Rapid detection method for alpha-alumina conversion rate of calcined alumina
The conversion rate of α-alumina in calcined alumina can be quickly and accurately detected using an X-ray detector and a standard curve model, solving the problems of long time consumption and unstable results of traditional methods, and realizing efficient and reliable conversion rate detection.
Patent Information
- Application Number
- CN202511237488.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-01
- Publication Date
- 2025-11-25
AI Technical Summary
Traditional detection methods for α-alumina conversion are time-consuming, damage samples, and produce unstable and poorly reproducible results, with some results showing a conversion rate greater than 100%.
The conversion rate of α-alumina in calcined alumina was rapidly detected using an X-ray detector. A standard curve was constructed, and the peak areas of the sample at three specific angles were detected using an X-ray diffractometer. A mathematical model was then established to calculate the conversion rate.
A rapid, accurate, and stable method for detecting α-alumina conversion rate was achieved. The detection results are representative, have good reproducibility, and avoid the shortcomings of traditional methods.
Smart Images
Figure CN121007918A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of detection, and relates to a rapid detection method for a-alumina conversion rate of calcined alumina. BACKGROUND
[0002] The calcined alumina is an alumina product formed by treating aluminum hydroxide or industrial alumina at a high temperature of 1200-1700 DEG C. The main chemical components are a-type and gamma-type alumina variants, wherein the a-type has a hexagonal close-packed lattice structure, and the melting point reaches 2050 DEG C, which is a core raw material for smelting of aluminum. The a-Al2O3 (corundum phase) conversion rate refers to the content (volume %) of a-alumina in all alumina contained in the alumina particles, and the conversion rate is a key index for evaluating the quality of the calcined alumina.
[0003] Traditional detection methods such as chemical method and thermogravimetric method have defects such as long time consumption, sample destruction and large error; and the a conversion rate is usually determined by a conventional XRD method, that is, the alumina particles are determined by a powder X-ray diffraction method, the peak height (I25.6) of the a phase (012 plane) appearing at 2 theta = 25.6 DEG and the peak height (I46) of the gamma phase, eta phase, chi phase, kappa phase, theta phase and delta phase appearing at 2 theta = 46 DEG are calculated from the obtained diffraction spectrum, and the a conversion rate is calculated by the following formula (1). a conversion rate = I25.6 / (I25.6+I46) x 100 (%).
[0004] The detection result of this method is unstable, the result reproducibility is poor, the two peaks are not representative, and part of the results will appear the phenomenon that the conversion rate is greater than 100%.
[0005] Therefore, a method capable of rapidly and accurately detecting the a-alumina conversion rate is urgently needed. SUMMARY
[0006] The application provides a rapid detection method for a-alumina conversion rate of calcined alumina, and the a-alumina conversion rate of the calcined alumina is rapidly and accurately detected based on an X-ray detector.
[0007] The technical scheme for solving the above technical problem is as follows: The application provides a rapid detection method for a-alumina conversion rate of calcined alumina, and the a-alumina conversion rate of the calcined alumina is rapidly and accurately detected based on an X-ray detector. S1, standard curve preparation: pure v-alumina raw material is ground to a particle size of 10-50 um, sieved, and the undersize is taken; 100% a-alumina conversion rate sample is ground to a particle size of 10-50 um, sieved, and the undersize is taken; the undersize is taken, and 50%-100% conversion rate gradient standard substances are prepared to obtain standard samples for standby; S2. Sample preparation: Grind the sample to be tested to a particle size of 10um-50um, sieve it, take the sieve blank, press it into a sample mold to obtain a sample sheet; S3. Sample installation: Install the standard sample obtained in step S1 and the sample sheet obtained in step S2 onto the X-ray diffractometer equipment respectively. S4. On-machine testing; S5. Data Processing: The test results of the above standard samples are used to create a standard curve. The sum of the peak areas of the three peaks of the sample is substituted into the standard curve to obtain the conversion rate.
[0008] In step S1, the conversion rate gradient can be configured according to actual conditions, as long as the test sample results are within the curve range. For example, the conversion rate of α-alumina can be 80%, 90%, or 100%.
[0009] More preferably, in step S4, the machine conditions are: scanning mode step scan.
[0010] More preferably, in step S4, the angle increment is 0.0020.
[0011] More preferably, in step S4, the sampling time is 0.3s.
