CN116253571A - Aluminum nitride ceramic granulating powder and preparation method thereof - Google Patents
Aluminum nitride ceramic granulating powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 125
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 59
- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000012798 spherical particle Substances 0.000 claims abstract description 38
- 239000002002 slurry Substances 0.000 claims abstract description 34
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 26
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- 239000011268 mixed slurry Substances 0.000 claims abstract description 23
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- 238000000034 method Methods 0.000 claims abstract description 22
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- 229920000570 polyether Polymers 0.000 claims abstract description 21
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 239000007791 liquid phase Substances 0.000 claims description 46
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
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- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 229910010293 ceramic material Inorganic materials 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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Abstract
The invention discloses aluminum nitride ceramic granulating powder and a preparation method thereof. The weight percentage of the components is 3 to 5 weight percent of Y 2 O 3 Powder, 0.1-0.5 wt% of Al 2 O 3 Powder, 30 to 50 weight percent of AlN powder with the oxygen content less than 0.8 weight percent, 0.1 to 0.2 weight percent of fish oil, 2 to 4 weight percent of polyvinyl butyral resin, 1 to 3 weight percent of acrylic resin, 0.1 to 0.3 weight percent of organic silicon polyether and 40 to 50 weight percent of absolute alcohol solvent. According to the invention, through reasonable solid-liquid ratio design, the mixed slurry is ensured to have proper viscosity, and when the mixed slurry is atomized in the centrifugal atomizer, the turntable can enable the slurry to have corresponding kinetic energy, so that fog drops with the droplet diameter meeting the requirement are formed. Proper temperatures are set at the air inlet and the air outlet of the drying tower, so that the temperature is not too low or too high when the fog drops are dried, and the falling process of the fog drops is ensuredAnd uniformly drying from outside to inside to form regular spherical particles.
Description
Technical field:
the invention belongs to the technical field of aluminum nitride ceramics, and particularly relates to aluminum nitride ceramic granulating powder and a preparation method thereof.
The background technology is as follows:
aluminum nitride (AlN) is a novel electronic ceramic material, and has the remarkable comprehensive advantages of high heat conductivity, excellent insulating property and dielectric property, no magnetism, thermal expansion coefficient matched with a silicon material, good light transmission characteristic, no toxicity and the like, can effectively meet the requirements of large voltage, high current and high insulativity, has good high-frequency characteristic, is the most ideal packaging and heat dissipation material for semiconductor power devices, integrated circuit chips and the like which are accepted in the world at present, and can better meet the use requirements of high frequency, microwaves, 5G fields, image display, transmission, storage, infrared windows, rail transit, smart grids, new energy automobiles, industrial control and the like.
Sintering preparation of densified aluminum nitride ceramics has been a hot spot of research because aluminum nitride is a covalent bond material, making it difficult to solid phase sinter, and sintering aids must be added to promote its densification sintering by liquid phase as a mass transfer medium. At present, an aluminum nitride ceramic substrate is mainly prepared by a tape casting method and is mainly suitable for forming sheet materials, but for aluminum nitride ceramic structural member products with the thickness of 5mm and above, a dry pressing forming mode is required to be adopted for preparation, and the method has higher requirements on the morphology, particle size distribution, flowability, apparent density and the like of powder.
In the existing process for producing aluminum nitride ceramic granulating powder, the solid-liquid ratio in the slurry has defects, when the solid content in the slurry is increased, the kinetic energy reduction viscosity of the slurry is high, and the diameter of liquid drops in atomization is increased, so that the process is unfavorable for atomization and granulation. In addition, the temperature of the air inlet and the air outlet of the drying tower is unreasonable, and the temperature of the air inlet and the air outlet is too low, so that fog drops are incompletely dried, and the phenomenon of agglomeration of granulating powder occurs; the temperature of the air inlet and the air outlet is too high, so that the surface of the fog drops is too fast to dry, and a hard shell is formed on the surface of the fog drops rapidly, thereby preventing the fog drops from shrinking normally, and finally obtaining the hollow irregular granulating powder.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
The invention comprises the following steps:
the invention aims to provide aluminum nitride ceramic granulating powder and a preparation method thereof, thereby overcoming the defects in the prior art.
