A hydrolysis-resistant aluminum nitride powder and a method for producing the same
By coating the surface of aluminum nitride powder with tetraethyl orthosilicate and hydroxyl-terminated polydimethylsiloxane, a silicon-carbon-oxygen inorganic network structure is formed, which solves the problem of easy hydrolysis of aluminum nitride powder in humid environments and achieves a significant improvement in hydrolysis resistance.
Patent Information
- Application Number
- CN202311406574.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-27
- Publication Date
- 2025-12-16
- Estimated Expiration
- 2043-10-27
AI Technical Summary
Aluminum nitride powder is prone to reacting with water in the air during storage and transportation, resulting in the formation of aluminum hydroxide on the surface and the release of ammonia gas, which affects its thermal conductivity and limits its application in the field of thermal conductivity.
Tetraethyl orthosilicate was used as a crosslinking agent to coat hydroxyl-terminated polydimethylsiloxane onto the surface of aluminum nitride powder. The silicon-carbon-oxygen inorganic network structure was formed by high-temperature calcination, which improved the hydrolysis resistance.
It significantly improves the hydrolysis resistance of aluminum nitride powder, preventing it from hydrolyzing after soaking in water at 80℃ for 73 hours, thus solving the problem of easy hydrolysis in humid environments.
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Abstract
Description
Technical Field
[0001] This invention relates to a method for preparing hydrolysis-resistant aluminum nitride powder, belonging to the field of ceramic technology. Background Technology
[0002] Aluminum nitride (AlN) has a wide range of excellent properties, including high thermal conductivity of 320 W / (m·K), good electrical insulation, low dielectric constant at room temperature, high melting point of over 2200℃, ultra-high bandgap of 6.2 eV, low dielectric loss, non-toxicity, high temperature resistance, and corrosion resistance. Therefore, it is widely used in substrate materials, integrated circuit substrate materials, and other fields, and is considered an ideal packaging material for next-generation highly integrated semiconductor substrates and electronic devices.
[0003] Although aluminum nitride (AlN) has many advantages and wide applications, it suffers from poor hydrolysis resistance. Particularly during storage and transportation, it readily reacts with moisture in the air, leading to the formation of aluminum hydroxide on the particle surface, accompanied by the generation and release of ammonia gas. Inhalation of ammonia can irritate and corrode the upper respiratory tract. The aluminum hydroxide on the powder surface also affects the thermal conductivity of AlN, thus limiting its applications in thermal conductivity fields such as functional materials, ceramic substrates, and semiconductor materials. Therefore, it is necessary to treat AlN to improve its hydrolysis resistance. Currently, the preparation methods for hydrolysis-resistant AlN powder mainly fall into three categories: heat treatment, inorganic modification, and organic modification. These methods primarily increase hydrolysis resistance by treating the surface of aluminum nitride to reduce the contact area with water. However, according to current results, the hydrolysis resistance of treated aluminum nitride powder is not outstanding at high temperatures. Therefore, the preparation of highly hydrolysis-resistant aluminum nitride powder is crucial. Summary of the Invention
[0004] In view of the above-mentioned problem of easy hydrolysis of aluminum nitride, the present invention provides a method for preparing hydrolysis-resistant aluminum nitride powder, which aims to effectively improve the hydrolysis resistance of aluminum nitride powder.
[0005] To achieve the above objectives, the present invention adopts the following technical solution:
[0006] This invention first discloses a method for preparing hydrolysis-resistant aluminum nitride powder, characterized in that: the hydrolysis-resistant aluminum nitride powder is obtained by coating the surface of aluminum nitride powder with hydroxyl-terminated polydimethylsiloxane linked by tetraethyl orthosilicate as a crosslinking agent. The method involves: first, using aluminum nitride powder as raw material, partially hydrolyzing it in water at a certain temperature to obtain Al(OH)3@AlN powder, followed by high-temperature dehydration to obtain Al2O3@AlN powder; then, placing Al2O3@AlN under acidic conditions, crosslinking Al2O3@AlN with the hydroxyl-terminated polydimethylsiloxane using tetraethyl orthosilicate to obtain the coated Al2O3@AlN powder; finally, calcining the coated Al2O3@AlN powder in a high-temperature oven to obtain the target product, hydrolysis-resistant aluminum nitride powder, denoted as Al2O3@AlN-P. Specifically, the method includes the following steps:
[0007] Step 1: Preparation of Al(OH)3@AlN powder
[0008] Add 5-10g of aluminum nitride and 40-80mL of deionized water to a single-necked flask, place the flask open in an oil bath at 60-90℃ for hydrolysis, measure the pH value every 1min, stop heating when pH=8-11, wash the reaction solution with deionized water, dry it, and obtain Al(OH)3@AlN powder.