[0012] More preferably, in step S4, the scanning angle is: 2θ: 24.8-26.2°, θ: 12.4°; 2θ: 42.5-44.5°, θ: 21.3°; 2θ: 56.6-58.3°, θ: 28.3°.
[0013] More preferably, in step S5, the sum of the three peaks of the test results of the above standard sample is used to create a standard curve.
[0014] More preferably, the formula for the standard curve is: y=ax+b Where y is the sum of the areas of the three peaks; a is the slope; b is the intersection of the curve and the y-axis; and x is the conversion rate corresponding to the peak area.
[0015] A further preferred method is to substitute the sum of the peak areas of the three peaks of the sample into the curve to obtain the conversion rate.
[0016] The beneficial effects of this invention are as follows: The detection method of this invention, by configuring different conversion rate gradients, calculates the conversion rate by establishing a mathematical model of the relationship between the peak area of the three peaks and the conversion rate. The detection method is simple, rapid, accurate, and stable, and can well reflect the conversion rate of the material. The three peaks of the detection method of this invention are more representative, the detection results are stable, and the results have good reproducibility. Attached Figure Description
[0017] Figure 1 This is the standard curve diagram of the present invention.
[0018] Figure 2 This is the diffraction pattern of sample B32-batch number 20250402 of this invention. in, Figure 2 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 2 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 2 (c) is the diffraction pattern of the sample at 2θ=57°.
[0019] Figure 3 This is the diffraction pattern of sample A11-batch number 20250512 of this invention. in, Figure 3 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 3 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 3 (c) is the diffraction pattern of the sample at 2θ=57°.
[0020] Figure 4 The diffraction pattern of sample B03-batch number 20250516 of this invention is shown. in, Figure 4 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 4 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 4 (c) is the diffraction pattern of the sample at 2θ=57°.
[0021] Figure 5 The diffraction patterns are those of parallel samples of the dry powder of this invention, batch number 20250214. in, Figure 5 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 5 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 5 (c) is the diffraction pattern of the sample at 2θ=57°.
[0022] Figure 6 The diffraction pattern of sample B31-batch number 20250417 of this invention. in, Figure 6 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 6 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 6 (c) is the diffraction pattern of the sample at 2θ=57°. Detailed Implementation
[0023] The principles and features of the present invention are described below (in conjunction with the accompanying drawings). The examples given are for illustrative purposes only and are not intended to limit the scope of the invention.
[0024] This invention discloses a rapid method for detecting the α-alumina conversion rate of calcined alumina. Those skilled in the art can refer to the content of this document and appropriately modify the process parameters to achieve the desired result. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art and are considered to be included in this invention. The methods and applications of this invention have been described through preferred embodiments, and those skilled in the art can obviously make modifications or appropriate alterations and combinations to the methods and applications described herein without departing from the content, spirit, and scope of this invention to realize and apply the technology of this invention.
[0025] It should be understood that the expression “one or more of…” individually includes each of the objects described after the expression, as well as various different combinations of two or more of the described objects, unless otherwise understood from the context and usage. The expression “and / or” combined with three or more described objects should be understood to have the same meaning, unless otherwise understood from the context.
[0026] The terms “including,” “having,” or “containing,” including the use of their grammatical synonyms, should generally be understood as open-ended and non-restrictive, for example, not excluding other unstated elements or steps, unless otherwise specifically stated or understood from the context.
[0027] It should be understood that the order of steps or the sequence of actions is not important as long as this application remains operational. Furthermore, two or more steps or actions can be performed simultaneously.
[0028] The use of any and all instances or exemplary language such as “e.g.” or “include” in this document is intended merely to better illustrate the application and does not constitute a limitation on the scope of the application. No language in this specification should be construed as indicating that any unclaimed element is essential to the practice of this application.
[0029] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.
[0030] The sources of some of the raw materials for this invention are shown below: The pure gamma alumina was purchased from a manufacturer that produces pure gamma alumina raw materials, and the 100% α-alumina was purchased from Japan Light Metals LS-22.
[0031] A rapid method for detecting the α-alumina conversion rate of calcined alumina includes the following detection steps: S1. Preparation of standard curves: Grind pure γ-alumina raw material to a particle size of 10um-50um, sieve, and collect the sieve blank; grind the 100% α-alumina conversion rate sample to a particle size of 10um-50um, sieve, and collect the sieve blank; use the above sieve blanks to prepare 50%-100% α-alumina conversion rate gradient standard substances with pure γ-alumina raw material and 100% α-alumina conversion rate sample respectively to obtain standard samples for later use; S2. Sample preparation: Grind the sample to be tested to a particle size of 10um-50um, sieve it, take the sieve blank, press it into a sample mold to obtain a sample sheet; S3. Sample installation: Install the standard sample obtained in step S1 and the sample sheet obtained in step S2 onto the X-ray diffractometer equipment respectively. S4. On-machine testing; S5. Data Processing: Construct a standard curve and substitute the sum of the peak areas of the three peaks of the sample into the standard curve to obtain the conversion rate.
