CN115872753A - Ceramic slurry for additive manufacturing of aluminum nitride ceramic substrate and preparation method and application thereof - Google Patents
Ceramic slurry for additive manufacturing of aluminum nitride ceramic substrate and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an additive manufacturing ceramic slurry of an aluminum nitride ceramic substrate, a preparation method and application thereof, aiming at the physical characteristics of aluminum nitride powder, high-purity nitride powder gradation with different particle sizes and a unique powder surface modification mode are adopted to prepare the additive manufacturing ceramic slurry with good thermal shock resistance and thermal conductivity, the obtained ceramic slurry is formed by a photocuring method to obtain a ceramic substrate blank with an inner runner, and the ceramic substrate blank is sintered in an air pressure furnace by a tool and a powder embedding sintering method to obtain a high-thermal conductivity aluminum nitride-based ceramic substrate with the inner runner.
Description
Technical Field
The invention relates to the technical field of ceramic substrates and ceramic additive manufacturing, in particular to aluminum nitride ceramic substrate additive manufacturing ceramic slurry and a preparation method and application thereof.
Background
With the vigorous development of the microelectronic packaging industry, the electronic packaging technology is developing towards miniaturization, high density, multi-power and high reliability, and the electronic packaging material also gradually becomes an industrial field with high technical content and high economic benefit and has an important position. The currently used substrate materials mainly include four major types, namely a plastic substrate, a metal substrate, a ceramic substrate and a composite substrate. The ceramic substrate is greatly superior to a common glass fiber PCB (printed circuit board) in heat dissipation performance, current carrying capacity, insulativity, thermal expansion coefficient and the like, so that the ceramic substrate is widely applied to products such as high-power electronic modules, aerospace, military electronics and the like.
Currently, two common substrate materials, aluminum oxide and aluminum nitride, are commonly used in the market. Wherein, the purity of the alumina substrate is generally more than 96 percent, the process is simple, the price is low, but the heat conduction effect is not good enough; aluminum nitride is characterized by a Coefficient of Thermal Expansion (CTE) comparable to that of semiconductor silicon (Si) and a high thermal conductivity, typically 5 to 10 times that of aluminum oxide. With the development of aluminum nitride process technology and the increasing demand of the market, aluminum nitride substrates are becoming more and more popular in the market and becoming excellent candidates for advanced integrated circuits. In addition, the composite material is also very suitable for VLSL components, packaging shells of microwave vacuum tubes, packaging of hybrid power switches and the like. It is expected that aluminum nitride will eventually become the mainstream material in the fields of substrates and high-density packaging.
The thermal conductivity is the most main performance of aluminum nitride, the theoretical thermal conductivity of the aluminum nitride is 320W/(m.k), the scale of aluminum nitride ceramic substrate production enterprises in China is small, the research and development investment is limited, technical staff is few, and the experience is insufficient, so that the overall level of the aluminum nitride ceramic substrate industry in China is low, the product lacks competitiveness, medium and low-end products are taken as the main, and high-end aluminum nitride substrates are also dependent on imports. Due to the special technical requirements of the aluminum nitride ceramic substrate, the equipment investment is large, and the manufacturing process is complex; under the influence of crystal lattices, air holes, defects, impurities, structures and the like, the conventional aluminum nitride substrate on the market generally has the thermal conductivity of 100-120W/(m.k), and the traditional domestic process can only be used as a simple-configuration planar ceramic substrate, but with the further development of the market, higher requirements can be put forward on the thermal conductivity, the heat dissipation performance and the configuration complexity of the aluminum nitride substrate.
Disclosure of Invention
The invention aims to provide ceramic slurry for additive manufacturing of an aluminum nitride ceramic substrate, and a preparation method and application thereof, so as to overcome the defect that the existing aluminum nitride ceramic substrate material cannot meet higher heat-conducting performance and heat dissipation performance.
An aluminum nitride ceramic substrate additive manufacturing ceramic slurry comprises the following components in parts by weight: 50-65 parts of aluminum nitride powder, 1-7 parts of powder surface modifier, 35-55 parts of photosensitive resin, 0.8-3.5 parts of photoinitiator, 1.5-3.5 parts of dispersant and 3-4 parts of viscosity regulator.
Preferably, the particle diameter of the aluminum nitride powder is 0.5-5 μm, and the purity is more than or equal to 99.9%.
Preferably, the powder surface modifier is one or more of dimer acid, fatty acid, pentaerythritol oleate and the like.
Preferably, the photosensitive resin is one or a mixture of aliphatic epoxy resin, polyacrylic resin and epoxy acrylate.