[0009] Step 2: Preparation of Al2O3@AlN powder
[0010] The Al(OH)3@AlN powder was thoroughly ground and then placed in an oven at 300-450℃ for 1-5 hours to obtain Al2O3@AlN powder.
[0011] Step 3: Preparation of coated Al2O3@AlN powder
[0012] Add 0.2–10 g of tetraethyl orthosilicate and 0.2–10 g of hydroxyl-terminated polydimethylsiloxane to 10–20 mL of industrial ethanol, mix well, and then slowly add acidic solution dropwise until the pH of the system is 1–7. Then stir at room temperature for 20–40 min to obtain a mixed solution.
[0013] Take 0.1-0.8g of Al2O3@AlN powder that has been ultrasonically stirred for 10-20min and add it to the mixed solution. Then place it in an oil bath and heat and stir at 60-90℃ for 30min. Centrifuge and wash with industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate. Vacuum dry at 50-80℃ for 10-30h to obtain coated Al2O3@AlN powder.
[0014] Step 4: Preparation of Al2O3@AlN-P powder
[0015] Take the coated Al2O3@AlN powder and place it in a crucible, then put it in a high-temperature oven and calcine it at 150-250℃ for 1-3 hours, then calcine it at 300-500℃ for 1-3 hours to obtain Al2O3@AlN-P powder.
[0016] Preferably, the aluminum nitride described in step 1 is dried in a vacuum oven at 80–100°C for 12–24 hours before use.
[0017] Preferably, pH test strips are used to test the pH value in step 1.
[0018] Preferably, the purity of the industrial ethanol described in step 3 is 95%.
[0019] Preferably, the acidic solution in step 3 is selected from hydrochloric acid, nitric acid, sulfuric acid, acetic acid, and boric acid.
[0020] The beneficial effects of this invention are reflected in:
[0021] 1. This invention involves heating aluminum nitride to partially hydrolyze the surface, followed by high-temperature dehydration to form Al2O3. Then, Al2O3 is cross-linked with hydroxyl-terminated polydimethylsiloxane (PDMS) via the hydrolysis product of tetraethyl orthosilicate. The hydroxyl groups dehydrate and condense to form a network, coating the powder surface. Simultaneously, the hydroxyl-terminated PDMS undergoes self-condensation, and methyl groups survive sintering after heating in air at high temperatures, thus forming a silicon-carbon-oxygen inorganic network structure. This method effectively improves the hydrolysis resistance of aluminum nitride powder.
[0022] 2. The aluminum nitride powder prepared by this invention does not hydrolyze when soaked in water at 80°C for 73 hours, and its resistance to hydrolysis is significantly improved, solving the problem of easy hydrolysis of aluminum nitride in humid environments. Attached Figure Description
[0023] Figure 1 The images shown are scanning electron microscope (SEM) images of the products obtained in Example 1 of the present invention, wherein: (a) is a scanning electron microscope image of aluminum nitride; (b) is a scanning electron microscope image of Al(OH)3@AlN; (c) is a scanning electron microscope image of Al2O3@AlN; (d) is a scanning electron microscope image of Al2O3@AlN-P; and (e) is a transmission electron microscope (TEM) image of Al2O3@AlN-P.
[0024] Figure 2 The figures show the pH values of the aluminum nitride suspension of the present invention over time, wherein: (a) the figures show the pH values of the modified aluminum nitride powders of Examples 1 and 2 over time; and (b) the figures show the pH values of the modified aluminum nitrides of Examples 1 and 3-5 over time.
[0025] Figure 3The image shows the XRD pattern of the original aluminum nitride and Al2O3@AlN-P after hydrolysis in Example 1 of this invention. Detailed Implementation
[0026] The embodiments of the present invention are described in detail below. These embodiments are implemented based on the technical solution of the present invention, and provide detailed implementation methods and specific operation processes. However, the scope of protection of the present invention is not limited to the following embodiments.
[0027] Example 1
[0028] In this embodiment, hydrolysis-resistant aluminum nitride powder is prepared according to the following steps:
[0029] Step 1: Preparation of Al(OH)3@AlN powder
[0030] Take 10g of aluminum nitride that has been dried in a vacuum oven at 100℃ for 24h and add 50mL of deionized water into a single-necked flask. Place the flask open in an oil bath at 80℃ for hydrolysis. Measure the pH value every 1min. Stop heating when pH=11. Wash the reaction solution 3 times with deionized water and dry to obtain Al(OH)3@AlN powder.
