CN113636529B - Preparation method of boron nitride and aluminum oxide heat conduction filler - Google Patents

Preparation method of boron nitride and aluminum oxide heat conduction filler Download PDF

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CN113636529B
CN113636529B CN202110803074.9A CN202110803074A CN113636529B CN 113636529 B CN113636529 B CN 113636529B CN 202110803074 A CN202110803074 A CN 202110803074A CN 113636529 B CN113636529 B CN 113636529B
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焦华
周雪蕊
赵康
靳洁晨
张鑫媛
汤玉斐
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Xian University of Technology
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Abstract

The invention discloses a preparation method of boron nitride and aluminum oxide heat-conducting filler, which comprises the steps of firstly freezing and thawing BN powder, and then adding the BN powder into a dopamine solution for dark reaction to obtain a BN solution system; secondly, preparing Al under the action of chelating agent and alkaline solution 2 O 3 A precursor solution system; al to be prepared 2 O 3 The precursor solution system and BN solution are stirred and mixed uniformly, and BN.Al is used as the precursor 2 O 3 Fixing the precursor form, ball milling, washing and drying, and calcining the obtained precursor powder at high temperature under the protection of inert gas to obtain the boron nitride-aluminum oxide heat-conducting filler. The method has the advantages of low cost, simplicity, easiness, good repeatability, high performance of the synthesized boron nitride-aluminum oxide heat conduction filler and good stability, is suitable for mass production, and can promote the commercialization process of the heat conduction powder material.

Description

Preparation method of boron nitride and aluminum oxide heat conduction filler
Technical Field
The invention relates to the technical field of heat-conducting powder materials, in particular to a preparation method of a boron nitride and aluminum oxide heat-conducting filler.
Background
With the rapid development of microelectronics technologies, electronic components are widely used in the electronics industry. In recent years, electronic components tend to be miniaturized and densely packed, so that heat generated by electronic products is greatly increased. The heat of the electronic component should be dissipated in time during the use process, otherwise the working temperature of the electronic component is raised, which poses serious threat to the stability and reliability of the electronic component, and even shortens the service life of the electronic component. Therefore, on the premise of ensuring the reliability of electronic components, the improvement of the heat dissipation capacity and the reduction of the production cost are the general targets of the design and the assembly of the current electronic products.
The polymer material has good plasticity and insulativity, but has poor heat conduction performance; boron Nitride (BN), silicon carbide (SiC), aluminum oxide (Al 2 O 3 ) The ceramic material has good thermal conductivity and insulativity, but has poor plasticity; the polymer-ceramic composite material can integrate the advantages of the two materials, overcomes the defect of a single material, and has high heat conductivity, good insulating property, good plasticity and good corrosion resistance. The ceramic heat conducting material is filled in the polymer matrix to form the composite material, and the heat conducting performance of the composite material is mainly determined by the ceramic filler. Filling ceramic materials with high thermal conductivity into a polymer matrix is the most common method for improving the thermal conductivity of the composite material at present.
Alumina has a series of excellent characteristics of high strength, acid and alkali corrosion resistance, high adsorption capacity, electric insulation and the like, but has low heat conductivity coefficient, and can not meet the use requirement of the heat conducting material for electronic packaging. Boron nitride with high thermal conductivity is a research hotspot for novel thermal conductive materials. Therefore, the preparation of the boron nitride-aluminum oxide heat-conducting filler is a necessary way for developing a novel heat-conducting filler.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a preparation method of a boron nitride and aluminum oxide heat conduction filler.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: a preparation method of a boron nitride and alumina heat-conducting filler comprises the following steps:
step 1, performing freeze thawing treatment on boron nitride powder;
step 2, preparing a dopamine solution: weighing 54mL of Tris-HCl tris-hydroxymethyl aminomethane hydrochloride solution, adding the solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding the solution into the beaker, weighing 0.03g of dopamine hydrochloride in the beaker, and uniformly stirring to obtain a dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2 for dark reaction, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 Adding into a beaker, adding 100mL of deionized water, stirring until the deionized water is completely dissolved to obtain Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 10-20g of NaOH powder, dissolving the weighed NaOH powder into 50mL of deionized water for a plurality of times, and uniformly stirring to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring, adding the alkaline solution obtained in step 6, and stirring to obtain white turbid liquid (Al) 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, and uniformly stirring to obtain a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high-temperature furnace and calcined at high temperature under the protection of inert gas, so that the boron nitride-aluminum oxide lamellar structure can be obtained.