In order to achieve the purpose, the invention provides aluminum nitride ceramic granulating powder, which comprises the following components in percentage by weight: 3 to 5wt% of Y 2 O 3 Powder, 0.1-0.5 wt% of Al 2 O 3 Powder, 30 to 50 weight percent of AlN powder with the oxygen content less than 0.8 weight percent, 0.1 to 0.2 weight percent of fish oil, 2 to 4 weight percent of polyvinyl butyral resin, 1 to 3 weight percent of acrylic resin, 0.1 to 0.3 weight percent of organic silicon polyether and 40 to 50 weight percent of absolute alcohol solvent.
The aluminum nitride ceramic granulating powder comprises the following components in percentage by weight: 3wt% of Y 2 O 3 Powder, 0.2wt% of Al 2 O 3 Powder, 45.8wt% of AlN powder with oxygen content less than 0.8 wt%, 0.1wt% of fish oil, 3.5wt% of polyvinyl butyral resin, 2.5wt% of acrylic resin, 0.1wt% of silicone polyether and 44.8wt% of absolute alcohol solvent.
The aluminum nitride ceramic granulating powder comprises the following components in percentage by weight: 3.5wt% of Y 2 O 3 Powder, 0.3wt% of Al 2 O 3 Powder, 46.2wt% of AlN powder with oxygen content less than 0.8%, 0.1wt% of fish oil, 2.5wt% of polyvinyl butyral resin, 1.5wt% of acrylic resin, 0.2wt% of silicone polyether and 45.7wt% of absolute alcohol solvent.
The aluminum nitride ceramic granulating powder comprises the following components in percentage by weight: 4wt% of Y 2 O 3 Powder, 0.5wt% of Al 2 O 3 Powder, 46.5wt% of AlN powder with oxygen content less than 0.8%, 0.2wt% of fish oil, 2wt% of polyvinyl butyral resin, 1wt% of acrylic resin, 0.3wt% of silicone polyether and 45.5wt% of absolute alcohol solvent.
The preparation method of the aluminum nitride ceramic granulating powder comprises the following steps:
s01, weighing 3-5 wt% of Y according to the weight percentage 2 O 3 Powder, 0.1-0.5 wt% of Al 2 O 3 Powder, 30 to 50 weight percent of AlN powder with the oxygen content less than 0.8 percent, 0.1 to 0.2 weight percent of fish oil, 2 to 4 weight percent of polyvinyl butyral resin, 1 to 3 weight percent of acrylic resin, 0.1 to 0.3 weight percent of organic silicon polyether and 40 to 50wt% of an absolute alcohol solvent;
s02, weighing fish oil, absolute alcohol solvent and Y 2 O 3 Powder, al 2 O 3 Sequentially placing the powder and AlN powder into a ball milling tank, and performing wet ball milling for 1-5 h by adopting a planetary ball mill in an environment of 25-30 ℃;
s03, sequentially adding the weighed polyvinyl butyral resin, acrylic resin and organic silicon polyether into a ball milling tank in the step S02, performing wet ball milling for 20-24 h by adopting a planetary ball mill at the temperature of 25-30 ℃, and performing Y 2 O 3 Powder, al 2 O 3 The powder and AlN powder are wrapped by polyvinyl butyral resin and acrylic resin to form mixed slurry with certain viscosity;
s04, conveying the mixed slurry to a rotary table of a centrifugal atomizer at a feeding speed of 1-30kg/h, and atomizing the mixed slurry in a nitrogen atmosphere; the turntable with the diameter of 50mm spreads the slurry on the turntable under the centrifugal action to form a film under the rotating speed of 8000-60000 rpm, and the slurry continuously moves towards the edge of the turntable; because the slurry at different positions is subjected to different shearing forces and has friction force with nitrogen, the slurry is dispersed into fine mist drops and then mixed with dry nitrogen; the size and the size distribution of fog drops are controlled by adjusting the size, the rotating speed, the slurry viscosity and the feeding speed of the rotating disc;
