Preparation method of high-stability aluminum oxide powder
By treating alumina powder with proton irradiation and modified ball milling, combined with modification with specific solutions, the problems of insufficient thermal conductivity and acid corrosion resistance of alumina powder were solved, and the preparation of highly stable alumina powder was achieved, which is suitable for heat dissipation materials in the electronics industry and new energy vehicles.
Patent Information
- Application Number
- CN202510789661.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-13
- Publication Date
- 2025-10-17
AI Technical Summary
Existing alumina powder has poor thermal conductivity and insufficient acid corrosion resistance, which limits its application in the electronics industry and new energy vehicles.
Alumina powder was treated with proton irradiation, then immersed in lanthanum nitrate solution and ball-milled with a modified ball mill. It was modified with a conditioning solution of nano-silica, bentonite, chitosan solution and yttrium nitrate solution to optimize the interlayer spacing and improve stability.
The thermal conductivity and acid corrosion resistance of alumina powder are significantly improved, meeting the needs of electronic devices and new energy vehicles for heat dissipation materials.
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Abstract
Description
TECHNICAL FIELD
[0001] The application relates to the technical field of alumina powder, in particular to a preparation method of high-stability alumina powder. BACKGROUND
[0002] With the development of the electronic industry and new energy vehicles, the power of related electronic devices is greatly improved, the heat dissipation capacity is also improved, and the demand for the thermal conductivity of the heat dissipation alumina is further improved. The poor thermal conductivity of the alumina powder in the prior art and the poor acid corrosion stability of the product limit the use efficiency of the product. Therefore, the application is further improved. SUMMARY
[0003] In view of the defects of the prior art, the application aims to provide a preparation method of high-stability alumina powder to solve the problems in the background art.
[0004] The application solves the technical problems by adopting the following technical scheme: The application provides a preparation method of high-stability alumina powder, which comprises the following steps Step 1: irradiating alumina in a proton irradiation box first, and obtaining irradiated alumina after irradiation; Step 2: immersing the irradiated alumina in a sufficient amount of lanthanum nitrate solution for immersion treatment, and obtaining immersed alumina agent after immersion, filtration and drying; Step 3: modifying and ball milling the immersed alumina agent and modified ball milling agent at a weight ratio of 5:2, the ball milling modification speed is 1000-1500 r / min, the ball milling time is 2 h, and high-thermal-conductivity alumina powder is obtained after water washing and drying.
[0005] Preferably, the irradiation power of the irradiation treatment is 350-400 W, and the irradiation time is 5-10 min.
[0006] Preferably, the mass fraction of the lanthanum nitrate solution is 2-5%, the immersion power of the immersion treatment is 350-400 W, and the immersion time is 20-30 min.
[0007] Preferably, the preparation method of the modified ball milling agent is as follows: Mixing and uniformly mixing nano-silicon dioxide in a sufficient amount of hydrochloric acid solution, then water washing and drying, stirring and adjusting the dried nano-silicon dioxide and adjusting liquid at a weight ratio of 2:5, and then water washing and drying to obtain the modified ball milling agent.
[0008] Preferably, the mass fraction of the hydrochloric acid solution is 2-5%.
[0009] Preferably, the stirring speed of the stirring conditioning treatment is 450-500 r / min, and the stirring time is 10-20 min.
[0010] Preferably, the preparation method of the conditioning liquid is as follows: The bentonite is first heat-treated at 210-220 DEG C for 5-10 min, then cooled to 55 DEG C at a rate of 1-3 DEG C / min, and kept for 5-10 min; after the keeping, 3-5 parts of the kept bentonite, 1-3 parts of the chitosan solution, 2-5 parts of sodium dodecyl benzene sulfonate, and 4-7 parts of yttrium nitrate solution are fully blended to obtain the conditioning liquid.
[0011] Preferably, the mass fraction of the chitosan solution is 2-5%, and the mass fraction of the yttrium nitrate solution is 1-4%.