Preferably, the photoinitiator adopts one or a mixture of TPO and DMPA; the dispersant is a hyper-dispersant, and the viscosity regulator is one or a mixture of glycerol and PEG 200.
A preparation method of ceramic slurry for additive manufacturing of an aluminum nitride ceramic substrate comprises the following steps:
s1, taking 45-65 parts of aluminum nitride powder, 1-7 parts of powder surface modifier, 35-55 parts of photosensitive resin, 0.8-3.5 parts of photoinitiator, 1.5-3.5 parts of dispersant and 3-4 parts of viscosity regulator according to parts by weight;
s2, uniformly mixing the aluminum nitride powder in absolute ethyl alcohol to obtain a mixed powder solution;
s3, ball-milling the mixed powder solution, uniformly mixing, performing vacuum defoaming, drying treatment and crushing on the uniformly mixed powder solution, and screening by using a screen to obtain powder A with the particle size of 15-53 mu m;
s4, adding a powder surface modifier into the powder A, adding zirconia ball grinding beads for uniform dispersion, and crushing and screening the uniformly mixed powder A to obtain powder B with the grain size of 15-35 mu m;
s5, uniformly mixing the photosensitive resin, the photoinitiator, the dispersant and the viscosity regulator to obtain a resin mixture; and adding the powder B into the resin mixture, uniformly mixing, defoaming, and filtering to obtain the ceramic slurry.
A preparation method of a high-thermal-conductivity aluminum nitride-based ceramic substrate comprises the following steps:
carrying out photocuring forming on the ceramic slurry of claim 1 or the ceramic slurry obtained by the preparation method of claim 6 to obtain a ceramic substrate biscuit, and carrying out degreasing treatment on the obtained ceramic substrate biscuit; putting the degreased ceramic substrate biscuit into a tool and embedding Al 2 O 3 And (3) cooling the powder with a furnace after high-temperature treatment to finally obtain the high-thermal-conductivity aluminum nitride-based ceramic substrate with the inner flow channel.
Preferably, the obtained ceramic slurry is placed in light curing equipment, and a ceramic substrate biscuit is obtained by molding through a light curing method; the laser power of the light curing equipment is 800-2400 mW, the laser scanning speed is 2000-5000mm/s, and the scanning layer thickness is 0.03-0.05mm.
Preferably, the degreased ceramic substrate biscuit is loaded into a tool, alumina powder embedding treatment is carried out, the temperature is raised to 1200-1300 ℃ according to the temperature rise rate of 1-1.5 ℃/min and is kept for 1-2h, then the temperature is raised to 1600-1700 ℃ according to the temperature rise rate of 5-10 ℃/min and is kept for 1-3h, furnace cooling is carried out after the temperature is raised, and finally the high-thermal-conductivity aluminum nitride-based ceramic substrate with the complex configuration can be obtained.
Preferably, the prepared aluminum nitride substrate has the thermal conductivity of 150-180W/(m.k), and an inner flow channel is arranged in the prepared aluminum nitride substrate.
Compared with the prior art, the invention has the following beneficial technical effects:
the high-thermal-conductivity aluminum nitride-based ceramic slurry for additive manufacturing is prepared from the raw materials in parts by weight, can realize the forming of a high-thermal-conductivity aluminum nitride-based ceramic substrate with a complex configuration, and introduces aluminum nitride powder with different particle sizes, so that the material has very high thermal shock resistance and thermal conductivity, the sintering shrinkage is reduced, and the problems of cracking and deformation of the ceramic substrate with a thin wall, a hollow structure, a curved surface complex structure and the like due to sintering stress in the processes of degreasing and sintering are solved; by adopting the powder surface modifier, a transition layer is formed on the surface of the aluminum nitride powder, and the transition layer can be better combined with photosensitive resin, so that the curing capability is enhanced, and the formability of additive manufacturing is improved.
According to the preparation method of the aluminum nitride-based ceramic substrate, ceramic slurry prepared according to requirements is formed by a photocuring method to obtain a ceramic substrate biscuit with an inner flow channel, the ceramic substrate biscuit is degreased and then is installed by a tool, the aluminum nitride-based ceramic substrate can be obtained by sintering in a pneumatic furnace by a powder embedding sintering method, and the aluminum nitride-based ceramic substrate with the inner flow channel can be formed;
according to the invention, the surface modification method is adopted for the aluminum nitride ceramic powder formed by additive manufacturing, so that a transition layer is formed on the surface of the aluminum nitride powder, and the aluminum nitride ceramic powder can be better combined with photosensitive resin, the curing difficulty of aluminum nitride ceramic slurry is reduced, and the additive manufacturing formability of aluminum nitride is enhanced; in addition, the aluminum nitride powder with high purity and different particle sizes is selected for grading, the thermal conductivity and the thermal shock resistance of the ceramic substrate are adjusted, the forming performance of the ceramic substrate with the inner runner is improved, and the forming difficulty of the aluminum nitride substrate with the complex structure is reduced.