Preferably, the number of freezing and thawing times in the step 1 is set to 10, the freezing is carried out for 24 hours, the thawing is carried out for 12 hours, and the freezing temperature is-20 ℃;
preferably, the preparation process of the Tris-HCl Tris (hydroxymethyl) aminomethane hydrochloride solution in the step 2 is as follows: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl Tris hydrochloride solution;
preferably, the dark reaction time of the step 3 is 12-24 hours;
preferably, the stirring process in the steps 2, 3, 4, 5, 6, 7 and 8 is performed by using a magnetic stirrer, and the stirring time is 5-60min;
preferably, the NaOH powder is added into the deionized water in the step 6 for 5-10 times.
Preferably, the mechanical ball milling time in the step 9 is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60deg.C for 24-48 hr.
Preferably, in the step 10, ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
(III) beneficial effects
The invention provides a preparation method of a boron nitride and alumina heat conduction filler. The beneficial effects are as follows:
the method comprises the steps of firstly, freezing and thawing BN powder, and then adding the BN powder into a dopamine solution for dark reaction to obtain a BN solution system; secondly, preparing Al under the action of chelating agent and alkaline solution 2 O 3 A precursor solution system; al to be prepared 2 O 3 The precursor solution system and BN solution are stirred and mixed uniformly, and BN.Al is used as the precursor 2 O 3 Fixing the precursor form, ball milling, washing and drying, and calcining the obtained precursor powder at high temperature under the protection of inert gas to obtain the boron nitride-aluminum oxide heat-conducting filler. The method has the advantages of low cost, simplicity, easy implementation, good repeatability, high performance of the synthesized boron nitride-aluminum oxide heat conduction filler and good stabilityIs suitable for mass production and can promote the commercialization process of the heat-conducting powder material.
Drawings
Fig. 1 is a flow chart of a preparation process of a boron nitride-aluminum oxide heat-conducting filler provided by the invention.
FIG. 2 is an X-ray diffraction pattern of the boron nitride-alumina heat conductive filler prepared in example 3 of the present invention.
FIG. 3 is a scanning electron microscope image of the boron nitride-alumina heat conductive filler prepared in example 3 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method and the flow of the boron nitride-aluminum oxide heat-conducting filler are shown in the process flow chart of fig. 1, and the specific operation steps are as follows:
step 1, performing freeze thawing treatment on boron nitride powder, wherein the number of freeze thawing times is set to 10, the freezing time is 24 hours, the thawing time is 12 hours, and the freezing temperature is-20 ℃;
step 2, preparing a dopamine solution: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl solution; weighing 54mLTris-HCl solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding, weighing 0.03g of dopamine hydrochloride, and stirring for 5-15min to obtain dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2, and performing dark reaction for 12-24 hours, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 In a beaker, 100mL of deionized water was added and stirred using a magnetic stirrer for 10-20min until complete dissolution to give Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water, and stirring for 5-15min by using a magnetic stirrer until the chelating agent is completely dissolved to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 10-20g of NaOH powder, dissolving the weighed NaOH powder in 50mL of deionized water for 5-10 times, and stirring for 20min by using a magnetic stirrer until the NaOH powder is completely dissolved to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring with a magnetic stirrer for 15-30min until completely dissolved, adding the alkaline solution obtained in step 6, and stirring with a magnetic stirrer for 15-30min to obtain white turbid liquid, which is Al 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, stirring for 1h by using a magnetic stirrer until the system is uniform, and marking as a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder. Wherein the time of mechanical ball milling is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60 ℃ for 24-48h;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high-temperature furnace and calcined at high temperature under the protection of inert gas, so that the boron nitride-aluminum oxide lamellar structure can be obtained. Wherein Ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
Example 1:
step 1, performing freeze thawing treatment on boron nitride powder, wherein the number of freeze thawing times is set to 10, the freezing time is 24 hours, the thawing time is 12 hours, and the freezing temperature is-20 ℃;
step 2, preparing a dopamine solution: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl solution; weighing 54mLTris-HCl solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding, weighing 0.03g of dopamine hydrochloride, and stirring for 5min to obtain a dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2, and carrying out dark reaction for 12 hours, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 In a beaker, 100mL of deionized water was added and stirred using a magnetic stirrer for 10min until complete dissolution to give Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water, and stirring for 5min by using a magnetic stirrer until the chelating agent is completely dissolved to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 16g of NaOH powder, dissolving the weighed NaOH powder in 50mL of deionized water for 8 times, and stirring for 20min by using a magnetic stirrer until the NaOH powder is completely dissolved to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring with a magnetic stirrer for 15min to completely dissolve, adding the alkaline solution obtained in step 6, and stirring with a magnetic stirrer for 15min to obtain white turbid liquid, which is Al 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, stirring for 1h by using a magnetic stirrer until the system is uniform, and marking as a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder. Wherein the time of mechanical ball milling is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60 ℃ for 24 hours;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high-temperature furnace and calcined at high temperature under the protection of inert gas, so that the boron nitride-aluminum oxide lamellar structure can be obtained. Wherein Ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
