Method for detecting purity content of aluminum nitride powder
The α-Al2O3 content in aluminum nitride powder was detected by X-ray diffraction technology, which solved the problems of high purity detection, cumbersome operation and low accuracy of aluminum nitride powder in the prior art, and achieved high-precision and low-cost purity detection.
Patent Information
- Application Number
- CN202510499622.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-21
- Publication Date
- 2025-07-11
AI Technical Summary
In the prior art, the purity detection method of aluminum nitride powder requires specific instruments, which are costly and cumbersome to operate and have low accuracy.
X-ray diffraction technology was used to detect the α-Al2O3 content in aluminum nitride powder, and the purity of aluminum nitride powder was calculated by formula purity of aluminum nitride powder = 100%-α-Al2O3 content.
The inspection process is simplified, the cost is reduced, and the accuracy and stability of the inspection results are improved, with an accuracy of up to 0.1%.
Smart Images
Figure CN120294041A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of aluminum nitride preparation, and particularly relates to a method for detecting the purity content of aluminum nitride powder. Background Art
[0002] Aluminum nitride is a covalent refractory compound with a hexagonal wurtzite structure, generally in the form of white or grayish-white powder, having advantages such as good electrical insulation, low dielectric constant and dielectric loss, thermal expansion coefficient matching with silicon, environmental protection and non-toxicity. Aluminum nitride ceramics are widely used in piezoelectric devices, structural ceramics, coatings, heaters, refractory materials, electro-optical devices, etc., and have become the most ideal substrate material and electronic device packaging material at present. The current main methods for synthesizing aluminum nitride powder are: direct nitridation of aluminum powder, carbothermal reduction method, chemical vapor deposition method and self-propagating high-temperature synthesis method. Among them, the aluminum nitride powder produced by the carbothermal reduction method has high purity, small particle size and narrow particle size distribution, and good stability.
[0003] At present, a nitrogen-oxygen analyzer is mostly used to detect the nitrogen and oxygen content of aluminum nitride powder, so as to determine the content of aluminum nitride in the sintered powder. For example: placing the aluminum nitride powder in a high-temperature sodium hydroxide solution to react to produce ammonia, and after condensation, absorbing and fully reacting with boric acid solution, using methyl red-methylene blue as an indicator, titrating with a standard solution of sulfuric acid or hydrochloric acid at a certain concentration, calculating the mass fraction of nitrogen element through the acid consumption, and thus calculating the mass fraction X of aluminum nitride. This method for detecting the content of aluminum nitride either requires specific instruments and has high detection costs, or the detection process is cumbersome and not intuitive, which is not conducive to operation and has low accuracy. Summary of the Invention
[0004] This application provides a method for detecting the purity content of aluminum nitride powder to reduce the difficulty of detecting the purity content of current aluminum nitride powder.
[0005] This application provides a method for detecting the purity content of aluminum nitride powder, and the method includes:
[0006] Obtaining the aluminum nitride powder to be measured;
[0007] Performing X-ray diffraction detection on the aluminum nitride powder to be measured to obtain the content of α-Al2O3;
[0008] According to the content of α-Al2O3, obtaining the purity of the aluminum nitride powder; the sum of the purity of the aluminum nitride powder and the content of α-Al2O3 is 100%;
[0009] According to the purity of the aluminum nitride powder, obtaining the purity of the aluminum nitride powder to be measured.
[0010] As an optional implementation manner, the purity range of the aluminum nitride powder to be measured is 1% to 100%.
[0011] As an optional implementation manner, the purity range of the aluminum nitride powder to be tested is 50% to 100%.
[0012] As an optional implementation manner, the purity range of the aluminum nitride powder to be tested is 90% to 100%.
[0013] As an optional implementation manner, the difference between the measured purity of the aluminum nitride powder and the actual purity of the aluminum nitride powder to be measured does not exceed 2%.
