A method for preparing aluminum nitride by spray granulation

Abstract

The invention discloses a preparation method of aluminum nitride by spray granulation, which belongs to the technical field of ceramic preparation. The method comprises: adding aluminum nitride powder and a dispersant into a ball mill for ball milling for 24 to 26 hours, adding an adhesive and a solvent thereto, wherein the adhesive is acrylic resin or PVB, and continuing ball milling for 15 to 18 hours after the adhesive and the solvent are added, the ball milling speed of the ball mill is set to 100 to 200 rpm, the diameter of the ball milling beads is 20 to 50 mm, the number of the ball milling beads is 200 to 300, and aluminum nitride slurry is formed after ball milling; the aluminum nitride slurry is sucked into a granulation tower, and the parameters of the granulation tower are set to: an air inlet temperature of 130 to 140 DEG C, an air outlet temperature of 80 to 90 DEG C, a rotation speed of an atomizing disk of 7000 to 8000 rpm, and a feed pump rotation speed of 50 to 60 rpm; collecting samples at a discharge port of the granulation tower, and then testing the samples and recording the test results.

Description

Technical Field

[0001] The invention relates to the technical field of ceramic preparation, and in particular to a method for preparing aluminum nitride by spray granulation. Background Art

[0002] With the rapid development of electronic integration and packaging technology, electronic components and equipment are developing towards miniaturization and micro-miniaturization, and the requirements for the heat dissipation performance of electronic packaging materials have also been greatly increased. If the generated heat cannot be dissipated to the outside in time, the internal accumulated heat will seriously cause the temperature of the components to rise, affecting their normal working state and eventually causing component failure. Therefore, higher and higher requirements are put forward for the heat dissipation of chip substrates and packaging materials;

[0003] Aluminum nitride has high thermal conductivity, good electrical insulation and low dielectric loss, and is an ideal substrate material and electronic device packaging material. The performance of aluminum nitride powder has an important impact on the performance of substrate materials. With the rapid development of microelectronics technology, microwave devices and millimeter wave devices are widely used, and high-performance aluminum nitride has become one of the hot spots of current research.

[0004] In industrial production, spray granulation is a common method for preparing solid particles. This technology uses the pressure of liquid or gas to break liquid or solid materials into tiny particles, and then solidifies these particles by drying or cooling to form the desired solid particle products. Spray granulation technology has the advantages of high production efficiency, uniform particle size, and simple operation. It is widely used in the fields of chemical industry, food, medicine, ceramics, metal powder, etc.

[0005] Ceramic technology has traditionally used spray drying with an organic solvent system, but there are still many problems, such as the morphology of spray granulated particles being hollow irregular spheres. Summary of the invention

[0006] The technical problem to be solved by the present invention is to provide a method for preparing aluminum nitride by spray granulation, so as to solve the problems raised by the background technology and improve the morphology of the spray granulation particles.

[0007] In order to solve the above technical problems, the technical solution of the present invention is:

[0008] A method for preparing aluminum nitride by spray granulation, the method comprising:

[0009] Add aluminum nitride powder and a dispersant to a ball mill and mill for 24 to 26 hours, wherein the content of the dispersant is 0.1% to 1%, and then add an adhesive and a solvent thereto, wherein the adhesive is an acrylic resin or PVB, and the content of the adhesive is 1% to 4%. After adding the adhesive and the solvent, continue to mill for 15 to 18 hours, the ball milling speed of the ball mill is set to 100 to 200 rpm, the diameter of the ball milling beads is 20 to 50 mm, the number of the ball milling beads is 200 to 300, and aluminum nitride slurry is formed after ball milling, and the solid content of the aluminum nitride slurry is 50% to 60%;

[0010] The aluminum nitride slurry is sucked into the granulation tower, and the parameters of the granulation tower are set as follows: the inlet air temperature is 130-140°C, the outlet air temperature is 80-90°C, the speed of the atomizing disk is 7000-8000rpm, and the speed of the feed pump is 50-60rpm;

[0011] Collect samples at the outlet of the granulation tower, then test the samples and record the test results.

[0012] Preferably, the adhesive is acrylic resin, and the content of the adhesive is 1.5%.

[0013] Preferably, the adhesive is acrylic resin, and the bulk density of the sample obtained under the condition of 1.5% is 0.81g / cm 3 .

[0014] Preferably, the solvent is ethanol.

[0015] Preferably, the content of the dispersant is 0.5%, and the solid content of the aluminum nitride slurry is 55%.