[0032] In step S3, the pressed sample sheet is installed on the X-ray diffractometer equipment, ensuring it is fully inserted, and the SAFETY button is clicked to close the protective door.
[0033] In step S4, the standard sample is scanned first, and then the sample to be tested is scanned.
[0034] As an optional implementation, in step S4, the machine conditions are: scanning mode step scan.
[0035] In step S4, the driving mode is 2θ single action.
[0036] As an optional implementation, in step S4, the angle increment is 0.0020.
[0037] As an optional implementation, in step S4, the sampling time is 0.3s.
[0038] As an optional implementation, in step S4, the scanning angle is: 2θ: 24.8-26.2°, θ: 12.4°; 2θ: 42.5-44.5°, θ: 21.3°; 2θ: 56.6-58.3°, θ: 28.3°.
[0039] As an optional implementation, in step S5, the sum of the three peaks of the test results of the above standard sample is used to create a standard curve.
[0040] As an optional implementation, the formula for the standard curve is: y=ax+b Where y is the sum of the areas of the three peaks; α is the slope; b is the intersection of the curve and the y-axis; and x is the conversion rate corresponding to the peak area.
[0041] A further preferred method is to substitute the sum of the peak areas of the three peaks of the sample into the curve to obtain the conversion rate a.
[0042] The present invention will now be described in detail with reference to embodiments and experimental data.
[0043] The following experimental examples illustrate the beneficial effects of the present invention. Experimental methods not specifying particular conditions in the following examples are generally performed according to national standards. If no corresponding national standard exists, then generally accepted international standards, standard conditions, or conditions recommended by the manufacturer shall be followed.
[0044] Example 1
[0045] Plotting the standard curve: Pure γ-alumina raw material was ground to a particle size of 10µm-50µm, sieved, and the undersize material was collected. The 100% α-alumina conversion rate sample was ground to a particle size of 10µm-50µm, sieved, and the undersize material was collected. Using the above undersize materials, 80%, 90%, and 100% α-alumina conversion rate gradient standard substances were prepared using the pure γ-alumina raw material and the 100% α-alumina conversion rate sample, respectively, to obtain standard samples for later use. The standard samples were installed on an X-ray diffractometer. Testing was performed using the step scanning mode, with an angle increment of 0.0020°, a sampling time of 0.3s, and scanning angles of: 2θ: 24.8-26.2°, θ: 12.4°; 2θ: 42.5-44.5°, θ: 21.3°; 2θ: 56.6-58.3°, θ: 28.3°. Open the Jada7 analysis software, click Fi1e, click EAD, find the saved file, double-click it, and the spectrum will be read in; left-click "Find Peaks" to mark the angle, right-click "Find Peaks" to record the "Ares" peak area data; make a standard curve by summing the peak areas of the three peaks that appear at the positions of 2θ=25°, 2θ=43°, and 2θ=57° of the above standard sample.
[0046] The test results are shown in Table 1 below: Table 1
[0047] The above results were plotted as a standard curve with α-alumina conversion rate on the x-axis and peak area of the three peaks on the y-axis, as shown below. Figure 1 As shown.
[0048] Experimental Example 2
[0049] Grind the material (sample to be tested) to a particle size of 10um-50um, sieve it, collect the sieve blank, press it into a sample pan using a sample trough, and obtain a sample sheet; mount the sample sheet onto the X-ray diffractometer; test on the instrument: scan mode step scan, angle increment of 0.0020, sampling time of 0.3s, scanning angles: 2θ: 24.8-26.2°, θ: 12.4°; 2θ: 42.5-44.5°, θ: 21.3°; 2θ: 56.6-58.3°, θ: 28.3°; Open the Jada7 analysis software, click FI1e, click read, locate the saved file, double-click, and the spectrum will be imported; left-click "Find Peaks" to mark the angle, right-click "Find Peaks" to record the "Ares" peak area data. Substitute the sum of the peak areas of the three peaks of the sample into the standard curve y=3474.6x-58620 to obtain the conversion rate x.