[0012] Compared with the prior art, the application has the following beneficial effects: The alumina powder is subjected to proton irradiation to activate the activity, and then is immersed in a lanthanum nitrate solution for improvement, so that the coordination effect of the alumina and the modified ball mill is improved; meanwhile, the modified ball mill is subjected to stirring conditioning treatment with nano-silica and the conditioning liquid; the bentonite in the conditioning liquid is subjected to heat treatment at 210-220 DEG C for 5-10 min, and then is cooled to 55 DEG C at a rate of 1-3 DEG C / min and kept for 5-10 min, so that the layer spacing of the sheet is optimized and the sheet interpenetration effect is improved; then, the chitosan solution, the sodium dodecyl benzene sulfonate, and the yttrium nitrate solution are used for improvement together, so that the acid corrosion stability of the product is improved. DETAILED DESCRIPTION
[0013] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to specific embodiments. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.
[0014] The preparation method of the high-stability alumina powder in the embodiment comprises the following steps Step one: the alumina is first subjected to irradiation treatment in a proton irradiation box, and then irradiation ends to obtain irradiated alumina; Step two: the irradiated alumina is immersed in a sufficient amount of lanthanum nitrate solution for immersion treatment, and then immersion ends to obtain an immersed alumina agent through filtration and drying; Step three: the immersed alumina agent and the modified ball mill are subjected to ball milling modification treatment according to a weight ratio of 5:2, the ball milling modification speed is 1000-1500 r / min, the ball milling time is 2 h, and then ball milling ends to obtain a high-thermal-conductivity alumina powder through water washing and drying.
[0015] The irradiation power of the irradiation treatment of the embodiment is 350-400W, and the irradiation time is 5-10min.
[0016] The mass fraction of the lanthanum nitrate solution of the embodiment is 2-5%; the immersion power of the immersion treatment is 350-400W, and the immersion time is 20-30min.
[0017] The preparation method of the modified ball mill agent of the embodiment is as follows: The nano-silicon dioxide is mixed in sufficient hydrochloric acid solution, and then washed with water and dried. The dried nano-silicon dioxide and the adjusting solution are stirred and adjusted at a weight ratio of 2:5. After stirring, the mixture is washed with water and dried to obtain the modified ball mill agent.
[0018] The mass fraction of the hydrochloric acid solution of the embodiment is 2-5%.
[0019] The stirring speed of the stirring and adjusting treatment of the embodiment is 450-500r / min, and the stirring time is 10-20min.
[0020] The preparation method of the adjusting solution of the embodiment is as follows: The bentonite is first heat-treated at 210-220℃ for 5-10min, and then cooled to 55℃ at a rate of 1-3℃ / min, and kept for 5-10min. After the keeping, 3-5 parts of the kept bentonite, 1-3 parts of a chitosan solution, 2-5 parts of sodium dodecyl benzene sulfonate, and 4-7 parts of a yttrium nitrate solution are fully blended to obtain the adjusting solution.
[0021] The mass fraction of the chitosan solution of the embodiment is 2-5%; the mass fraction of the yttrium nitrate solution is 1-4%.
[0022] The high-thermal-conductivity alumina powder prepared by the preparation method of the high-thermal-conductivity alumina powder of the embodiment.
[0023] Embodiment 1. The preparation method of the high-stability alumina powder of the embodiment comprises the following steps Step one: irradiating the alumina in a proton irradiation box for irradiation treatment, and obtaining irradiated alumina after the irradiation; Step two: immersing the irradiated alumina in sufficient lanthanum nitrate solution for immersion treatment, and obtaining immersed alumina agent after filtration and drying; Step three: ball-milling the immersed alumina agent and the modified ball mill agent at a weight ratio of 5:2 for modification treatment, and obtaining high-thermal-conductivity alumina powder after ball-milling at a speed of 1000r / min for 2h, washing with water, and drying.
[0024] The irradiation power of the irradiation treatment of the embodiment is 350W, and the irradiation time is 5min.
[0025] The mass fraction of the lanthanum nitrate solution of the embodiment is 2%; the immersion power of the immersion treatment is 350W, and the immersion time is 20min.
[0026] The preparation method of the modified ball mill agent of the embodiment is as follows: The nano-silicon dioxide is first mixed in sufficient hydrochloric acid solution, and then washed with water and dried. The dried nano-silicon dioxide and the adjusting solution are stirred and adjusted at a weight ratio of 2:5. After stirring, the mixture is washed with water and dried to obtain the modified ball mill agent.