s05, mixing the fog drops with dry nitrogen, and then entering a drying tower from a centrifugal atomizer, wherein in the descending process of the fog drops in the drying tower, the organic solvent in the fog drops starts to evaporate and dry, and the drying of the fog drops is the evaporation process of the liquid phase in the fog drops; when the drying starts, the evaporation speed of the liquid phase of the fog drops increases rapidly and reaches the maximum value; then entering a constant drying stage, wherein the liquid phase moves from the inside to the outside of the fog drops, so that the surfaces of the fog drops are in a liquid phase saturated state, and the fog drops keep a lower temperature; when the critical liquid phase content is reached, the liquid phase evaporation speed of the fog drops is reduced because the liquid phase content in the fog drops is reduced at the moment, so that the temperature of the fog drops is increased, the liquid phase evaporation speed of the fog drops is further reduced, the drying process gradually goes deep into the fog drops along with the time, the liquid phase evaporation speed of the fog drops continuously decreases, and hard shells are formed on the outer parts due to drying, so that the dry spherical particles are obtained;
s06, the dried spherical particles fall into a trapping tank at the bottom of a drying tower to be collected, so as to obtain 5-15wt% of spherical particles with the particle size of 30-60 mu m, 70-90wt% of spherical particles with the particle size of 60-100 mu m and 5-15wt% of spherical particles with the particle size of 100-150 mu m; wherein the particle diameter D50 of the spherical particles is 60-100 mu m, and the apparent density of the spherical particles is 0.8-1.1 g/cm 3 。
Preferably, in the technical scheme, the ball milling medium in the ball milling tank in the steps S02 and S03 is alumina balls with the purity of 20-30 vt percent and more than or equal to 99.99 percent.
Preferably, in the technical scheme, the revolution speed of the planetary ball mill in the steps S02 and S03 is 100-300rpm, and the rotation speed is 300-500rpm.
Preferably, in the technical scheme, in the step S03, the viscosity of the mixed slurry is less than 200mpas at 25-30 ℃.
Preferably, in step S03, Y is included in the mixed slurry 2 O 3 Powder, al 2 O 3 The solid content of the powder and AlN powder is 45-55%.
Preferably, in the technical scheme, in the step S05, the temperature of an air inlet of the drying tower is 150-350 ℃, and the temperature of an air outlet of the drying tower is 80-150 ℃.
Compared with the prior art, the invention has the following beneficial effects:
through reasonable formula design, the solid-liquid ratio in the formula is proper, the mixed slurry is ensured to have proper viscosity, and when the slurry is atomized in the centrifugal atomizer, the turntable can enable the slurry to have corresponding kinetic energy, form fog drops with the droplet diameter meeting the requirement, and ensure that the subsequent drying process is smoothly carried out. Proper temperatures are set at the air inlet and the air outlet of the drying tower, so that the temperature is not too low or too high when the fog drops are dried, and the fog drops are uniformly dried from outside to inside in the falling process, so that regular spherical particles are formed.
Description of the drawings:
FIG. 1 is a diagram of the morphology of aluminum nitride ceramic granulated powder at 100 times magnification by a scanning electron microscope;
FIG. 2 is a graph of morphology of aluminum nitride ceramic granulated powder at 500 times magnification by a scanning electron microscope;
FIG. 3 is a graph of morphology of aluminum nitride ceramic granulated powder at 1000 times magnification by a scanning electron microscope;
FIG. 4 is a graph of morphology of aluminum nitride ceramic granulated powder at 500 Xmagnification by a scanning electron microscope;
FIG. 5 is a graph of morphology of aluminum nitride ceramic granulated powder at 1000 times magnification by a scanning electron microscope;
FIG. 6 is a graph of morphology of aluminum nitride ceramic granulated powder at 200 times magnification by a scanning electron microscope;
FIG. 7 is a graph of morphology of aluminum nitride ceramic granulated powder at 200 Xmagnification by a scanning electron microscope.
