Silica micropowder composite powder and preparation method thereof

Abstract

The invention relates to the technical field of building materials, in particular to silica powder composite powder and a preparation method thereof. The composite material comprises the following raw materials in parts by weight: 80-90 parts of silica powder, 2-10 parts of a silane coupling agent, 5-12 parts of nano oxide and 1-5 parts of a dispersing agent. The invention provides the composite powder capable of improving the dispersity of the silica powder and improving the compatibility of the silica powder and a matrix material, and the composite powder has important significance for promoting the application of the silica powder in the modern industry.

Description

Technical Field

[0001] The invention relates to the technical field of building materials, and in particular to a silicon micropowder composite powder and a preparation method thereof. Background Art

[0002] In modern industry, silicon powder is widely used in building materials, electronic packaging materials, ceramic materials and other fields. Its main function is to improve the performance of materials as a filler. Silicon powder has good chemical stability, insulation and high temperature resistance, so it plays an important role in improving the mechanical strength, thermal stability and electrical insulation performance of materials.

[0003] However, due to the high surface energy of silica powder, it is easy to agglomerate, which limits its uniform dispersion in the composite material and thus affects the performance of the composite material. Summary of the invention

[0004] The present invention provides a composite powder capable of improving the dispersibility of silicon micropowder and enhancing its compatibility with a matrix material, which is of great significance for promoting the application of silicon micropowder in modern industry.

[0005] The technical scheme adopted by the present invention is: a silicon micropowder composite powder, which comprises the following raw materials by weight: silicon micropowder accounts for 80-90 parts, silane coupling agent accounts for 2-10 parts, nano oxide accounts for 5-12 parts, and dispersant accounts for 1-5 parts.

[0006] As a further improvement of the present invention, the particle size of the silicon micropowder is 0.5-10 microns.

[0007] As a further improvement of the present invention, the functional groups of the silane coupling agent contain epoxy groups, mercapto groups, and amino groups.

[0008] As a further improvement of the present invention, the nano-oxide is one or more of nano-aluminum oxide, nano-silicon oxide, nano-titanium oxide, and nano-zinc oxide.

[0009] As a further improvement of the present invention, the dispersant is one or more of sodium polyacrylate, polyvinyl alcohol, and sodium dodecyl sulfate.

[0010] A method for preparing a silicon micropowder composite powder comprises the following steps:

[0011] Step 1: Weigh the raw materials according to the above weight parts, mix the silicon micropowder and the silane coupling agent, and stir at a temperature of 80-120°C to make the silane coupling agent evenly adhere to the surface of the silicon micropowder;

[0012] Step 2: Add nano oxide and dispersant to the mixture obtained in step 1, and continue stirring until it is completely mixed;

[0013] Step 3: treating the mixture obtained in step 2 with ultrasound, the ultrasound frequency is 20-50kHz, and the treatment time is 10-60 minutes;

[0014] Step 4: Dry the mixture obtained in step 3 under vacuum conditions to finally obtain silicon micropowder composite powder.

[0015] As a further improvement of the present invention, the stirring speed in step 1 is 500-1000 rpm, and the stirring time is 1-3 hours.

[0016] As a further improvement of the present invention, the stirring speed in step 2 is 300-800 rpm, and the stirring time is 0.5-2 hours.

[0017] As a further improvement of the present invention, the ultrasonic treatment in step three is performed in an intermittent manner, with each treatment time being 10-30 minutes, an interval time being 5-15 minutes, and the number of treatments being 3-5 times.

[0018] As a further improvement of the present invention, the drying treatment in step 4 is carried out using a vacuum rotary evaporator, and the vacuum degree is controlled at 0.05-0.1 MPa, the drying speed is 10-30 rpm, the drying temperature is 100-150°C, and the drying time is 8-24 hours.

[0019] The beneficial effects of the present invention are as follows: (1) The present invention successfully prepares a silicon micropowder composite powder through a specific raw material ratio and preparation steps. The powder has excellent dispersibility and compatibility with the matrix material, effectively solving the problem of easy agglomeration of silicon micropowder, thereby improving the overall performance of the composite material.

[0020] (2) The preparation method of the present invention is simple and efficient, the process parameters are easy to control, and it is easy to realize industrial production. In addition, the entire preparation process is environmentally friendly and meets the requirements of sustainable development.

[0021] (3) The silicon micropowder composite powder prepared by the present invention has outstanding performance in improving the mechanical strength, thermal stability and electrical insulation performance of the material, and is particularly suitable for the fields of building materials, electronic packaging materials and ceramic materials, and has broad market application prospects. DETAILED DESCRIPTION

[0022] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present application more clearly understood, the present application is further described in detail below in conjunction with the embodiments. It should be understood that the embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0023] The invention provides a silicon micropowder composite powder, which comprises the following raw materials by weight: 80-90 parts of silicon micropowder, 2-10 parts of silane coupling agent, 5-12 parts of nano oxide and 1-5 parts of dispersant.