[0027] The mass fraction of the hydrochloric acid solution of the embodiment is 2%.
[0028] The stirring speed of the stirring and adjusting treatment of the embodiment is 450r / min, and the stirring time is 10min.
[0029] The preparation method of the adjusting solution of the embodiment is as follows: The bentonite is first heat-treated at 210℃ for 5min, then cooled to 55℃ at a rate of 1℃ / min, and kept for 5min. After the keeping, 3 parts of the kept bentonite, 1 part of chitosan solution, 2 parts of sodium dodecyl benzene sulfonate, and 4 parts of yttrium nitrate solution are fully blended to obtain the adjusting solution.
[0030] The mass fraction of the chitosan solution of the embodiment is 2%, and the mass fraction of the yttrium nitrate solution is 1%.
[0031] The high-thermal-conductivity aluminum oxide powder of the embodiment is prepared by the preparation method of the high-thermal-conductivity aluminum oxide powder.
[0032] Embodiment 2. The preparation method of the high-stability aluminum oxide powder of the embodiment comprises the following steps Step one: the aluminum oxide is first irradiated in a proton irradiation box, and then irradiated to obtain irradiated aluminum oxide; Step two: the irradiated aluminum oxide is immersed in sufficient lanthanum nitrate solution for immersion treatment, and then filtered and dried to obtain an immersion aluminum oxide agent; Step three: the immersion aluminum oxide agent and the modified ball mill agent are ball-milled and modified at a weight ratio of 5:2, the ball-milling and modifying speed is 1500r / min, the ball-milling time is 2h, and then the mixture is washed with water and dried to obtain the high-thermal-conductivity aluminum oxide powder.
[0033] The irradiation power of the irradiation treatment of the embodiment is 400W, and the irradiation time is 10min.
[0034] The mass fraction of the lanthanum nitrate solution of the embodiment is 5%; the immersion power of the immersion treatment is 400W, and the immersion time is 30min.
[0035] The preparation method of the modified ball mill agent of the embodiment is as follows: The nano-silica is mixed in a sufficient amount of hydrochloric acid solution, then washed with water and dried, the dried nano-silica and the adjusting solution are stirred and adjusted at a weight ratio of 2:5, after stirring, the mixture is washed with water and dried to obtain the modified ball mill agent.
[0036] The mass fraction of the hydrochloric acid solution of the embodiment is 5%.
[0037] The stirring speed of the stirring and adjusting treatment of the embodiment is 500 r / min, and the stirring time is 20 min.
[0038] The preparation method of the adjusting solution of the embodiment is as follows: The bentonite is first heat treated at 220℃ for 10 min, then cooled to 55℃ at a rate of 3℃ / min, and kept for 10 min, after the keeping, 5 parts of the kept bentonite, 3 parts of a chitosan solution, 5 parts of sodium dodecyl benzene sulfonate and 7 parts of a yttrium nitrate solution are fully blended to obtain the adjusting solution.
[0039] The mass fraction of the chitosan solution of the embodiment is 5%, and the mass fraction of the yttrium nitrate solution is 4%.
[0040] The high-thermal-conductivity alumina powder of the embodiment is prepared by the preparation method of the high-thermal-conductivity alumina powder.
[0041] Embodiment 3. The preparation method of the high-stability alumina powder of the embodiment comprises the following steps Step one: the alumina is first irradiated in a proton irradiation box, and after irradiation, irradiated alumina is obtained; Step two: the irradiated alumina is immersed in a sufficient amount of lanthanum nitrate solution for immersion treatment, after immersion, the mixture is filtered and dried to obtain an immersed alumina agent; Step three: the immersed alumina agent and the modified ball mill agent are ball-milled at a weight ratio of 5:2, the ball-milling speed is 1250 r / min, the ball-milling time is 2 h, after ball-milling, the mixture is washed with water and dried to obtain the high-thermal-conductivity alumina powder.
[0042] The irradiation power of the irradiation treatment of the embodiment is 370 W, and the irradiation time is 7.5 min.
[0043] The mass fraction of the lanthanum nitrate solution of the embodiment is 3.5%, and the immersion power of the immersion treatment is 370 W, and the immersion time is 25 min.