[0014] As an optional implementation, the difference does not exceed 1%.
[0015] As an optional implementation manner, the difference does not exceed 0.5%.
[0016] As an optional implementation manner, the difference does not exceed 0.1%.
[0017] As an optional implementation manner, the step of obtaining the aluminum nitride powder to be tested includes:
[0018] The aluminum nitride powder to be tested was prepared by carbothermal reduction method.
[0019] As an optional implementation, the X-ray diffraction detection device includes an X-ray diffractometer.
[0020] The above technical solution provided by the embodiment of the present application has the following advantages compared with the prior art:
[0021] The method provided in the embodiment of the present application uses X-ray diffraction detection to detect the content of α-Al2O3 in the aluminum nitride powder to be tested, and the purity of the aluminum nitride powder to be tested is obtained by the purity of the aluminum nitride powder = 100% - the content of α-Al2O3. This method uses innovative ideas and cleverly uses X-ray diffraction technology (XRD) to determine the content of the impurity phase in the aluminum nitride powder - α-Al2O3 (α-aluminum oxide), and then indirectly calculates the purity of the aluminum nitride powder. This method not only simplifies the detection process and reduces the detection cost, but also improves the accuracy and stability of the detection results, with an accuracy of up to 0.1%. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.
[0023] To more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the accompanying drawings required in the description of the embodiments or the prior art. Obviously, for those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.
[0024] Figure 1 Schematic flow chart of the method provided by the embodiment of the present application;
[0025] Figure 2 X-ray diffraction peak pattern provided by Embodiment 1 of the present application;
[0026] Figure 3 X-ray diffraction peak pattern provided by Embodiment 2 of the present application;
[0027] Figure 4 X-ray diffraction peak pattern provided by Embodiment 3 of the present application;
[0028] Figure 5 X-ray diffraction peak pattern provided by Embodiment 4 of the present application;
[0029] Figure 6 X-ray diffraction peak pattern provided by Embodiment 5 of the present application. Detailed implementation manners
[0030] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the following will clearly and completely describe the technical solutions in the embodiments of the present application with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are some, rather than all, of the embodiments of the present application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present application without creative efforts belong to the scope of protection of the present application.
[0031] Unless otherwise specifically stated, various raw materials, reagents, instruments, and equipment used in the present application can be obtained through market purchases or can be prepared by existing methods.
[0032] Currently, a nitrogen and oxygen analyzer is mostly used to detect the nitrogen and oxygen content of aluminum nitride powder, so as to determine the content of aluminum nitride in the sintered powder. For example: placing the aluminum nitride powder in a high-temperature sodium hydroxide solution to react to produce ammonia, absorbing and fully reacting it with a boric acid solution after condensation, using methyl red - methylene blue as an indicator, and titrating with a standard solution of sulfuric acid or hydrochloric acid at a certain concentration. The mass fraction of nitrogen element is calculated through the acid consumption, and thus the mass fraction X of aluminum nitride is calculated. This method for detecting the content of aluminum nitride either requires specific instruments, has a high detection cost, or has a cumbersome and unintuitive detection process, which is not conducive to operation and has low accuracy.
[0033] The inventors found that in the aluminum nitride powder completely decarbonized by the carbothermal reduction method, no other impurities are introduced, and only two powders, aluminum nitride and α-Al2O3, exist, and the presence of aluminum nitride has little effect on detecting the content of α-Al2O3 using an X-ray diffractometer.
[0034] Therefore, the present application intends to provide a method for detecting the purity content of aluminum nitride powder, which uses an X-ray diffractometer to measure the content of α-Al2O3 in the aluminum nitride powder, and thereby infers the content of aluminum nitride in the powder.