[0016] The above technical solution has the following beneficial effects:

[0017] The present application discloses a method for preparing aluminum nitride by spray granulation. The aluminum nitride particles obtained by spray granulation have regular spherical particles, good spheroidization effect and good fluidity. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a morphology diagram of aluminum nitride particles obtained by spray granulation in Example 4 of the present invention;

[0019] Figure 2 This is a morphology diagram of aluminum nitride particles obtained by spray granulation in Example 5 of the present invention;

[0020] Figure 3 This is a morphology picture of the aluminum nitride particles obtained by spray granulation in Example 6 of the present invention. DETAILED DESCRIPTION

[0021] The specific embodiments of the present invention are further described below in conjunction with the accompanying drawings. It should be noted that the description of these embodiments is used to help understand the present invention, but does not constitute a limitation of the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0022] Example 1

[0023] A method for preparing aluminum nitride by spray granulation comprises the following steps:

[0024] The aluminum nitride powder and the dispersant are added to a ball mill and ball milled for 24 to 26 hours, wherein the content of the dispersant is 0.1% to 1%, and then an adhesive and a solvent are added thereto, wherein the solvent is ethanol, the adhesive is acrylic resin or PVB, and the content of the adhesive is 1% to 4%. After adding the adhesive and the solvent, the ball milling is continued for 15 to 18 hours, the ball milling speed of the ball mill is set to 100 to 200 rpm, the diameter of the ball milling beads is 20 to 50 mm, the number of the ball milling beads is 200 to 300, and aluminum nitride slurry is formed after ball milling, and the solid content of the aluminum nitride slurry is 50% to 60%;

[0025] The aluminum nitride slurry is sucked into the granulation tower, and the parameters of the granulation tower are set as follows: the inlet air temperature is 130-140°C, the outlet air temperature is 80-90°C, the speed of the atomizing disk is 7000-8000rpm, and the speed of the feed pump is 50-60rpm;

[0026] Collect samples at the outlet of the granulation tower, then test the samples and record the test results.

[0027] Example 2

[0028] A method for preparing aluminum nitride by spray granulation comprises the following steps:

[0029] Aluminum nitride powder and a dispersant are added to a ball mill and ball milled for 24 hours, wherein the content of the dispersant is 0.1%, and then an adhesive and a solvent are added thereto, wherein the solvent is ethanol, the adhesive is acrylic resin or PVB, and the content of the adhesive is 1%. After adding the adhesive and the solvent, the ball milling is continued for 15 hours, the ball milling speed of the ball mill is set to 100 rpm, the diameter of the ball milling beads is 20 to 50 mm, the number of the ball milling beads is 200, and aluminum nitride slurry is formed after ball milling, and the solid content in the aluminum nitride slurry is 50%;

[0030] The aluminum nitride slurry was sucked into the granulation tower. The parameters of the granulation tower were set as follows: the inlet air temperature was 130°C, the outlet air temperature was 80°C, the speed of the atomizing disk was 7000rpm, and the speed of the feed pump was 50rpm.

[0031] Collect samples at the outlet of the granulation tower, test them and record the test results.

[0032] Example 3

[0033] A method for preparing aluminum nitride by spray granulation comprises the following steps:

[0034] Aluminum nitride powder and a dispersant are added to a ball mill and ball milled for 26 hours, wherein the content of the dispersant is 1%, and then a binder and a solvent are added thereto, wherein the solvent is ethanol, the binder is acrylic resin or PVB, and the content of the binder is 4%. After adding the binder and the solvent, the ball milling is continued for 18 hours, the ball milling speed of the ball mill is set to 200 rpm, the ball milling bead diameter is 50 mm, the number of the ball milling beads is 300, and aluminum nitride slurry is formed after ball milling, and the solid content of the aluminum nitride slurry is 60%;

[0035] The aluminum nitride slurry was sucked into the granulation tower. The parameters of the granulation tower were set as follows: the inlet air temperature was 140°C, the outlet air temperature was 90°C, the speed of the atomizing disk was 8000rpm, and the speed of the feed pump was 60rpm.

[0036] Collect samples at the outlet of the granulation tower, then test the samples and record the test results.

[0037] Example 4

[0038] A method for preparing aluminum nitride by spray granulation comprises the following steps:

[0039] Aluminum nitride powder and a dispersant are added to a ball mill and ball milled for 25 hours, wherein the content of the dispersant is 0.5%, and then a binder and ethanol are added thereto, wherein the binder is PVB and the content of the binder is 1.5%. After adding the binder and the solvent, the ball milling is continued for 16 hours, the ball milling speed of the ball mill is set to 150 rpm, the diameter of the ball milling beads is 35 mm, the number of the ball milling beads is 250, and aluminum nitride slurry is formed after ball milling, and the solid content in the aluminum nitride slurry is 55%;

[0040] The aluminum nitride slurry was sucked into the granulation tower. The parameters of the granulation tower were set as follows: the inlet air temperature was 135°C, the outlet air temperature was 85°C, the speed of the atomizing disk was 7500rpm, and the speed of the feed pump was 55rpm.

[0041] Collect samples at the outlet of the granulation tower, then test the samples and record the test results. Figure 1 , is the morphology of the aluminum nitride spray granulation obtained under the conditions of this embodiment.