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
Example 1
The aluminum nitride ceramic granulating powder comprises the following components in percentage by weight: 3wt% of Y 2 O 3 Powder, 0.2wt% of Al 2 O 3 Powder, 45.8wt% of AlN powder with oxygen content less than 0.8 wt%, 0.1wt% of fish oil, 3.5wt% of polyvinyl butyral resin, 2.5wt% of acrylic resin, 0.1wt% of silicone polyether and 44.8wt% of absolute alcohol solvent.
The preparation method of the aluminum nitride ceramic granulating powder comprises the following steps:
s01, weighing 3wt% of Y according to the weight percentage 2 O 3 Powder, 0.2wt% of Al 2 O 3 Powder, 45.8wt% of AlN powder with oxygen content less than 0.8%, 0.1wt% of fish oil, 3.5wt% of polyvinyl butyral resin and 2.5wt% of acrylic resin0.1wt% of organosilicon polyether and 44.8wt% of absolute alcohol solvent;
s02, weighing fish oil, absolute alcohol solvent and Y 2 O 3 Powder, al 2 O 3 Sequentially placing the powder and AlN powder into a ball milling tank, wherein a ball milling medium in the ball milling tank is alumina balls with the purity of 25vt percent or more than 99.99 percent, performing wet ball milling for 2 hours by adopting a planetary ball mill under the environment of 26 ℃, wherein the revolution speed of the planetary ball mill is 100rpm, and the rotation speed is 300rpm;
s03, sequentially adding the weighed polyvinyl butyral resin, acrylic resin and organic silicon polyether into the ball milling tank in the step S02, performing wet ball milling for 20 hours by adopting a planetary ball mill under the environment of 26 ℃, wherein the revolution speed of the planetary ball mill is 150rpm, the rotation speed is 350rpm and the Y is 2 O 3 Powder, al 2 O 3 The powder and AlN powder are wrapped by polyvinyl butyral resin and acrylic resin to form mixed slurry with the viscosity of 100 mpas;
s04, conveying the mixed slurry to a rotary table of a centrifugal atomizer at a feeding speed of 20kg/h, and atomizing the mixed slurry in a nitrogen atmosphere; the turntable with the diameter of 50mm spreads the slurry on the turntable under the centrifugal action at the rotating speed of 20000rpm to form a film, and the slurry continuously moves towards the edge of the turntable; because the slurry at different positions is subjected to different shearing forces and has friction force with nitrogen, the slurry is dispersed into fine mist drops and then mixed with dry nitrogen;
s05, mixing the fog drops with dry nitrogen, and then entering a drying tower from a centrifugal atomizer, wherein the temperature of an air inlet of the drying tower is 300 ℃, the temperature of an air outlet of the drying tower is 130 ℃, and in the descending process of the fog drops in the drying tower, the organic solvent in the fog drops starts to evaporate and dry, and the drying of the fog drops is the evaporation process of the liquid phase in the fog drops; when the drying starts, the evaporation speed of the liquid phase of the fog drops increases rapidly and reaches the maximum value; then entering a constant drying stage, wherein the liquid phase moves from the inside to the outside of the fog drops, so that the surfaces of the fog drops are in a liquid phase saturated state, and the fog drops keep a lower temperature; when the critical liquid phase content is reached, the liquid phase evaporation speed of the fog drops is reduced because the liquid phase content in the fog drops is reduced at the moment, so that the temperature of the fog drops is increased, the liquid phase evaporation speed of the fog drops is further reduced, the drying process gradually goes deep into the fog drops along with the time, the liquid phase evaporation speed of the fog drops continuously decreases, and hard shells are formed on the outer parts due to drying, so that the dry spherical particles are obtained;
s06, the dried spherical particles fall into a trapping tank at the bottom of a drying tower to be collected, and as shown in figure 1, 10 weight percent of spherical particles with the particle size of 30-60 mu m, 82 weight percent of spherical particles with the particle size of 60-100 mu m and 8 weight percent of spherical particles with the particle size of 100-150 mu m are obtained; wherein the particle diameter D50 of the spherical particles is 60-100 mu m, and the apparent density of the spherical particles is 0.92g/cm 3 。
Example 2
The aluminum nitride ceramic granulating powder comprises the following components in percentage by weight: 3.5wt% of Y 2 O 3 Powder, 0.3wt% of Al 2 O 3 Powder, 46.2wt% of AlN powder with oxygen content less than 0.8%, 0.1wt% of fish oil, 2.5wt% of polyvinyl butyral resin, 1.5wt% of acrylic resin, 0.2wt% of silicone polyether and 45.7wt% of absolute alcohol solvent.