[0035] Figure 1 is a schematic flow chart of the method provided by the embodiments of the present application. As Figure 1 shown, the embodiments of the present application provide a method for detecting the purity content of aluminum nitride powder, and the method includes:
[0036] S1. Obtain the aluminum nitride powder to be tested;
[0037] In some embodiments, obtaining the aluminum nitride powder to be tested includes: preparing the aluminum nitride powder by the carbothermal reduction method to obtain the aluminum nitride powder to be tested. The inventors found that in the aluminum nitride powder completely decarbonized by the carbothermal reduction method, no other impurities are introduced, and only two powders, aluminum nitride and α-Al2O3, exist.
[0038] In some embodiments, the present method can perform purity detection on aluminum nitride powder with a purity range of 1% to 100%.
[0039] Furthermore, the present method can perform relatively accurate purity detection on aluminum nitride powder with a purity range of 50% to 100%.
[0040] Even further, the present method can perform more accurate purity detection on aluminum nitride powder with a purity range of 90% to 100%.
[0041] S2. Perform X-ray diffraction detection on the aluminum nitride powder to be tested to obtain the content of α-Al2O3;
[0042] In some embodiments, the equipment for the X-ray diffraction detection includes an X-ray diffractometer.
[0043] In S2, a common X-ray diffractometer is used to scan the aluminum nitride powder sample. X-ray diffraction technology can accurately identify the phase composition and content in the sample by analyzing the diffraction effect of the substance on X-rays. The content of α-Al2O3 (α-aluminum oxide) is mainly detected because α-aluminum oxide is a common impurity phase in the preparation process of aluminum nitride.
[0044] S3. Obtain the purity of the aluminum nitride powder according to the content of α-Al2O3; the sum of the purity of the aluminum nitride powder and the content of α-Al2O3 is 100%.
[0045] In S3, by analyzing the diffraction peak intensity or area of α-Al2O3 in the X-ray diffraction pattern, and using the standard curve or quantitative analysis method, accurately calculate the content of α-Al2O3 in the aluminum nitride powder. Subsequently, based on the principle that the sum of the purity of the aluminum nitride powder and the content of α-Al2O3 is 100%, calculate the purity of the aluminum nitride powder through the formula "purity of the aluminum nitride powder = 100% - content of α-Al2O3".
[0046] S4. Obtain the purity of the aluminum nitride powder to be measured according to the purity of the aluminum nitride powder = 100% - content of α-Al2O3.
[0047] In some embodiments, the difference between the measured purity of the aluminum nitride powder and the actual purity of the aluminum nitride powder to be measured does not exceed 2%. That is, the detection accuracy of the purity of the aluminum nitride powder can reach 2%.
[0048] Furthermore, the difference between the measured purity of the aluminum nitride powder and the actual purity of the aluminum nitride powder to be measured does not exceed 1%. That is, the detection accuracy of the purity of the aluminum nitride powder can reach 1%.
[0049] Even further, the difference between the measured purity of the aluminum nitride powder and the actual purity of the aluminum nitride powder to be measured does not exceed 0.5%. That is, the detection accuracy of the purity of the aluminum nitride powder can reach 0.5%.
[0050] Still further, the difference between the measured purity of the aluminum nitride powder and the actual purity of the aluminum nitride powder to be measured does not exceed 0.1%. That is, the detection accuracy of the purity of the aluminum nitride powder can reach 0.1%.
[0051] This method has the following advantages:
[0052] 1. Low cost: Only an ordinary X-ray diffractometer is required to complete the detection, without expensive special equipment, reducing the detection cost.
[0053] 2. Simple operation: The detection method is simple and fast, without complex pretreatment steps or professional skills, improving the detection efficiency.
[0054] 3. Accurate and stable results: Utilizing the high sensitivity and accuracy of X-ray diffraction technology, it can stably and accurately detect the content of α-Al2O3 in the aluminum nitride powder, and then calculate the purity of the aluminum nitride, with an accuracy of up to 0.1%.
[0055] 4. Strong applicability: This method is not only applicable to laboratory research, but also applicable to on-line monitoring and quality control in industrial production, with broad application prospects.