[0031] Step 2: Preparation of Al2O3@AlN powder
[0032] The Al(OH)3@AlN powder was thoroughly ground and then heated in a high-temperature oven at 300°C for 2 hours to obtain Al2O3@AlN powder.
[0033] Step 3: Preparation of coated Al2O3@AlN powder
[0034] Add 0.6 g of tetraethyl orthosilicate and 5.4 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0035] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0036] Step 4: Preparation of Al2O3@AlN-P powder
[0037] The coated Al2O3@AlN powder was placed in a crucible and then placed in a high-temperature oven. It was first calcined at 200℃ for 1 hour and then at 400℃ for 1 hour to obtain Al2O3@AlN-P powder.
[0038] Example 2
[0039] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0040] Add 0.6 g of tetraethyl orthosilicate and 5.4 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0041] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Stir at room temperature for 30min, centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0042] Example 3
[0043] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0044] Add 0.6 g of tetraethyl orthosilicate and 5.4 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 15 min to obtain a mixed solution.
[0045] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0046] Example 4
[0047] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0048] Add 0.6 g of tetraethyl orthosilicate and 5.4 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 45 min to obtain a mixed solution.
[0049] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0050] Example 5
[0051] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0052] Add 0.6 g of tetraethyl orthosilicate and 5.4 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 60 min to obtain a mixed solution.
[0053] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0054] Example 6
[0055] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0056] Add 1.2 g of tetraethyl orthosilicate and 4.8 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0057] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0058] Example 7
[0059] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0060] Add 1.8 g of tetraethyl orthosilicate and 4.2 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0061] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0062] Example 8
[0063] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0064] Add 2.4 g of tetraethyl orthosilicate and 3.6 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0065] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0066] Example 9
[0067] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0068] Add 3g of tetraethyl orthosilicate and 3g of hydroxyl-terminated polydimethylsiloxane to 14mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30min to obtain a mixed solution.
[0069] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0070] Example 10
[0071] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0072] Add 3.6 g of tetraethyl orthosilicate and 2.4 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0073] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0074] Example 11
[0075] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0076] Add 4.2 g of tetraethyl orthosilicate and 1.8 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0077] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0078] Example 12
[0079] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0080] Add 4.8 g of tetraethyl orthosilicate and 1.2 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0081] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0082] Example 13
[0083] This embodiment prepares hydrolysis-resistant aluminum nitride powder using the same method as in Example 1, with the only difference being step 3:
[0084] Add 5.4 g of tetraethyl orthosilicate and 0.6 g of hydroxyl-terminated polydimethylsiloxane to 14 mL of 95% industrial ethanol, mix well, then slowly add dilute hydrochloric acid solution until the pH of the system is 2-3, and then stir at room temperature for 30 min to obtain a mixed solution.
[0085] Take 0.5g of Al2O3@AlN powder that has been ultrasonically stirred for 15min and add it to the above mixed solution. Then put it in an oil bath and heat and stir at 80℃ for 30min. Centrifuge, wash three times with 95% industrial ethanol to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dry at 60℃ for 24h to obtain coated Al2O3@AlN powder.
[0086] Figure 1 The images shown are scanning electron microscope (SEM) images of the products obtained in Example 1 of this invention, wherein: (a) is an SEM image of aluminum nitride; (b) is an SEM image of Al(OH)3@AlN; (c) is an SEM image of Al2O3@AlN; (d) is an SEM image of Al2O3@AlN-P; and (e) is a transmission electron microscope (TEM) image of Al2O3@AlN-P. From image (b), it can be seen that Al(OH)3@AlN has a distinct nanocluster structure on its surface compared to the original aluminum nitride, indicating the formation of Al(OH)3. Furthermore, in image (c), the surface layered structure is more disordered than the Al(OH)3@AlN powder distribution, while in image (d), the Al2O3@AlN-P powder surface is denser. This is due to the formation of a core-shell structure on the powder surface after high-temperature sintering, with a thickness of approximately 20 nm, as shown in image (e).
[0087] The hydrolysis resistance test of this invention is carried out by mixing Al2O3@AlN-P powder with deionized water at a mass ratio of 1:20, and observing the change of pH value over time in an oil bath at 80°C. The hydrolysis resistance test is terminated when the pH value reaches approximately 9.