[0044] The preparation method of the modified ball mill agent of the embodiment is as follows: The nano-silicon dioxide is mixed in sufficient hydrochloric acid solution, washed with water and dried, the dried nano-silicon dioxide and the adjusting solution are stirred and adjusted according to a weight ratio of 2:5, washed with water and dried to obtain the modified ball mill agent.
[0045] The mass fraction of the hydrochloric acid solution in this embodiment is 3.5%.
[0046] The stirring speed of the stirring and adjusting treatment in this embodiment is 470 r / min, and the stirring time is 15 min.
[0047] The preparation method of the adjusting solution in this embodiment is as follows: The bentonite is first heat treated at 215℃ for 7.5 min, then cooled to 55℃ at a rate of 2℃ / min, and kept for 7.5 min, then 4 parts of the kept bentonite, 2 parts of chitosan solution, 3.5 parts of sodium dodecyl benzene sulfonate and 5.5 parts of yttrium nitrate solution are fully blended to obtain the adjusting solution.
[0048] The mass fraction of the chitosan solution in this embodiment is 3.5%, and the mass fraction of the yttrium nitrate solution is 2.5%.
[0049] The high-thermal-conductivity alumina powder is prepared by the preparation method of the high-thermal-conductivity alumina powder in this embodiment.
[0050] Embodiment 4. The preparation method of the high-stability alumina powder in this embodiment comprises the following steps Step one: the alumina is first irradiated in a proton irradiation box, and the irradiated alumina is obtained after irradiation; Step two: the irradiated alumina is immersed in sufficient lanthanum nitrate solution for immersion treatment, and then filtered and dried to obtain the immersed alumina agent; Step three: the immersed alumina agent and the modified ball mill agent are ball-milled and modified according to a weight ratio of 5:2, the ball-milling and modifying speed is 1200 r / min, the ball-milling time is 2 h, and then washed with water and dried to obtain the high-thermal-conductivity alumina powder.
[0051] The irradiation power of the irradiation treatment in this embodiment is 360 W, and the irradiation time is 7 min.
[0052] The mass fraction of the lanthanum nitrate solution in this embodiment is 3%, and the immersion power of the immersion treatment is 360 W, and the immersion time is 22 min.
[0053] The preparation method of the modified ball mill agent in this embodiment is as follows: The nano-silicon dioxide is mixed in sufficient hydrochloric acid solution, washed with water and dried, the dried nano-silicon dioxide and the adjusting solution are stirred and adjusted according to a weight ratio of 2:5, washed with water and dried to obtain the modified ball mill agent.
[0054] The mass fraction of the hydrochloric acid solution of the embodiment is 3%.
[0055] The stirring speed of the stirring adjustment treatment of the embodiment is 460 r / min, and the stirring time is 12 min.
[0056] The preparation method of the adjustment liquid of the embodiment is as follows: The bentonite is first heat-treated at 212℃ for 6 min, then cooled to 55℃ at a rate of 2℃ / min, and kept for 6 min. After the end of the keeping, 4 parts of the kept bentonite, 2 parts of the chitosan solution, 3 parts of sodium dodecyl benzene sulfonate, and 5 parts of the yttrium nitrate solution are fully blended to obtain the adjustment liquid.
[0057] The mass fraction of the chitosan solution of the embodiment is 3%; and the mass fraction of the yttrium nitrate solution is 2%.
[0058] The high-thermal-conductivity alumina powder of the embodiment is prepared by the preparation method of the high-thermal-conductivity alumina powder.
[0059] Comparative Example 1. Different from Example 3 is that the yttrium nitrate solution is not used for immersion treatment.
[0060] Comparative Example 2. Different from Example 3 is that the modified ball mill agent is not used for treatment.
[0061] Comparative Example 3. Different from Example 3 is that the modification method of the modified ball mill agent is different; and the adjustment liquid is not added for treatment.
[0062] Comparative Example 4. Different from Example 3 is that the chitosan solution, the sodium dodecyl benzene sulfonate, and the yttrium nitrate solution are not added to the adjustment liquid for ball mill treatment.