The preparation method of the aluminum nitride ceramic granulating powder comprises the following steps:
s01, weighing 3.5wt% of Y according to the weight percentage 2 O 3 Powder, 0.3wt% of Al 2 O 3 Powder, 46.2wt% of AlN powder with oxygen content less than 0.8%, 0.1wt% of fish oil, 2.5wt% of polyvinyl butyral resin, 1.5wt% of acrylic resin, 0.2wt% of silicone polyether and 45.7wt% of absolute alcohol solvent;
s02, weighing fish oil, absolute alcohol solvent and Y 2 O 3 Powder, al 2 O 3 Sequentially placing the powder and AlN powder into a ball milling tank, wherein a ball milling medium in the ball milling tank is alumina balls with the purity of 25vt percent or more than 99.99 percent, performing wet ball milling for 3 hours by adopting a planetary ball mill under the environment of 27 ℃, wherein the revolution speed of the planetary ball mill is 150rpm, and the rotation speed is 350rpm;
s03, weighing polyvinyl butyral resin, acrylic resin and organosilicon polymerSequentially adding ether into the ball milling tank of the step S02, performing wet ball milling for 21 hours by adopting a planetary ball mill under the environment of 27 ℃, wherein the revolution speed of the planetary ball mill is 200rpm, the rotation speed is 400rpm, and the Y is 2 O 3 Powder, al 2 O 3 The powder and AlN powder are wrapped by polyvinyl butyral resin and acrylic resin to form mixed slurry with the viscosity of 120 mpas;
s04, conveying the mixed slurry to a rotary table of a centrifugal atomizer at a feeding speed of 10kg/h, and atomizing the mixed slurry in a nitrogen atmosphere; the turntable with the diameter of 50mm spreads the slurry on the turntable under the centrifugal action at the rotating speed of 30000rpm to form a film, and the slurry continuously moves towards the edge of the turntable; because the slurry at different positions is subjected to different shearing forces and has friction force with nitrogen, the slurry is dispersed into fine mist drops and then mixed with dry nitrogen;
s05, mixing the fog drops with dry nitrogen, and then entering a drying tower from a centrifugal atomizer, wherein the temperature of an air inlet of the drying tower is 260 ℃, the temperature of an air outlet of the drying tower is 110 ℃, and in the descending process of the fog drops in the drying tower, the organic solvent in the fog drops starts to evaporate and dry, and the drying of the fog drops is the evaporation process of the liquid phase in the fog drops; when the drying starts, the evaporation speed of the liquid phase of the fog drops increases rapidly and reaches the maximum value; then entering a constant drying stage, wherein the liquid phase moves from the inside to the outside of the fog drops, so that the surfaces of the fog drops are in a liquid phase saturated state, and the fog drops keep a lower temperature; when the critical liquid phase content is reached, the liquid phase evaporation speed of the fog drops is reduced because the liquid phase content in the fog drops is reduced at the moment, so that the temperature of the fog drops is increased, the liquid phase evaporation speed of the fog drops is further reduced, the drying process gradually goes deep into the fog drops along with the time, the liquid phase evaporation speed of the fog drops continuously decreases, and hard shells are formed on the outer parts due to drying, so that the dry spherical particles are obtained;
s06, the dried spherical particles fall into a trapping tank at the bottom of a drying tower to be collected, and 9wt% of spherical particles with the particle size of 30-60 mu m, 81wt% of spherical particles with the particle size of 60-100 mu m and 10wt% of spherical particles with the particle size of 100-150 mu m are obtained as shown in figures 2-3; wherein the particle diameter of the spherical particlesD50 is 60-100 μm, and the apparent density of the spherical particles is 0.95g/cm 3 。
Example 3
The aluminum nitride ceramic granulating powder comprises the following components in percentage by weight: 4wt% of Y 2 O 3 Powder, 0.5wt% of Al 2 O 3 Powder, 46.5wt% of AlN powder with oxygen content less than 0.8%, 0.2wt% of fish oil, 2wt% of polyvinyl butyral resin, 1wt% of acrylic resin, 0.3wt% of silicone polyether and 45.5wt% of absolute alcohol solvent.