[0024] The particle size of the silicon micropowder in the present invention is 0.5-10 microns. The functional groups of the silane coupling agent include epoxy, mercapto and amino groups. The nano oxide is one or more of nano aluminum oxide, nano silicon oxide, nano titanium oxide and nano zinc oxide. The dispersant is one or more of sodium polyacrylate, polyvinyl alcohol and sodium dodecyl sulfate.

[0025] A method for preparing a silicon micropowder composite powder comprises the following steps:

[0026] Step 1: weigh the raw materials according to the above weight parts, mix the silicon micropowder and the silane coupling agent, and stir at a temperature of 80-120° C. to make the silane coupling agent evenly adhere to the surface of the silicon micropowder, wherein the stirring speed is 500-1000 rpm and the stirring time is 1-3 hours;

[0027] Step 2: Add nano oxide and dispersant to the mixture obtained in step 1, and continue stirring until it is completely mixed, wherein the stirring speed is 300-800 rpm and the stirring time is 0.5-2 hours;

[0028] Step 3: treating the mixture obtained in step 2 with ultrasound, the ultrasound frequency is 20-50kHz, the treatment time is 10-60 minutes, wherein the ultrasound treatment is intermittent treatment, each treatment time is 10-30 minutes, the interval time is 5-15 minutes, and the number of treatments is 3-5 times;

[0029] Step 4: Dry the mixture obtained in step 3 under vacuum conditions to finally obtain a silicon micropowder composite powder, wherein the drying process is carried out using a vacuum rotary evaporator, the vacuum degree is controlled to be 0.05-0.1MPa during the drying process, the drying speed is 10-30 rpm, the drying temperature is 100-150°C, and the drying time is 8-24 hours.

[0030] Embodiment 1:

[0031] This embodiment provides a method for preparing a silicon micropowder composite powder, wherein 85 parts of silicon micropowder, 5 parts of a silane coupling agent, 7 parts of nano-alumina, and 3 parts of sodium polyacrylate are weighed, and the specific steps are as follows.

[0032] (i) placing silicon micropowder and silane coupling agent into a mixer, setting the temperature to 100° C., stirring at a speed of 750 rpm, and continuing stirring for 2 hours to ensure that the silane coupling agent is evenly covered on the surface of the silicon micropowder;

[0033] (ii) adding nano-alumina and sodium polyacrylate to the mixture, and continuing stirring at a speed of 500 rpm for 1 hour until all ingredients are completely mixed;

[0034] (iii) placing the mixture in an ultrasonic cleaner, setting the frequency to 30 kHz, using an intermittent treatment method, treating for 20 minutes each time, with an interval of 10 minutes, for a total of 4 times;

[0035] (iv) placing the treated mixture into a vacuum rotary evaporator for drying, controlling the vacuum degree at 0.08 MPa, the drying speed at 20 rpm, the temperature at 120° C., and the drying time for 16 hours to obtain a silicon micropowder composite powder.

[0036] Through the above steps, the successfully prepared silicon micropowder composite powder has good dispersibility and excellent compatibility, and its particle size distribution is uniform, the surface is smooth, and there is no obvious agglomeration phenomenon.

[0037] Embodiment 2:

[0038] This embodiment provides a method for preparing a silicon micropowder composite powder, which includes weighing 82 parts of silicon micropowder, 3 parts of a silane coupling agent, 10 parts of nano silicon oxide, and 2 parts of polyvinyl alcohol. The specific steps are as follows.

[0039] (i) placing silicon micropowder and silane coupling agent into a mixer, setting the temperature to 90° C., stirring at a speed of 600 rpm, and continuing stirring for 1.5 hours to ensure that the silane coupling agent is evenly covered on the surface of the silicon micropowder;

[0040] (ii) adding nano-silicon oxide and polyvinyl alcohol to the mixture, continuing to stir, adjusting the speed to 400 rpm, stirring for 1 hour, until all the ingredients are completely mixed; (iii) placing the mixture in an ultrasonic cleaner, setting the frequency to 40 kHz, using an intermittent treatment method, each treatment lasting 15 minutes, with an interval of 5 minutes, for a total of 5 treatments;

[0041] (iv) placing the treated mixture into a vacuum rotary evaporator for drying, with the vacuum degree controlled at 0.07 MPa, the drying speed at 15 rpm, the temperature set at 130° C., and the drying time at 12 hours to obtain a silicon micropowder composite powder.

[0042] Through the above steps, the successfully prepared silicon micropowder composite powder has good dispersibility and excellent compatibility, and its particle size distribution is uniform, the surface is smooth, and there is no obvious agglomeration phenomenon.

[0043] Embodiment 3:

[0044] This embodiment provides a method for preparing a silicon micropowder composite powder. 88 parts of silicon micropowder, 4 parts of silane coupling agent, 8 parts of nano-titanium oxide, and 1 part of sodium dodecyl sulfate are weighed. The specific steps are as follows.