Example 2:
step 1, performing freeze thawing treatment on boron nitride powder, wherein the number of freeze thawing times is set to 10, the freezing time is 24 hours, the thawing time is 12 hours, and the freezing temperature is-20 ℃;
step 2, preparing a dopamine solution: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl solution; weighing 54mLTris-HCl solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding, weighing 0.03g of dopamine hydrochloride, and stirring for 10min to obtain a dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2, and carrying out dark reaction for 12 hours, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 In a beaker, 100mL of deionized water was added and stirred using a magnetic stirrer for 15min until complete dissolution to give Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water, and stirring for 10min by using a magnetic stirrer until the chelating agent is completely dissolved to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 18g of NaOH powder, dissolving the weighed NaOH powder in 50mL of deionized water for 8 times, and stirring for 20min by using a magnetic stirrer until the NaOH powder is completely dissolved to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring with a magnetic stirrer for 20min to completely dissolve, adding the alkaline solution obtained in step 6, and stirring with a magnetic stirrer for 20min to obtain white turbid liquid, which is Al 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, stirring for 1h by using a magnetic stirrer until the system is uniform, and marking as a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder. Wherein the time of mechanical ball milling is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60 ℃ for 24 hours;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high-temperature furnace and calcined at high temperature under the protection of inert gas, so that the boron nitride-aluminum oxide lamellar structure can be obtained. Wherein Ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
Example 3:
step 1, performing freeze thawing treatment on boron nitride powder, wherein the number of freeze thawing times is set to 10, the freezing time is 24 hours, the thawing time is 12 hours, and the freezing temperature is-20 ℃;
step 2, preparing a dopamine solution: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl solution; weighing 54mLTris-HCl solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding, weighing 0.03g of dopamine hydrochloride, and stirring for 15min to obtain a dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2, and carrying out dark reaction for 12 hours, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 In a beaker, 100mL of deionized water was added and stirred using a magnetic stirrer for 20min until complete dissolution to give Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water, and stirring for 15min by using a magnetic stirrer until the chelating agent is completely dissolved to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 20g of NaOH powder, dissolving the weighed NaOH powder in 50mL of deionized water for 8 times, and stirring for 20min by using a magnetic stirrer until the NaOH powder is completely dissolved to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring with a magnetic stirrer for 30min to completely dissolve, adding the alkaline solution obtained in step 6, and stirring with a magnetic stirrer for 30min to obtain white turbid liquid, which is Al 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, stirring for 1h by using a magnetic stirrer until the system is uniform, and marking as a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder. Wherein the time of mechanical ball milling is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60 ℃ for 24 hours;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high temperature furnace and inertAnd (3) calcining at high temperature under the protection of gas to obtain the boron nitride-aluminum oxide lamellar structure. Wherein Ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
Example 4:
step 1, performing freeze thawing treatment on boron nitride powder, wherein the number of freeze thawing times is set to 10, the freezing time is 24 hours, the thawing time is 12 hours, and the freezing temperature is-20 ℃;
step 2, preparing a dopamine solution: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl solution; weighing 54mLTris-HCl solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding, weighing 0.03g of dopamine hydrochloride, and stirring for 5min to obtain a dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2, and carrying out dark reaction for 24 hours, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 In a beaker, 100mL of deionized water was added and stirred using a magnetic stirrer for 10min until complete dissolution to give Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water, and stirring for 5min by using a magnetic stirrer until the chelating agent is completely dissolved to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 16g of NaOH powder, dissolving the weighed NaOH powder into 50mL of deionized water for 10 times, and stirring for 20min by using a magnetic stirrer until the NaOH powder is completely dissolved to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring with a magnetic stirrer for 15min until the alkaline solution is completely dissolved, adding the alkaline solution obtained in step 6, and continuing using magnetismStirring with a stirring machine for 15min to obtain white turbid liquid, which is Al 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, stirring for 1h by using a magnetic stirrer until the system is uniform, and marking as a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder. Wherein the time of mechanical ball milling is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60 ℃ for 48 hours;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high-temperature furnace and calcined at high temperature under the protection of inert gas, so that the boron nitride-aluminum oxide lamellar structure can be obtained. Wherein Ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