The preparation method of the aluminum nitride ceramic granulating powder comprises the following steps:
s01, weighing 4wt% of Y according to the weight percentage 2 O 3 Powder, 0.5wt% of Al 2 O 3 Powder, 46.5wt% of AlN powder with oxygen content less than 0.8%, 0.2wt% of fish oil, 2wt% of polyvinyl butyral resin, 1wt% of acrylic resin, 0.3wt% of organic silicon polyether and 45.5wt% of absolute alcohol solvent;
s02, weighing fish oil, absolute alcohol solvent and Y 2 O 3 Powder, al 2 O 3 Sequentially placing the powder and AlN powder into a ball milling tank, wherein a ball milling medium in the ball milling tank is alumina balls with the purity of 25vt percent and more than or equal to 99.99 percent, performing wet ball milling for 4 hours by adopting a planetary ball mill under the environment of 28 ℃, wherein the revolution speed of the planetary ball mill is 200rpm, and the rotation speed is 400rpm;
s03, sequentially adding the weighed polyvinyl butyral resin, acrylic resin and organic silicon polyether into a ball milling tank in the step S02, performing wet ball milling for 22 hours by adopting a planetary ball mill at the temperature of 28 ℃, wherein the revolution speed of the planetary ball mill is 250rpm, the rotation speed is 450rpm and the Y 2 O 3 Powder, al 2 O 3 The powder and AlN powder are wrapped by polyvinyl butyral resin and acrylic resin to form mixed slurry with the viscosity of 130 mpas;
s04, conveying the mixed slurry to a rotary table of a centrifugal atomizer at a feeding speed of 5kg/h, and atomizing the mixed slurry in a nitrogen atmosphere; the turntable with the diameter of 50mm spreads the slurry on the turntable under the centrifugal action to form a film at the rotating speed of 40000rpm, and the slurry continuously moves towards the edge of the turntable; because the slurry at different positions is subjected to different shearing forces and has friction force with nitrogen, the slurry is dispersed into fine mist drops and then mixed with dry nitrogen;
s05, mixing the fog drops with dry nitrogen, and then entering a drying tower from a centrifugal atomizer, wherein the temperature of an air inlet of the drying tower is 230 ℃, the temperature of an air outlet of the drying tower is 100 ℃, and in the descending process of the fog drops in the drying tower, the organic solvent in the fog drops starts to evaporate and dry, and the drying of the fog drops is the evaporation process of the liquid phase in the fog drops; when the drying starts, the evaporation speed of the liquid phase of the fog drops increases rapidly and reaches the maximum value; then entering a constant drying stage, wherein the liquid phase moves from the inside to the outside of the fog drops, so that the surfaces of the fog drops are in a liquid phase saturated state, and the fog drops keep a lower temperature; when the critical liquid phase content is reached, the liquid phase evaporation speed of the fog drops is reduced because the liquid phase content in the fog drops is reduced at the moment, so that the temperature of the fog drops is increased, the liquid phase evaporation speed of the fog drops is further reduced, the drying process gradually goes deep into the fog drops along with the time, the liquid phase evaporation speed of the fog drops continuously decreases, and hard shells are formed on the outer parts due to drying, so that the dry spherical particles are obtained;