[0045] (i) placing silicon micropowder and silane coupling agent into a mixer, setting the temperature to 110° C., stirring at a speed of 800 rpm, and continuing stirring for 1.8 hours to ensure that the silane coupling agent is evenly covered on the surface of the silicon micropowder;

[0046] (ii) adding nano titanium oxide and sodium dodecyl sulfate to the mixture and continuing stirring at a speed of 600 rpm for 1.2 hours until all ingredients are completely mixed;

[0047] (iii) placing the mixture in an ultrasonic cleaner, setting the frequency to 50 kHz, using an intermittent treatment method, treating for 25 minutes each time, with an interval of 12 minutes, for a total of 4 times;

[0048] (iv) placing the treated mixture into a vacuum rotary evaporator for drying, controlling the vacuum degree at 0.09 MPa, the drying speed at 25 rpm, the temperature at 140° C., and the drying time for 20 hours to obtain a silicon micropowder composite powder.

[0049] Through the above steps, the successfully prepared silicon micropowder composite powder has good dispersibility and excellent compatibility, and its particle size distribution is uniform, the surface is smooth, and there is no obvious agglomeration phenomenon.

[0050] Performance Testing

[0051] The silicon micropowder composite powders obtained in the above Examples 1-3 were subjected to performance tests, including performance in terms of dispersibility, mechanical strength, thermal stability, and electrical insulation performance.

[0052] (I) Dispersion test: The particle size distribution of the silica powder composite was measured using a laser particle size analyzer.

[0053] (ii) Mechanical strength test: A universal material testing machine is used to perform tensile strength and flexural strength tests on the composite material containing silicon micropowder composite powder.

[0054] (III) Thermal stability test: The thermal stability of the silicon micropowder composite powder was tested using a thermogravimetric analyzer (TGA) to record its weight changes at different temperatures.

[0055] (IV) Electrical insulation performance test: Use a dielectric constant tester to measure the dielectric constant of the silicon micropowder composite powder.

[0056] The results of the above tests are shown in the following table.

[0057]

[0058]

[0059] In summary, the silicon micropowder composite powder provided by the present invention exhibits excellent performance in terms of dispersibility, mechanical strength, thermal stability and electrical insulation performance. In particular, through specific raw material ratios and preparation steps, the problem of easy agglomeration of silicon micropowder is successfully solved, and the overall performance of the composite material is significantly improved. This technology has broad market application prospects and is particularly suitable for the fields of building materials, electronic packaging materials and ceramic materials.

[0060] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some of the technical features thereof may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A silicon micropowder composite powder, characterized in that: The raw materials include the following by weight: 80-90 parts of silicon micropowder, 2-10 parts of silane coupling agent, 5-12 parts of nano oxide and 1-5 parts of dispersant.

2. The silicon micropowder composite powder according to claim 1, characterized in that: The particle size of the silicon micropowder is 0.5-10 microns.

3. The silicon micropowder composite powder according to claim 1, characterized in that: The functional groups of the silane coupling agent include epoxy group, mercapto group and amino group.

4. The silicon micropowder composite powder according to claim 1, characterized in that: The nano-oxide is one or more of nano-aluminum oxide, nano-silicon oxide, nano-titanium oxide, and nano-zinc oxide.

5. The silicon micropowder composite powder according to claim 1, characterized in that: The dispersant is one or more of sodium polyacrylate, polyvinyl alcohol and sodium dodecyl sulfate.

6. A method for preparing a silicon micropowder composite powder, characterized in that: The following steps are involved: Step 1: Weigh the raw materials according to the above weight parts, mix the silicon micropowder and the silane coupling agent, and stir at a temperature of 80-120°C to make the silane coupling agent evenly adhere to the surface of the silicon micropowder; Step 2: Add nano oxide and dispersant to the mixture obtained in step 1, and continue stirring until it is completely mixed; Step 3: treating the mixture obtained in step 2 with ultrasound, the ultrasound frequency is 20-50kHz, and the treatment time is 10-60 minutes; Step 4: Dry the mixture obtained in step 3 under vacuum conditions to finally obtain silicon micropowder composite powder.

7. The method for preparing a silicon micropowder composite powder according to claim 6, characterized in that: The stirring speed in the step 1 is 500-1000 rpm, and the stirring time is 1-3 hours.

8. The method for preparing a silicon micropowder composite powder according to claim 6, characterized in that: The stirring speed in the step 2 is 300-800 rpm, and the stirring time is 0.5-2 hours.

9. The method for preparing a silicon micropowder composite powder according to claim 6, characterized in that: The ultrasonic treatment in step 3 is performed in an intermittent manner, with each treatment lasting 10-30 minutes, an interval of 5-15 minutes, and 3-5 treatments.

10. The method for preparing a silicon micropowder composite powder according to claim 6, characterized in that: The drying treatment in step 4 is carried out using a vacuum rotary evaporator. During the drying process, the vacuum degree is controlled to be 0.05-0.1 MPa, the drying speed is 10-30 rpm, the drying temperature is 100-150° C., and the drying time is 8-24 hours.

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