Example 5:
step 1, performing freeze thawing treatment on boron nitride powder, wherein the number of freeze thawing times is set to 10, the freezing time is 24 hours, the thawing time is 12 hours, and the freezing temperature is-20 ℃;
step 2, preparing a dopamine solution: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl solution; weighing 54mLTris-HCl solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding, weighing 0.03g of dopamine hydrochloride, and stirring for 10min to obtain a dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2, and carrying out dark reaction for 24 hours, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 In a beaker and 100mL of deionized water was added and stirred for 15mi using a magnetic stirrern to be completely dissolved to obtain Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water, and stirring for 10min by using a magnetic stirrer until the chelating agent is completely dissolved to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 18g of NaOH powder, dissolving the weighed NaOH powder into 50mL of deionized water for 10 times, and stirring for 20min by using a magnetic stirrer until the NaOH powder is completely dissolved to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring with a magnetic stirrer for 20min to completely dissolve, adding the alkaline solution obtained in step 6, and stirring with a magnetic stirrer for 20min to obtain white turbid liquid, which is Al 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, stirring for 1h by using a magnetic stirrer until the system is uniform, and marking as a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder. Wherein the time of mechanical ball milling is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60 ℃ for 48 hours;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high-temperature furnace and calcined at high temperature under the protection of inert gas, so that the boron nitride-aluminum oxide lamellar structure can be obtained. Wherein Ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
Example 6:
step 1, performing freeze thawing treatment on boron nitride powder, wherein the number of freeze thawing times is set to 10, the freezing time is 24 hours, the thawing time is 12 hours, and the freezing temperature is-20 ℃;
step 2, preparing a dopamine solution: 9.8mL of concentrated hydrochloric acid is weighed and slowly dissolved in 80mL of deionized water for multiple times, and the volume is fixed to 100mL to obtain dilute hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL of deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl solution; weighing 54mLTris-HCl solution into a beaker sealed by tinfoil, weighing 6mL of absolute ethyl alcohol, adding, weighing 0.03g of dopamine hydrochloride, and stirring for 15min to obtain a dopamine solution;
step 3, weighing 1.24g of the boron nitride powder obtained in the step 1, adding the boron nitride powder into the dopamine solution shown in the step 2, and carrying out dark reaction for 24 hours, and marking the solution as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 In a beaker, 100mL of deionized water was added and stirred using a magnetic stirrer for 20min until complete dissolution to give Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: 9.6g of citric acid (C) 6 H 8 O 7 ·H 2 O) dissolving in 20mL of deionized water, and stirring for 15min by using a magnetic stirrer until the chelating agent is completely dissolved to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 20g of NaOH powder, dissolving the weighed NaOH powder into 50mL of deionized water for 10 times, and stirring for 20min by using a magnetic stirrer until the NaOH powder is completely dissolved to obtain an alkaline solution;
step 7, adding the chelating agent solution obtained in step 5 to the Al (NO) obtained in step 4 3 ) 3 Mixing the above solutions, stirring with a magnetic stirrer for 30min to completely dissolve, adding the alkaline solution obtained in step 6, and stirring with a magnetic stirrer for 30min to obtain white turbid liquid, which is Al 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, stirring for 1h by using a magnetic stirrer until the system is uniform, and marking as a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder. Wherein the time of mechanical ball milling is 6 hours; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: drying at 60 ℃ for 48 hours;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 The precursor powder is placed in a high-temperature furnace and calcined at high temperature under the protection of inert gas, so that the boron nitride-aluminum oxide lamellar structure can be obtained. Wherein Ar is selected as inert gas, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
X-ray diffraction analysis (XRD) of the boron nitride-alumina thermally conductive filler prepared in example 3 of the present invention (as shown in FIG. 2), it can be seen from FIG. 2 that BN and Al are present in the composite material 2 O 3 The characteristic peaks of the composite material are good in crystallinity and basically have no impurity phase, so that the conclusion that the boron nitride-aluminum oxide heat-conducting filler can be successfully prepared by the method of the invention can be drawn.
The morphology of the boron nitride-aluminum oxide heat-conducting filler prepared in example 3 of the invention (shown in fig. 3) is analyzed by using a Scanning Electron Microscope (SEM), and it can be seen that small Al is contained in the composite material 2 O 3 The lamellae are coated with lamellae of large BN.