s06, the dried spherical particles fall into a trapping tank at the bottom of a drying tower to be collected, and as shown in figures 4-5, 8wt% of spherical particles with the particle size of 30-60 mu m, 80wt% of spherical particles with the particle size of 60-100 mu m and 12wt% of spherical particles with the particle size of 100-150 mu m are obtained; wherein the particle diameter D50 of the spherical particles is 60-100 mu m, and the apparent density of the spherical particles is 0.96g/cm 3 。
To improve the performance of the granulated powder and to maximize the utilization of the equipment, the solids content of the slurry must be as great as possible to shorten the spray drying time and thereby obtain approximately spherical particles. The higher the solids content, the greater the viscosity of the slurry, and the excessive viscosity is detrimental to spray granulation, as shown in fig. 6, which can produce many larger size droplets. However, when the solution content is high, the slurry viscosity is small, the slurry is not easy to dry, the slurry is not easy to form, the granulated particles of the hollow spheres are easy to appear, and the material humidity is increased, as shown in fig. 7. Therefore, the invention ensures that the mixed slurry has proper viscosity by properly designing the formula, and the turntable can ensure that the slurry has corresponding kinetic energy when being atomized in the centrifugal atomizer, so as to form fog drops with the droplet diameter meeting the requirement and ensure that the subsequent drying process is smoothly carried out. Proper temperatures are set at the air inlet and the air outlet of the drying tower, so that the temperature is not too low or too high when the fog drops are dried, and the fog drops are uniformly dried from outside to inside in the falling process, so that regular spherical particles are formed.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. An aluminum nitride ceramic granulated powder, which is characterized in that: the weight percentage of the components is 3 to 5 weight percent of Y 2 O 3 Powder, 0.1-0.5 wt% of Al 2 O 3 Powder, 30 to 50 weight percent of AlN powder with the oxygen content less than 0.8 weight percent, 0.1 to 0.2 weight percent of fish oil, 2 to 4 weight percent of polyvinyl butyral resin, 1 to 3 weight percent of acrylic resin, 0.1 to 0.3 weight percent of organic silicon polyether and 40 to 50 weight percent of absolute alcohol solvent.
2. The aluminum nitride ceramic granulated powder as claimed in claim 1, wherein: the weight percentage of the components is 3wt% of Y 2 O 3 Powder, 0.2wt% of Al 2 O 3 Powder, 45.8wt% of AlN powder with oxygen content less than 0.8 wt%, 0.1wt% of fish oil, 3.5wt% of polyvinyl butyral resin, 2.5wt% of acrylic resin, 0.1wt% of silicone polyether and 44.8wt% of absolute alcohol solvent.
3. The aluminum nitride ceramic granulated powder as claimed in claim 1, wherein: the weight percentage of the components is 3.5wt% of Y 2 O 3 Powder, 0.3wt% of Al 2 O 3 Powder, 46.2wt% of AlN powder with oxygen content less than 0.8%, 0.1wt% of fish oil, 2.5wt% of polyvinyl butyral resin, 1.5wt% of acrylic resin, 0.2wt% of silicone polyether and 45.7wt% of absolute alcohol solvent.
4. The aluminum nitride ceramic granulated powder as claimed in claim 1, wherein: the weight percentage of the components is 4wt% of Y 2 O 3 Powder, 0.5wt% of Al 2 O 3 Powder, 46.5wt% of AlN powder with oxygen content less than 0.8%, 0.2wt% of fish oil, 2wt% of polyvinyl butyral resin, 1wt% of acrylic resin, 0.3wt% of silicone polyether and 45.5wt% of absolute alcohol solvent.