[0056] In summary, the aluminum nitride powder purity detection method proposed in the embodiments of the present application provides an efficient and economical solution for the field of aluminum nitride preparation and quality control with its advantages of low cost, easy operation, high accuracy, and stability. The popularization and application of this method will help improve the overall quality level of aluminum nitride products and promote the application and development of aluminum nitride materials in more fields.
[0057] The following further elaborates on the present application in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present application and not to limit the scope of the present application. For the experimental methods without specific conditions noted in the following embodiments, they are generally determined according to national standards. If there is no corresponding national standard, they are carried out according to general international standards, conventional conditions, or the conditions recommended by the manufacturer.
[0058] Example 1
[0059] Add a small amount of α-Al2O3 to the powder of pure aluminum nitride phase (aluminum nitride powder of Xiamen Juchi), and detect the content of α-aluminum oxide in the powder. The specific steps are as follows:
[0060] (1) Blending of aluminum nitride and α-Al2O3: Take the pure-phase aluminum nitride powder provided by Xiamen Juchi and blend it with α-Al2O3 to form a 10g sample, in which α-Al2O3 accounts for 2%, and mix well.
[0061] (2) XRD detection: Use an X-ray diffractometer to quantitatively detect α-Al2O3 in the sample. The X-ray diffraction peak pattern is as Figure 2 shown.
[0062] It can be seen from the figure that the measured α-Al2O3 is 1.9%. Therefore, the purity of the aluminum nitride powder is 98.1%.
[0063] Example 2
[0064] Add a small amount of α-Al2O3 to the powder of pure aluminum nitride phase (aluminum nitride powder of Xiamen Juchi), and detect the content of α-aluminum oxide in the powder. The specific steps are as follows:
[0065] (1) Blending of aluminum nitride and α-Al2O3: Take the pure-phase aluminum nitride powder provided by Xiamen Juchi and blend it with α-Al2O3 to form a 10g sample, in which α-Al2O3 accounts for 4%, and mix well.
[0066] (2) XRD detection: Use an X-ray diffractometer to quantitatively detect α-Al2O3 in the sample. The X-ray diffraction peak pattern is as Figure 3 shown.
[0067] It can be seen from the figure that the measured α-Al2O3 is 3.5%. Therefore, the purity of the aluminum nitride powder is 96.5%.
[0068] Example 3
[0069] Add a small amount of α-Al2O3 to the powder of pure aluminum nitride phase (aluminum nitride powder from Xiamen Juchi), and detect the content of α-aluminum oxide in the powder. The specific steps are as follows:
[0070] (1) Blending of aluminum nitride and α-Al2O3: Take the pure-phase aluminum nitride powder provided by Xiamen Juchi and blend it with α-Al2O3 to form a 10g sample, where α-Al2O3 accounts for 6%, and mix well.
[0071] (2) XRD detection: Use an X-ray diffractometer to quantitatively detect α-Al2O3 in the sample. Its X-ray diffraction peak pattern is as Figure 4 shown.
[0072] It can be seen from the figure that the measured α-Al2O3 is 5.2%. Therefore, the purity of the aluminum nitride powder is 94.8%.
[0073] Example 4
[0074] Add a small amount of α-Al2O3 to the powder of pure aluminum nitride phase (aluminum nitride powder from Xiamen Juchi), and detect the content of α-aluminum oxide in the powder. The specific steps are as follows:
[0075] (1) Blending of aluminum nitride and α-Al2O3: Take the pure-phase aluminum nitride powder provided by Xiamen Juchi and blend it with α-Al2O3 to form a 10g sample, where α-Al2O3 accounts for 10%, and mix well.
[0076] (2) XRD detection: Use an X-ray diffractometer to quantitatively detect α-Al2O3 in the sample. Its X-ray diffraction peak pattern is as Figure 5 shown.