The block body obtained by compounding the boron nitride-alumina heat conduction filler and the epoxy resin is tested to have heat conduction performance, and the heat conduction coefficient is 0.62437 W.m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the Thermal conductivity of 0.43718 W.m of block obtained by compounding pure BN powder with epoxy resin -1 ·K -1 The heat conduction performance of the composite filler is improved by about 1.5 times, which indicates that the composite filler can obtain more excellent heat conduction performance.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (6)

1. The preparation method of the boron nitride and aluminum oxide heat conduction filler is characterized by comprising the following steps of:
step 1, performing freeze thawing treatment on boron nitride powder;
step 2, preparing a dopamine solution: weighing 54mLTris-HCl tris (hydroxymethyl) aminomethane hydrochloride solution, adding the solution into a beaker sealed by tinfoil, weighing 6mL absolute ethyl alcohol, adding the solution into the beaker, weighing 0.03g dopamine hydrochloride in the beaker, and uniformly stirring to obtain a dopamine solution;
step 3, weighing 1.24 and g, adding the boron nitride powder obtained in the step 1 into the dopamine solution shown in the step 2 for dark reaction, and marking as solution A;
step 4, preparing Al (NO) 3 ) 3 Solution: 37.5g of Al (NO) was weighed out 3 ) 3 Adding into beaker, adding 100mL deionized water, stirring to dissolve completely to obtain Al (NO) 3 ) 3 A solution;
step 5, preparing a chelating agent solution: weigh 9.6g citric acid (C 6 H 8 O 7 ·H 2 O) dissolving in 20mL deionized water to obtain a chelating agent solution;
step 6, preparing an alkaline solution: weighing 10-20g of NaOH powder, dissolving the weighed NaOH powder into 50mL deionized water for a plurality of times, and uniformly stirring to obtain an alkaline solution;
step (a)7 adding the chelating agent solution obtained in the step 5 to the Al (NO) obtained in the step 4 3 ) 3 Mixing the above solutions, stirring, adding the alkaline solution obtained in step 6, and stirring to obtain white turbid liquid (Al) 2 O 3 The precursor solution system is marked as solution B;
step 8, adding the solution A obtained in the step 3 into the solution B obtained in the step 7, and uniformly stirring to obtain a mixed suspension C;
step 9, mechanically ball-milling the mixed suspension solution C obtained in the step 8, centrifugally washing, and drying in an oven to obtain BN.Al 2 O 3 Precursor powder;
step 10, the BN/Al obtained in step 9 is treated 2 O 3 Placing the precursor powder in a high-temperature furnace, and calcining at high temperature under the protection of inert gas to obtain a boron nitride-aluminum oxide lamellar structure;
setting the freezing and thawing times in the step 1 to be 10 times, freezing 24-h, thawing for 12 hours, and enabling the freezing temperature to be-20 ℃;
ar is selected as inert gas in the step 10, the high-temperature calcination temperature is 1200 ℃, and the time is 120min.
2. The method for preparing the boron nitride and aluminum oxide heat-conducting filler according to claim 1, wherein the preparation process of the Tris-HCl Tris (hydroxymethyl) aminomethane hydrochloride solution in the step 2 is as follows: slowly dissolving 9.8. 9.8mL concentrated hydrochloric acid into 80mL deionized water for multiple times, and fixing the volume to 100mL to obtain diluted hydrochloric acid; weighing 0.073g of Tris in a beaker, adding 60mL deionized water, and uniformly stirring to obtain a Tris solution; dropping dilute hydrochloric acid solution into Tris solution by a dropper, and regulating the pH value of the solution to about 8.5 to obtain Tris-HCl Tris hydrochloride solution.
3. The method for preparing the boron nitride and aluminum oxide heat-conducting filler according to claim 1, wherein the dark reaction time in the step 3 is 12-24 h.
4. The method for preparing the boron nitride and aluminum oxide heat-conducting filler according to claim 1, wherein the stirring process in the steps 2, 3, 4, 5, 6, 7 and 8 is performed by using a magnetic stirrer, and the stirring time is 5-60 min.
5. The method for preparing the boron nitride and aluminum oxide heat-conducting filler according to claim 1, wherein the process of adding the NaOH powder into the deionized water in the step 6 is divided into 5-10 times.
6. The method for preparing the boron nitride and aluminum oxide heat-conducting filler according to claim 1, wherein the mechanical ball milling time in the step 9 is 6h; during centrifugal washing, ultrapure water is firstly used for washing 3 times, and then absolute ethyl alcohol is used for washing 3 times; the drying conditions are as follows: 60. drying at 24-48 deg.C and h.
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