5. The preparation method of the aluminum nitride ceramic granulating powder comprises the following steps:
s01, weighing 3-5 wt% of Y according to the weight percentage 2 O 3 Powder, 0.1-0.5 wt% of Al 2 O 3 Powder, 30 to 50 weight percent of AlN powder with the oxygen content less than 0.8 percent, 0.1 to 0.2 weight percent of fish oil, 2 to 4 weight percent of polyvinyl butyral resin, 1 to 3 weight percent of acrylic resin, 0.1 to 0.3 weight percent of organic silicon polyether and 40 to 50 weight percent of absolute alcohol solvent;
s02, weighing fish oil, absolute alcohol solvent and Y 2 O 3 Powder, al 2 O 3 Sequentially placing the powder and AlN powder into a ball milling tank, and performing wet ball milling for 1-5 h by adopting a planetary ball mill in an environment of 25-30 ℃;
s03, sequentially adding the weighed polyvinyl butyral resin, acrylic resin and organic silicon polyether into a ball milling tank in the step S02, performing wet ball milling for 20-24 h by adopting a planetary ball mill at the temperature of 25-30 ℃, and performing Y 2 O 3 Powder, al 2 O 3 The powder and AlN powder are wrapped by polyvinyl butyral resin and acrylic resin to form mixed slurry with certain viscosity;
s04, conveying the mixed slurry to a rotary table of a centrifugal atomizer at a feeding speed of 1-30kg/h, and atomizing the mixed slurry in a nitrogen atmosphere; the turntable with the diameter of 50mm spreads the slurry on the turntable under the centrifugal action to form a film under the rotating speed of 8000-60000 rpm, and the slurry continuously moves towards the edge of the turntable; because the slurry at different positions is subjected to different shearing forces and has friction force with nitrogen, the slurry is dispersed into fine mist drops and then mixed with dry nitrogen; the size and the size distribution of fog drops are controlled by adjusting the size, the rotating speed, the slurry viscosity and the feeding speed of the rotating disc;
s05, mixing the fog drops with dry nitrogen, and then entering a drying tower from a centrifugal atomizer, wherein in the descending process of the fog drops in the drying tower, the organic solvent in the fog drops starts to evaporate and dry, and the drying of the fog drops is the evaporation process of the liquid phase in the fog drops; when the drying starts, the evaporation speed of the liquid phase of the fog drops increases rapidly and reaches the maximum value; then entering a constant drying stage, wherein the liquid phase moves from the inside to the outside of the fog drops, so that the surfaces of the fog drops are in a liquid phase saturated state, and the fog drops keep a lower temperature; when the critical liquid phase content is reached, the liquid phase evaporation speed of the fog drops is reduced because the liquid phase content in the fog drops is reduced at the moment, so that the temperature of the fog drops is increased, the liquid phase evaporation speed of the fog drops is further reduced, the drying process gradually goes deep into the fog drops along with the time, the liquid phase evaporation speed of the fog drops continuously decreases, and hard shells are formed on the outer parts due to drying, so that the dry spherical particles are obtained;
s06, the dried spherical particles fall into a trapping tank at the bottom of a drying tower to be collected, so as to obtain 5-15wt% of spherical particles with the particle size of 30-60 mu m, 70-90wt% of spherical particles with the particle size of 60-100 mu m and 5-15wt% of spherical particles with the particle size of 100-150 mu m; wherein the particle diameter D50 of the spherical particles is 60-100 mu m, and the apparent density of the spherical particles is 0.8-1.1 g/cm 3 。
6. The method for preparing aluminum nitride ceramic granulated powder according to claim 5, wherein: the ball milling medium in the ball milling tank in the steps S02 and S03 is alumina balls with the purity of 20-30 vt percent and more than or equal to 99.99 percent.
7. The method for preparing aluminum nitride ceramic granulated powder according to claim 5, wherein: in the steps S02 and S03, the revolution speed of the planetary ball mill is 100-300rpm, and the rotation speed is 300-500rpm.
8. The method for preparing aluminum nitride ceramic granulated powder according to claim 5, wherein: in step S03, the viscosity of the mixed slurry is less than 200mpas at 25-30 ℃.
9. The method for preparing aluminum nitride ceramic granulated powder according to claim 5, wherein: in step S03, Y is included in the mixed slurry 2 O 3 Powder, al 2 O 3 The solid content of the powder and AlN powder is 45-55%.
10. The method for preparing aluminum nitride ceramic granulated powder according to claim 5, wherein: in the step S05, the temperature of an air inlet of the drying tower is 150-350 ℃, and the temperature of an air outlet of the drying tower is 80-150 ℃.
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