[0050] Table 2
[0051] Table 3
[0052] Figure 2 The diffraction pattern of sample B32-batch number 20250402 is shown below. Figure 2 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 2 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 2 (c) is the diffraction pattern of the sample at 2θ=57°.
[0053] Figure 3 The diffraction pattern of sample A11-batch number 20250512 is shown below. Figure 3 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 3 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 3 (c) is the diffraction pattern of the sample at 2θ=57°.
[0054] Figure 4 The diffraction pattern of sample B03-batch number 20250516 is shown below. Figure 4 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 4 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 4 (c) is the diffraction pattern of the sample at 2θ=57°.
[0055] Figure 5 The diffraction patterns of parallel samples of dry powder, batch number 20250214, are shown below. Figure 5(a) is the diffraction pattern of the sample at 2θ = 25°. Figure 5 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 5 (c) is the diffraction pattern of the sample at 2θ=57°.
[0056] Figure 6 The diffraction pattern of sample B31-batch number 20250417 is shown below. Figure 6 (a) is the diffraction pattern of the sample at 2θ = 25°. Figure 6 (b) is the diffraction pattern of the sample at 2θ = 43°. Figure 6 (c) is the diffraction pattern of the sample at 2θ=57°.
[0057] Method accuracy verification: The conversion rate of sample B03-batch number 20250519 was tested using a semi-quantitative method (95±1)%. The conversion rate measured by the testing method of this invention was 95.6%, proving that the detection method of this invention is stable and accurate.
[0058] In summary, the detection method of this invention, by configuring different conversion rate gradients and establishing a mathematical model relating the peak area of the three peaks to the conversion rate, calculates the conversion rate. The method is simple, rapid, accurate, and stable, and effectively reflects the material conversion rate. Furthermore, the three peaks in this detection method are more representative, the results are stable, and the reproducibility is good.
[0059] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A rapid method for detecting the α-alumina conversion rate of calcined alumina, characterized in that, The following testing steps are included: S1. Preparation of standard curves: Grind pure γ-alumina raw material to a particle size of 10um-50um, sieve, and collect the sieve blank; grind the 100% α-alumina conversion rate sample to a particle size of 10um-50um, sieve, and collect the sieve blank; use the above sieve blanks to prepare 50%-100% α-alumina conversion rate gradient standard substances with pure γ-alumina raw material and 100% α-alumina conversion rate sample respectively to obtain standard samples for later use; S2. Sample preparation: Grind the sample to be tested to a particle size of 10um-50um, sieve it, take the sieve blank, press it into a sample mold to obtain a sample sheet; S3. Sample installation: Install the standard sample obtained in step S1 and the sample sheet obtained in step S2 onto the X-ray diffractometer equipment respectively. S4. On-machine testing; S5. Data Processing: Construct a standard curve and substitute the sum of the peak areas of the three peaks of the sample into the standard curve to obtain the conversion rate.
2. The rapid detection method for α-alumina conversion rate of calcined alumina according to claim 1, characterized in that, In step S4, the machine setup condition is: step scan mode.
3. The rapid detection method for α-alumina conversion rate of calcined alumina according to claim 2, characterized in that, In step S4, the angle increment is 0.0020.
4. The rapid detection method for α-alumina conversion rate of calcined alumina according to claim 3, characterized in that, In step S4, the sampling time is 0.3s.
5. The rapid detection method for α-alumina conversion rate of calcined alumina according to claim 2, characterized in that, In step S4, the scanning angle is: 2θ: 24.8-26.2°, θ: 12.4°; 2θ: 42.5-44.5°, θ: 21.3°; 2θ: 56.6-58.3°, θ: 28.3°.
6. The rapid detection method for α-alumina conversion rate of calcined alumina according to claim 2, characterized in that, In step S5, the sum of the three peaks of the test results of the above standard sample is used to create a standard curve.
7. The rapid detection method for α-alumina conversion rate of calcined alumina according to claim 6, characterized in that, The formula for the standard curve is: y = ax + b Where y is the sum of the areas of the three peaks; a is the slope; b is the intersection of the curve and the y-axis; and x is the α-alumina conversion rate corresponding to the peak area.
8. The rapid detection method for α-alumina conversion rate of calcined alumina according to claim 7, characterized in that, Substitute the sum of the peak areas of the three peaks of the sample into the curve formula to obtain the conversion rate.