; that is, the bottom sample block of the quartz crucible is 10 mm long, 10 mm wide, and has a thickness equal to the thickness of the corresponding position of the crucible.

6. The method for evaluating the high-temperature structural stability of a quartz crucible as described in claim 1, characterized in that, In the experimental testing steps, a hardness tester is used to test the hardness of the first group of test samples to obtain the sample hardness value; the water displacement method is used to test the density of the second group of test samples to obtain the sample density value; and a transparency layer tester is used to test the transparency layer thickness of the third group of test samples to obtain the sample transparency layer thickness value.

7. A method for evaluating the high-temperature structural stability of a quartz crucible, characterized in that, Includes the following steps: Experimental sampling: During the production or experiment of each batch of quartz crucibles, at least one piece of scrap material from the production process of that batch of quartz crucibles is randomly selected to obtain a sample block. One side of the sample block is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible. The sample block is cut into three groups of test sample blocks of equal size, and the thickness of each group of test sample blocks is the thickness of the corresponding position of the crucible. Experimental testing: The hardness of the first group of test samples was tested to obtain the hardness values ​​of the samples; The density of the second group of test samples was measured to obtain the sample density values. The thickness of the transparent layer of the third group of test samples was measured to obtain the thickness value of the transparent layer of the sample. Result determination: The hardness value, density value, and transparent layer thickness value of the sample block obtained by measurement are substituted into the following formula to calculate the Y value of the sample block. The obtained Y value is used as the performance index for evaluating the high-temperature structural stability of the quartz crucible during the sampling period in the production process or experiment. X = (Sample hardness value / 520) * Sample density value * (Sample transparent layer thickness value / 25) Y = 2.9X 2 -172X+3031 Where X is the relationship coefficient between the sample hardness value, sample density value, and sample transparent layer thickness value; Y is the performance index for evaluating the high-temperature structural stability of the quartz crucible.

8. The method for evaluating the high-temperature structural stability of a quartz crucible as described in claim 7, characterized in that, In the experimental sampling steps: the sample block is 50 mm long and 50 mm wide, with one side of the sample block in the thickness direction being the inner wall of the crucible and the other side being the outer wall of the quartz crucible; the sample block is cut into three groups of test sample blocks of equal size, with each group of test sample blocks being 10 mm long and 10 mm wide, with one side of the test sample block in the thickness direction being the inner wall of the crucible and the other side being the outer wall of the quartz crucible.

9. The method for evaluating the high-temperature structural stability of a quartz crucible as described in claim 7, characterized in that, In the experimental testing steps, a hardness tester is used to test the hardness of the first group of test samples to obtain the sample hardness value; the water displacement method is used to test the density of the second group of test samples to obtain the sample density value; and a transparency layer tester is used to test the transparency layer thickness of the third group of test samples to obtain the sample transparency layer thickness value.

10. The method for evaluating the high-temperature structural stability of a quartz crucible as described in any one of claims 1-9, characterized in that, The quartz crucible is a quartz crucible used for pulling single-crystal silicon rods.

Images