[0063] The thermal conductivity of the alumina of the products of Examples 1-4 and Comparative Examples 1-4 (in the measurement, the product is pressed into a shape, the pressing pressure is 10 MPa, the pressing time is 1 h, then sintering treatment is performed, the sintering temperature is 350℃, the sintering time is 1 h, and finally the thermal conductivity is tested) is as follows:
[0064] It can be seen from the comparative examples 1-4 and the example 3 that the product of the example 3 has excellent acid corrosion stability, and the product still has excellent acid corrosion resistance under different degrees of acid corrosion conditions, the product is not treated by immersing in lanthanum nitrate solution, and is not treated by the modified ball mill agent, the acid corrosion stability effect of the product is significantly deteriorated, and the modification methods of the modified ball mill agent are different; the product performance has a deteriorating trend without adding the adjusting liquid treatment, adding the chitosan solution, sodium dodecyl benzene sulfonate and yttrium nitrate solution ball milling treatment in the adjusting liquid, and only the product raw material obtained by the method of the application has the most significant performance effect.
[0065] It will be obvious to a person skilled in the art that, without departing from the spirit or essential characteristics of the application, the present application can be carried out in other specific forms than those described and exemplified herein. Thus, the present examples are to be considered in all respects as illustrative and not restrictive, and the scope of the application is indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalents are intended to be embraced therein.
[0066] Furthermore, it should be understood that although the description is made according to the embodiments, not every embodiment contains only one independent technical solution, and the description is made in this way only for the sake of clarity, and a person skilled in the art should consider the description as a whole, and the technical solutions in each embodiment can also be combined appropriately to form other embodiments that can be understood by a person skilled in the art.
Claims
1. A method for preparing highly stable alumina powder, characterized in that: The following steps are involved: Step 1: irradiating the alumina in a proton irradiation box, and obtaining irradiated alumina after the irradiation is completed; Step 2: Immersing the irradiated alumina into a sufficient amount of lanthanum nitrate solution for immersion treatment, filtering and drying after the immersion is completed to obtain an immersion alumina agent; Step 3: ball mill the immersed alumina agent and modified ball milling agent according to a weight ratio of 5:2, the ball milling speed is 1000-1500r / min, and the ball milling is carried out for 2h. After the ball milling is completed, the powder is washed with water and dried to obtain high thermal conductivity alumina powder.
2. The method for preparing a highly stable alumina powder according to claim 1, wherein: The irradiation power of the irradiation treatment is 350-400W, and the irradiation time is 5-10 minutes.
3. The method for preparing a highly stable alumina powder according to claim 1, wherein: The mass fraction of the lanthanum nitrate solution is 2-5%; the immersion power of the immersion treatment is 350-400W, and the immersion time is 20-30 minutes.
4. The method for preparing a highly stable alumina powder according to claim 1, wherein: The preparation method of the modified ball mill is as follows: The nano-silica is first mixed thoroughly with a sufficient amount of hydrochloric acid solution, then washed with water and dried. The dried nano-silica and the regulating liquid are stirred and regulated in a weight ratio of 2:
5. After stirring, the mixture is washed with water and dried to obtain a modified ball mill.
5. The method for preparing a highly stable alumina powder according to claim 4, wherein: The mass fraction of the hydrochloric acid solution is 2-5%.
6. The method for preparing a highly stable alumina powder according to claim 4, wherein: The stirring speed of the stirring adjustment process is 450-500 r / min, and the stirring time is 10-20 min.
7. The method for preparing a highly stable alumina powder according to claim 4, wherein: The preparation method of the regulating solution is: The bentonite is first heat-treated at 210-220°C for 5-10 minutes, then cooled to 55°C at a rate of 1-3°C / min and kept warm for 5-10 minutes. After the insulation is completed, 3-5 parts of the insulated bentonite, 1-3 parts of chitosan solution, 2-5 parts of sodium dodecylbenzenesulfonate, and 4-7 parts of yttrium nitrate solution are fully blended to obtain a regulating solution.
8. The method for preparing a highly stable alumina powder according to claim 7, characterized in that: The mass fraction of the chitosan solution is 2-5%; the mass fraction of the yttrium nitrate solution is 1-4%.