Test methods for evaluating the high-temperature structural stability of quartz crucibles
Patent Information
- Application Number
- CN202511775237.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-28
- Publication Date
- 2026-09-01
- Estimated Expiration
- 2045-11-28
AI Technical Summary
[0004]高温粘度测量费用高且估检测周期长,耽误出厂速度,进而导致客户抱怨等待时间过长
Smart Images

Figure CN121521201B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the technical field of high-temperature structural stability testing methods for quartz crucibles used in pulling single-crystal silicon rods, and particularly to a testing method for evaluating the high-temperature structural stability of quartz crucibles. Background Technology
[0002] The high-temperature structural stability of the quartz crucible is one of the core factors determining the success or failure of the single crystal pulling process and the final crystal quality. The high-temperature structural stability of the quartz crucible is extremely important in crystal pulling. In the pursuit of higher efficiency, larger sizes, and higher quality single-crystal silicon production, the pulling time and the duration of the high-temperature section during pulling are becoming increasingly longer, placing higher demands on the high-temperature structural stability of the quartz crucible. This directly affects the safety, stability, yield, and economic benefits of production. If the high-temperature structural stability of the quartz crucible is low, bulging, deformation, and edge collapse are likely to occur during crystal pulling. This can range from affecting the yield rate and contaminating the heat shield, resulting in silicon material waste, to more serious issues such as silicon leakage, damage to the thermal field, and even safety accidents.
[0003] Currently, the industry mainly evaluates the high-temperature structural stability of quartz crucibles using high-temperature viscosity measurement. The high-temperature viscosity testing method for quartz crucibles involves randomly selecting one quartz crucible sample from each batch, cutting it to a specified size, and preparing the sample for 8 hours as required. The sample preparation process must be strictly controlled, and the sample size must be accurately measured, otherwise it will affect the test results. Then, the prepared sample is sent to a specialized testing unit to queue for testing. The testing fee is 5,000 yuan per sample, and the results are available in at least 4 days. High-temperature viscosity testing involves collecting data and calculating the viscosity during the process of heating the sample to an extremely high temperature. The higher the viscosity, theoretically the better the high-temperature structural stability.
[0004] High-temperature viscosity measurement is expensive and has a long testing cycle, which delays the delivery speed and leads to customer complaints about long waiting times. Summary of the Invention
[0005] In view of this, the present invention proposes a testing method for evaluating the high-temperature structural stability of quartz crucibles, which can quickly and efficiently complete the factory testing of the high-temperature structural stability of quartz crucibles.
[0006] A method for evaluating the high-temperature structural stability of a quartz crucible includes the following steps:
[0007] 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.
[0008] Experimental testing: The hardness of the first group of test samples was tested to obtain the hardness values of the samples;
[0009] The density of the second group of test samples was measured to obtain the sample density values.
[0010] 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.
[0011] 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.
[0012] X = (sample hardness value / 520) * sample density value * (sample transparent layer thickness value / 25)
[0013] Y=2.9X 2 -172X+3031
[0014] 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.
[0015] Preferably, when a sample block is obtained from a location of the quartz crucible sample, a Y value is calculated by substituting it into the formula. The Y value is then used as a performance index to evaluate the high-temperature structural stability of the quartz crucible sample.
[0016] 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.
[0017] Preferably, 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.
[0018] Preferably, in the experimental sampling step, the center of the pattern on the outer surface of the quartz crucible sample block at the straight wall position coincides with the center of the unfolded rectangle on the outer surface of the straight wall;
[0019] 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.
[0020] 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.
[0021] Preferably, in the experimental sampling step:
[0022] 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.
[0023] 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.
[0024] 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.
[0025] 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.
[0026] 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.
[0027] 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.
[0028] Preferably, 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; a 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.
[0029] A method for evaluating the high-temperature structural stability of a quartz crucible includes the following steps:
[0030] 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.