Furthermore, after the aluminum nitride substrate biscuit obtained by the light curing method is placed into a tool and combined with a powder embedding process, degreasing and sintering treatment are carried out, so that the surface precision and the dimensional precision of the additive manufacturing ceramic substrate can be effectively improved.
Drawings
FIG. 1 is a schematic diagram of the surface modification process of aluminum nitride powder in the example.
Fig. 2 is a comparison diagram of a formed object in an embodiment of the present invention, fig. 2a is a schematic diagram of a conventional substrate structure, and fig. 2b is a schematic diagram of a high thermal conductivity additive manufactured aluminum nitride ceramic substrate structure prepared in embodiment 2 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The high-thermal-conductivity aluminum nitride-based ceramic slurry for additive manufacturing comprises the following components in parts by weight: 50 to 65 portions of aluminum nitride powder, 1 to 7 portions of powder surface modifier, 35 to 55 portions of photosensitive resin, 0.8 to 3.5 portions of photoinitiator, 1.5 to 3.5 portions of dispersant and 3 to 4 portions of viscosity regulator.
The particle size of the aluminum nitride powder is 0.5-5 μm, the purity is more than or equal to 99.9%, the weight ratio of submicron and micron powder is 1.
The powder surface modifier is one or more of dimer acid, fatty acid, pentaerythritol oleate, etc.
The photosensitive resin is one or a mixture of aliphatic epoxy resin, polyacrylic resin and epoxy acrylate, and the photoinitiator is one or a mixture of TPO and DMPA; the dispersant is a hyper-dispersant, and the viscosity regulator is one or a mixture of glycerol and PEG 200.
A preparation method of a high-thermal-conductivity aluminum nitride-based ceramic substrate comprises the following steps:
taking 45-65 parts of aluminum nitride powder, 1-7 parts of powder surface modifier, 35-55 parts of photosensitive resin, 0.8-3.5 parts of photoinitiator, 1.5-3.5 parts of dispersant and 3-4 parts of viscosity regulator according to parts by weight;
uniformly mixing the aluminum nitride powder in absolute ethyl alcohol to obtain a mixed powder solution;
putting the mixed powder solution into a ball mill, adding zirconia balls for milling, uniformly dispersing, uniformly ball-milling for 12-24 hours, performing vacuum defoaming, drying, crushing, and screening by using a screen to obtain powder A with the particle size of 15-53 mu m suitable for additive manufacturing;
adding a powder surface modifier into the powder A, adding zirconia ball milling beads for uniform dispersion, carrying out ball milling for 12-24 hours, crushing and screening the uniformly mixed powder to obtain the finally used powder B with the grain diameter of 15-35 mu m suitable for ceramic additive manufacturing.
Uniformly mixing the photosensitive resin, the photoinitiator, the dispersant and the viscosity regulator to obtain a resin mixture;
adding the powder B into the resin mixture, uniformly mixing, placing the mixture into a vacuum defoaming machine for defoaming, and filtering to obtain ceramic slurry with the solid content of 87%/wt, which can be used for additive manufacturing;
and forming the ceramic slurry by using a photocuring method to obtain a ceramic substrate biscuit, degreasing the ceramic substrate biscuit, and sintering in a pneumatic furnace by using a tool and a powder burying sintering method to obtain the high-thermal-conductivity aluminum nitride-based ceramic substrate with a complex configuration.
And (3) putting the mixed powder solution into a vacuum defoaming machine, mixing for 1-10 hours, then putting the mixed powder solution into a vacuum drying box, carrying out vacuum treatment for 5-12 hours at normal temperature to obtain uniformly mixed powder, adding the uniformly mixed powder into the resin mixture after the surface modification in the step 4), mixing uniformly, then putting the mixture into the vacuum defoaming machine, carrying out vacuum defoaming for 1-10 hours, removing bubbles in the slurry, and filtering to obtain the high-thermal-conductivity aluminum nitride-based ceramic slurry suitable for additive manufacturing.
Placing the obtained slurry into photocuring equipment, and forming by adopting a photocuring method to obtain a ceramic substrate biscuit; the laser power of the light curing equipment is 800-2400 mW, the laser scanning speed is 2000-5000mm/s, and the scanning layer thickness is 0.03-0.05mm.