[0088] Figure 2Figure 1 shows the pH value of the aluminum nitride suspension of the present invention changing over time, wherein: (a) Figure 2 shows the pH value of Al2O3@AlN-P in Examples 1 and 2 changing over time; (b) Figure 3 shows the pH value of Al2O3@AlN-P in Examples 1 and 3-5 changing over time. Figure 2 (a) It can be seen that the hydrolysis resistance of the powder subjected to heat coating is significantly improved, which is due to the increased coating rate at relatively higher temperatures. Figure 2 (b) It can be seen that the best effect is achieved when the hydrolysis time of tetraethyl orthosilicate (TEOS) is 30 min. This may be because the hydrolysis product Si(OH)4 of TEOS undergoes a condensation reaction with PDMS at a longer time, resulting in an unsatisfactory coating effect after the addition of powder.
[0089] Table 1 shows the pH value of Al2O3@AlN-P in Examples 1 and 6-13 of this invention over time. The graph shows that the results of the ten sets of data are relatively similar. When TEOS:PDMS = 1:9, the pH value reaches 8.8 after 73 hours, which is better than the other data. Therefore, this ratio was selected. The results suggest that the difference may be due to the relatively excessive amount of TEOS and PDMS powder, resulting in no significant difference under different ratios.
[0090] Table 1
[0091]
[0092] Figure 3 The figures show the XRD patterns of the original aluminum nitride and Al2O3@AlN-P after hydrolysis in Example 1 of this invention. The figure shows that the diffraction peak of Al(OH)3 after hydrolysis of the original AlN is strong, accompanied by a decrease in the peak of pure AlN, which is a direct result and evidence of AlN hydrolysis. The diffraction peaks of Al(OH)3 and AlOOH in the Al2O3@AlN-P powder are very weak after 73 hours of hydrolysis; these may be diffraction peaks of Al(OH)3@AlN. The results indicate that the powder pretreated with AlN before coating has stronger resistance to hydrolysis.
[0093] The above are merely exemplary embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for producing an anti-hydrolysis aluminum nitride powder, characterized by: The anti-hydrolysis aluminum nitride powder is obtained by coating hydroxyl-terminated polydimethylsiloxane on the surface of aluminum nitride powder with tetraethyl orthosilicate as a crosslinking agent, and the preparation method comprises the following steps: Step 1, preparation of Al(OH)3@AlN powder 5-10 g of aluminum nitride and 40-80 mL of deionized water are taken into a single-necked flask, which is placed in an oil bath at 60-90 DEG C for hydrolysis, and the pH value is measured every 1 min, and when the pH value is 8-11, the heating is stopped, the reaction solution is washed with deionized water, and dried to obtain Al(OH)3@AlN powder; Step 2, preparation of Al2O3@AlN powder The Al(OH)3@AlN powder is fully ground and then heated in an oven at 300-450 DEG C for 1-5 h to obtain Al2O3@AlN powder; Step 3, preparation of coated Al2O3@AlN powder 0.2-10 g of tetraethyl orthosilicate and 0.2-10 g of hydroxyl-terminated polydimethylsiloxane are added into 10-20 mL of industrial ethanol, mixed uniformly, and then slowly dripped into an acidic solution until the pH value of the system is 1-7, and then stirred at room temperature for 20-40 min to obtain a mixed solution; 0.1-0.8 g of Al2O3@AlN powder after ultrasonic stirring for 10-20 min is taken into the mixed solution, and then placed in an oil bath at 60-90 DEG C for heating and stirring for 30 min, centrifuged and washed to remove excess hydroxyl-terminated polydimethylsiloxane and tetraethyl orthosilicate, and vacuum dried at 50-80 DEG C for 10-30 h to obtain coated Al2O3@AlN powder; Step 4, preparation of Al2O3@AlN-P powder The coated Al2O3@AlN powder is placed in a crucible and then put into a high-temperature oven, first calcined at 150-250 DEG C for 1-3 h, and then calcined at 300-500 DEG C for 1-3 h to obtain Al2O3@AlN-P powder.
2. The method of producing an anti-hydrolysis aluminum nitride powder according to claim 1, wherein The aluminum nitride in step 1 is dried in a vacuum oven at 80-100 DEG C for 12-24 h.
3. The method of claim 1, wherein the anti-hydrolysis aluminum nitride powder is prepared by the steps of: preparing a mixture of aluminum powder and a binder; and sintering the mixture at a temperature of 600 to 800°C in a nitrogen atmosphere. The acidic solution in step 3 is selected from one of hydrochloric acid, nitric acid, sulfuric acid, acetic acid and boric acid.
4. The anti-hydrolysis aluminum nitride powder obtained by the preparation method in any one of claims 1-3.
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