[0031] Experimental testing: The hardness of the first group of test samples was tested to obtain the hardness values of the samples;
[0032] The density of the second group of test samples was measured to obtain the sample density values.
[0033] 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.
[0034] 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.
[0035] X = (Sample hardness value / 520) * Sample density value * (Sample transparent layer thickness value / 25) Y = 2.9X 2 -172X+3031
[0036] 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.
[0037] Preferably, in the experimental sampling step: 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.
[0038] Preferably, 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; a 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.
[0039] Preferably, the quartz crucible described above is a quartz crucible used for pulling single-crystal silicon rods.
[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 method for evaluating the high-temperature structural stability of a quartz crucible includes the following steps:
[0049] (1) Experimental sampling: One quartz crucible sample 1 was randomly selected from each batch of quartz crucibles. Two sample blocks were obtained from the straight wall 4 of the quartz crucible sample, two sample blocks were obtained from the R-angle 3 of the quartz crucible sample, and two sample blocks were obtained from the bottom 2 of the quartz crucible sample. The thickness of the sample block was the thickness of the corresponding position of the crucible. Each sample block was cut into three groups of test sample blocks of equal size, and the thickness of each group of test sample blocks was the thickness of the corresponding position of the crucible.
[0050] Specifically, the center of the pattern on the outer surface of the straight wall of the quartz crucible sample for two adjacent sample blocks at the straight wall position coincides with the center of the unfolded rectangle on the outer surface of the straight wall. The pattern on the outer surface of the two sample blocks at the straight wall position 4 of the quartz crucible sample 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 position 4 of the quartz crucible sample are 100 mm long and 50 mm wide, and the thickness is the thickness of the corresponding position of the crucible. In other words, each sample block at the straight wall position of the quartz crucible sample is 50 mm long and 50 mm wide, and the thickness 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 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 and 10 mm wide, and the thickness 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 center of the pattern on the outer surface of two adjacent sample blocks at the radius (R) of the quartz crucible sample coincides with the midpoint of the arc formed by the outer surface of the radius. The pattern on the outer surface of the two sample blocks at the radius of the quartz crucible sample is a rectangle with a length of 100 mm and a width of 50 mm; that is, the two sample blocks at the radius of the quartz crucible sample are 100 mm long and 50 mm wide, and the thickness is the thickness of the corresponding position of the crucible. In other words, each sample block at the radius of the quartz crucible sample is 50 mm long and 50 mm wide, and the thickness 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 quartz crucible sample at its R-corner position is cut into three sets of equally sized test blocks. The pattern on the outer surface of the R-corner test block of each quartz crucible sample is a square with a length of 10 mm and a width of 10 mm. That is, the quartz crucible sample at its R-corner position is 10 mm long and 10 mm wide, and its thickness 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 center of the pattern on the outer surface of the bottom of two adjacent sample blocks at the bottom of the quartz crucible sample coincides with the center of the outer surface of the bottom. The pattern on the outer surface of the bottom of the two sample blocks at the bottom of the quartz crucible sample is a rectangle with a length of 100 mm and a width of 50 mm; that is, the two sample blocks at the bottom of the quartz crucible sample are 100 mm long and 50 mm wide, with a thickness equal to the thickness of the corresponding position of the crucible. Each sample block at the bottom of the quartz crucible sample is 50 mm long and 50 mm wide, with a thickness equal to 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 of the quartz crucible sample is cut into three sets of equally sized test sample blocks. The pattern on the outer surface of the bottom of each test sample block at the bottom of the quartz crucible sample is a square with a length of 10 mm and a width of 10 mm; that is, the test sample block at the bottom of the quartz crucible sample is 10 mm long and 10 mm wide, with a thickness equal to 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 testing: The first group of test samples were tested using a hardness tester to obtain the hardness values of the samples; the hardness values of two adjacent samples at the straight wall position of the quartz crucible sample were 314.6 and 316.9, respectively; the hardness values of two adjacent samples at the R-corner position of the quartz crucible sample were 289.5 and 287.8, respectively; the hardness values of two adjacent samples at the bottom position of the quartz crucible sample were 320.4 and 321.7, respectively.