[0042] Example 5

[0043] A method for preparing aluminum nitride by spray granulation comprises the following steps:

[0044] Aluminum nitride powder and a dispersant are added to a ball mill and ball milled for 25 hours, wherein the content of the dispersant is 0.5%, and then a binder and ethanol are added thereto, wherein the binder is an acrylic resin, and the content of the binder is 1.5%. After adding the binder and the solvent, the ball milling is continued for 16 hours, the ball milling speed of the ball mill is set to 150 rpm, the ball milling bead diameter is 35 mm, the number of the ball milling beads is 250, and aluminum nitride slurry is formed after ball milling, and the solid content in the aluminum nitride slurry is 55%;

[0045] The aluminum nitride slurry was sucked into the granulation tower. The parameters of the granulation tower were set as follows: the inlet air temperature was 135°C, the outlet air temperature was 85°C, the speed of the atomizing disk was 7500rpm, and the speed of the feed pump was 55rpm.

[0046] Collect samples at the outlet of the granulation tower, then test the samples and record the test results. Figure 2 , is the morphology of the aluminum nitride spray granulation obtained under the conditions of this embodiment.

[0047] Example 6

[0048] A method for preparing aluminum nitride by spray granulation comprises the following steps:

[0049] Aluminum nitride powder and a dispersant are added to a ball mill and ball milled for 26 hours, wherein the content of the dispersant is 0.5%, and then a binder and ethanol are added thereto, wherein the binder is an acrylic resin, and the content of the binder is 3%. After adding the binder and the solvent, the ball milling is continued for 18 hours, the ball milling speed of the ball mill is set to 150 rpm, the diameter of the ball milling beads is 35 mm, the number of the ball milling beads is 250, and aluminum nitride slurry is formed after ball milling, and the solid content in the aluminum nitride slurry is 55%;

[0050] The aluminum nitride slurry was sucked into the granulation tower. The parameters of the granulation tower were set as follows: the inlet air temperature was 135°C, the outlet air temperature was 85°C, the speed of the atomizing disk was 7500rpm, and the speed of the feed pump was 55rpm.

[0051] Collect samples at the outlet of the granulation tower, then test the samples and record the test results. Figure 3 , is the morphology of the aluminum nitride spray granulation obtained under the conditions of this embodiment.

[0052] The results of the tests of Example 4, Example 5 and Example 6 are shown in Table 1 below;

[0053] Table 1:

[0054] Bulk density g / cm3 Liquidity s / 100g Particle morphology Example 4 0.77 4.93 Hollow irregular sphere Example 5 0.81 4.84 Regular spherical Example 6 0.68 7.73 Hollow irregular sphere

[0055] In Example 5, the aluminum nitride spray granulation prepared under the condition that the binder is acrylic resin and the content of the binder is 1.5% has good spheroidization effect and good fluidity.

[0056] The embodiments of the present invention are described in detail above with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. For those skilled in the art, various changes, modifications, substitutions and variations of these embodiments are made without departing from the principles and spirit of the present invention, and still fall within the scope of protection of the present invention.

Claims

1. A method for preparing aluminum nitride by spray granulation, characterized in that: The preparation method comprises: Add aluminum nitride powder and a dispersant to a ball mill and mill for 24 to 26 hours, wherein the content of the dispersant is 0.1% to 1%, and then add an adhesive and a solvent thereto, wherein the adhesive is an acrylic resin or PVB, and the content of the adhesive is 1% to 4%. After adding the adhesive and the solvent, continue to mill for 15 to 18 hours, the ball milling speed of the ball mill is set to 100 to 200 rpm, the diameter of the ball milling beads is 20 to 50 mm, the number of the ball milling beads is 200 to 300, and aluminum nitride slurry is formed after ball milling, and the solid content of the aluminum nitride slurry is 50% to 60%; The aluminum nitride slurry is sucked into the granulation tower, and the parameters of the granulation tower are set as follows: the inlet air temperature is 130-140°C, the outlet air temperature is 80-90°C, the speed of the atomizing disk is 7000-8000rpm, and the speed of the feed pump is 50-60rpm; Collect samples at the outlet of the granulation tower, then test the samples and record the test results.

2. The method for preparing aluminum nitride by spray granulation according to claim 1, characterized in that: The adhesive is acrylic resin, and the content of the adhesive is 1.5%.

3. The method for preparing aluminum nitride by spray granulation according to claim 2, characterized in that: The adhesive is acrylic resin, and the bulk density of the sample obtained under the condition of 1.5% is 0.81g / cm 3 .

4. The method for preparing aluminum nitride by spray granulation according to claim 1, characterized in that: The solvent is ethanol.

5. The method for preparing aluminum nitride by spray granulation according to claim 1, characterized in that: The content of the dispersant is 0.5%, and the solid content of the aluminum nitride slurry is 55%.

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