[0077] It can be seen from the figure that the measured α-Al2O3 is 8.4%. Therefore, the purity of the aluminum nitride powder is 91.6%.
[0078] Example 5
[0079] Detect the content of α-Al2O3 in the powder of pure aluminum nitride phase. Its X-ray diffraction peak pattern is as Figure 6 shown.
[0080] It can be seen from the figure that the measured α-Al2O3 is 0.4%. Therefore, the purity of the aluminum nitride powder is 99.6%.
[0081] Various embodiments of the present application may exist in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity and should not be construed as a rigid limitation on the scope of the present application; therefore, it should be considered that the described range description has specifically disclosed all possible sub-ranges and single values within that range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., and single numbers within the range, such as 1, 2, 3, 4, 5, and 6, and this applies regardless of the range. Additionally, whenever a numerical range is indicated herein, it means including any cited number (fraction or integer) within the indicated range.
[0082] In the present application, unless otherwise stated, the orientation terms such as "upper" and "lower" specifically refer to the drawing directions in the figures. Additionally, in the description of the specification of the present application, the terms "include", "comprise", etc. mean "including but not limited to". In this text, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. In this text, "and / or" describes the associated relationship of associated objects and indicates that three relationships can exist. For example, A and / or B can mean: A exists alone, A and B exist simultaneously, or B exists alone. Wherein A and B can be singular or plural. In this text, "at least one" means one or more, and "a plurality" means two or more. "At least one kind", "at least one (item) of the following" or similar expressions refer to any combination of these items, including any combination of single item (s) or plural items (s). For example, "at least one (item) of a, b, or c", or, "at least one (item) of a, b, and c" can both mean: a, b, c, a - b (i.e., a and b), a - c, b - c, or a - b - c, where a, b, and c can be single or multiple respectively.
[0083] The above description is only the specific implementation manners of the present application, enabling those skilled in the art to understand or implement the present application. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to these embodiments shown herein, but rather to the broadest scope consistent with the principles and novel features claimed herein.
Claims
1. A method for detecting the purity content of aluminum nitride powder, characterized in that, The method includes: obtaining aluminum nitride powder to be measured; performing X-ray diffraction detection on the aluminum nitride powder to be measured to obtain the content of α-Al2O3; obtaining the purity of the aluminum nitride powder according to the content of α-Al2O3; the sum of the purity of the aluminum nitride powder and the content of α-Al2O3 is 100%; obtaining the purity of the aluminum nitride powder to be measured.
2. The detection method for the purity content of aluminum nitride powder according to claim 1, characterized in that, The purity range of the aluminum nitride powder to be measured is 1% to 100%.
3. The detection method of the purity content of aluminum nitride powder according to claim 2, characterized in that, The purity range of the aluminum nitride powder to be measured is 50% to 100%.
4. The method for detecting the purity content of aluminum nitride powder according to claim 3, wherein, The purity range of the aluminum nitride powder to be measured is 90% to 100%.
5. The detection method for the purity content of aluminum nitride powder according to claim 1, characterized in that, The difference between the measured purity of the aluminum nitride powder and the actual purity of the aluminum nitride powder to be measured does not exceed 2%.
6. The detection method of the purity content of aluminum nitride powder according to claim 5, wherein, The difference does not exceed 1%.
7. The detection method of the purity content of aluminum nitride powder according to claim 6, characterized in that, The difference does not exceed 0.5%.
8. The detection method for the purity content of aluminum nitride powder according to claim 7, wherein, The difference does not exceed 0.1%.
9. The detection method of the purity content of aluminum nitride powder according to claim 1, characterized in that, The obtaining of the aluminum nitride powder to be measured includes: preparing the aluminum nitride powder to be measured by a carbothermal reduction method.
10. The detection method for the purity content of aluminum nitride powder according to claim 1, characterized in that, The equipment for the X-ray diffraction detection includes an X-ray diffractometer.