[0054] The density of the second group of test samples was tested using the water displacement method, and the density values of the samples were obtained. The density values of two adjacent samples at the straight wall position of the quartz crucible sample were 2.49 and 2.43, respectively; the density values of two adjacent samples at the R-corner position of the quartz crucible sample were 2.39 and 2.34, respectively; and the density values of two adjacent samples at the bottom position of the quartz crucible sample were 2.40 and 2.43, respectively.
[0055] The transparency layer thickness of the third group of test samples was measured using a transparency layer tester, and the transparency layer thickness values were obtained. The transparency layer thicknesses of two adjacent samples at the straight wall position of the quartz crucible sample were 7 and 6, respectively; the transparency layer thicknesses of two adjacent samples at the radius (R) position of the quartz crucible sample were 3 and 4, respectively; and the transparency layer thicknesses of two adjacent samples at the bottom position of the quartz crucible sample were 4 and 5, respectively.
[0056] (3) Result determination: First, the sample block is divided into three groups of test samples, and the sample block hardness value, sample block density value, and sample block transparent layer thickness value are measured respectively. The Y value of the sample block is calculated using the following formulas 1 and 2.
[0057] Formula 1: X = (sample hardness value / 520) * sample density value * (sample transparent layer thickness value / 25)
[0058] Formula 2: Y = 2.9X 2 -172X+3031
[0059] 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.
[0060] Next, the samples obtained from six locations of the quartz crucible sample 1 were analyzed, and the six Y values obtained were calculated by substituting them into the formula. The magnitudes of the six Y values were compared, and the smallest Y value was used as the performance index for evaluating the high-temperature structural stability of the quartz crucible sample 1.
[0061] Substitute the data above into the formula to calculate Y, and the results are shown in the table below.
[0062] 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 among the six positions of the quartz crucible sample is 2958.96. This means that the high-temperature structural stability performance index of one of the sample blocks at the straight wall position of the quartz crucible sample is the lowest. In other words, the high-temperature structural stability performance index of this batch of quartz crucibles is 2958.96.
[0064] The high-temperature structural stability of a quartz crucible is one of the core factors determining the success or failure of the single-crystal pulling process and the final crystal quality. The quality of quartz crucibles within the same batch varies very little, so randomly selecting a sample can reflect the overall quality of crucibles in the batch. Because a quartz crucible is a single unit, the weakest point during high-temperature crystal pulling, where the Y-value is lowest, is prone to bulging, deformation, and edge collapse. Therefore, multiple samples are taken from three locations: the straight wall, the radius (R-corner), and the bottom of the quartz crucible, to determine its high-temperature structural stability. Extensive testing revealed that a straight line formed by the center of the slowly unfolding rectangle on the outer surface of the straight wall is a location with a high probability of low high-temperature structural stability on the straight wall; a straight line formed by the midpoint of the arc formed on the outer surface of the radius (R-corner) is a location with a high probability of low high-temperature structural stability at the radius; and the center of the outer surface of the bottom of the quartz crucible is a location with a high probability of low high-temperature structural stability at the bottom. Therefore, by taking samples at locations where the high-temperature structural stability of the quartz crucible is relatively low, and detecting the corresponding Y value at those locations, the high-temperature structural stability of this batch of quartz crucibles can be reflected.
[0065] Example 2
[0066] A method for evaluating the high-temperature structural stability of a quartz crucible includes the following steps:
[0067] (1) Experimental sampling: One quartz crucible sample 1 is randomly selected from each batch of quartz crucibles. A sample block is obtained from the weakest position of quartz crucible sample 1. The sample block is 50 mm long and 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. The sample block is cut into three groups of test sample blocks of equal size. Each group of test sample blocks is 10 mm long and 10 mm wide, and the thickness is the thickness of the corresponding position of the crucible. One side of the thickness direction of the test sample block is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.
[0068] (2) Experimental testing: The first group of test samples were tested for hardness using a hardness tester, and the hardness value of the sample was 290.5; the second group of test samples were tested for density using the water displacement method, and the density value of the sample was 2.39; the third group of test samples were tested for transparent layer thickness using a transparent layer tester, and the transparent layer thickness value of the sample was 5.
[0069] (3) Result determination: First, the hardness value, density value and transparent layer thickness value of the sample block obtained by measuring the sample block are substituted into Formula 1 and Formula 2 below 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.
[0070] Formula 1: X = (sample hardness value / 520) * sample density value * (sample transparent layer thickness value / 25)
[0071] Formula 2: Y = 2.9X 2 -172X+3031
[0072] 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.
[0073] After substituting the numerical values, the obtained Y value is 2985.28. The Y value is a performance index for evaluating the high-temperature structural stability of quartz crucible sample 1 in this batch.
[0074] After accumulating data over a long period, it can be determined which part of the quartz crucible sample has poor high-temperature structural stability (i.e., the lowest Y value), which is the weakest point of the quartz crucible and is prone to bulging, deformation, and edge collapse. Therefore, the number of samples can be reduced, and samples can be taken at the location with the highest probability of low high-temperature structural stability of the quartz crucible. The Y value at the corresponding location can then reflect the high-temperature structural stability of this batch of quartz crucibles.
[0075] 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 transparent layer thickness 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, ultimately yielding Formula 1 and Formula 2. Using Formula 1 and Formula 2 as inputs, and obtaining the Y value based on hardness, density, and transparent layer thickness, the high-temperature structural stability of the quartz crucible is predicted. Furthermore, 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.
[0076] The above-described Examples 1 and 2 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. Before the crucible is used, it can be confirmed whether the high-temperature structural stability is sufficient, reducing abnormalities that occur during use. This not only improves product stability and reduces abnormalities during crystal pulling, but also significantly improves customer satisfaction.
[0077] Example 3
[0078] A method for evaluating the high-temperature structural stability of a quartz crucible includes the following steps:
[0079] (1) Experimental sampling: During the production process or experiment of each batch of quartz crucibles, at least one piece of the edge material from the production process of the batch of quartz crucibles is randomly selected to obtain a sample block. 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. 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, that is, one side of the thickness direction of the test sample block is the inner wall of the crucible, and the other side is the outer wall of the quartz crucible.
[0080] (2) In the experimental testing steps, the first group of test samples was tested for hardness using a hardness tester, and the hardness value of the sample was 325.6; the second group of test samples was tested for density using the water displacement method, and the density value of the sample was 2.43; the third group of test samples was tested for transparent layer thickness using a transparent layer tester, and the transparent layer thickness value of the sample was 6.
[0081] (3) Substitute the hardness value, density value, and transparent layer thickness value of the sample block obtained by measuring the sample block into Formula 1 and Formula 2 below to calculate the Y value of the sample block, which is 2968.58. 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.
[0082] Formula 1: X = (sample hardness value / 520) * sample density value * (sample transparent layer thickness value / 25) Formula 2: Y = 2.9X 2 -172X+3031
[0083] 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.
[0084] After a period of practice, it was found that the detection method for evaluating the high-temperature structural stability of quartz crucibles as described in Example 3 can 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. Based on this result, the process can be adjusted, which can effectively help determine the process development and process improvement effects. It can also more comprehensively evaluate newly developed products, shorten experimental time, reduce experimental costs, and provide a basis for continuous improvement.
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.
Citation Information
Patent Citations
Long-life quartz crucible capable of improving first rod crystallization rate of monocrystalline silicon
CN116377579A
Quartz sand evaluation method for producing bubble-free quartz crucible and product thereof
CN119354975A