Degreasing and sintering a ceramic substrate biscuit obtained by molding through a photocuring method, loading the degreased ceramic substrate biscuit into a tool, carrying out aluminum oxide powder embedding treatment, heating to 1200-1300 ℃ at a heating rate of 1-1.5 ℃/min, keeping the temperature for 1-2h, then heating to 1600-1700 ℃ at a heating rate of 5-10 ℃/min, keeping the temperature for 1-3h, and carrying out furnace cooling after the heating is finished, thereby finally obtaining the high-thermal-conductivity aluminum nitride-based ceramic substrate with a complex configuration.
Example 1:
step 1, taking 51 parts of aluminum nitride powder (wherein the micron-level and submicron-level is 1;
step 2, uniformly mixing the aluminum nitride powder in absolute ethyl alcohol to obtain a mixed powder solution;
step 3, putting the mixed powder solution into a ball mill, adding zirconia balls for grinding to perform uniform dispersion treatment, performing uniform ball milling for 20 hours, performing vacuum defoaming, drying and crushing on the uniformly mixed powder solution, and screening by using a screen to obtain powder A with the particle size of 15-53 mu m suitable for additive manufacturing;
and 4, adding 3 parts of powder surface modifier into the powder A, adding zirconia ball milling beads for uniform dispersion, carrying out ball milling for 20 hours, and crushing and screening the uniformly mixed powder to obtain the finally used powder B with the particle size of 15-35 mu m suitable for ceramic additive manufacturing.
Step 5, uniformly mixing 40 parts of photosensitive resin, 1.2 parts of photoinitiator, 1.6 parts of dispersant and 3.2 parts of viscosity regulator to obtain a resin mixture;
step 6, adding the powder B into the resin mixture, uniformly mixing, placing the mixture into a vacuum defoaming machine for defoaming, and filtering to obtain ceramic slurry for additive manufacturing;
and 7: placing the obtained ceramic slurry into photocuring equipment, and forming by adopting a photocuring method, wherein the laser power is 210mW, the laser scanning speed is 2200mm/s, and the scanning distance is 0.05mm, so that an aluminum nitride-based ceramic substrate biscuit with an inner flow channel can be obtained;
and 8: degreasing the obtained ceramic substrate biscuit;
and step 9: putting the degreased ceramic substrate biscuit into a tool and embedding Al 2 O 3 In the powder, heating to 1250 ℃ at a heating rate of 1.2 ℃/min, keeping the temperature for 1.5h, then heating to 1650 ℃ at a heating rate of 6.5 ℃/min, keeping the temperature for 2h, cooling along with the furnace after the heating is finished, and finally obtaining a high-thermal-conductivity aluminum nitride-based ceramic substrate with an inner runner, wherein the prepared aluminum nitride-based ceramic substrate structure is shown in fig. 2 b; an aluminum nitride-based ceramic substrate prepared based on conventional processes using the same ratio of materials as in example 1 is shown in fig. 2 a.
Example 2:
step 1, 53 parts of aluminum nitride powder (wherein the micron-level and submicron-level 1;
step 2, uniformly mixing the aluminum nitride powder in absolute ethyl alcohol to obtain a mixed powder solution;
step 3, putting the mixed powder solution into a ball mill, adding zirconia balls for grinding, uniformly dispersing, uniformly ball-milling for 24 hours, performing vacuum defoaming, drying and crushing on the uniformly mixed powder solution, and screening by using a screen to obtain powder A with the particle size of 15-53 mu m suitable for additive manufacturing;
and 4, adding 3.5 parts of powder surface modifier into the powder A, adding zirconia ball grinding beads for uniform dispersion, carrying out ball milling for 24 hours, and crushing and screening the uniformly mixed powder to obtain the finally used powder B with the particle size of 15-35 mu m suitable for ceramic additive manufacturing.
Step 5, mixing 37.5 parts of photosensitive resin, 1.2 parts of photoinitiator, 1.6 parts of dispersant and 3.2 parts of viscosity regulator uniformly to obtain a resin mixture;
step 6, adding the powder B into the resin mixture, uniformly mixing, placing the mixture into a vacuum defoaming machine for defoaming, and filtering to obtain ceramic slurry for additive manufacturing;
and 7: placing the obtained ceramic slurry into photocuring equipment, and forming by adopting a photocuring method, wherein the laser power is 220mW, the laser scanning speed is 2000mm/s, and the scanning distance is 0.06mm, so that an aluminum nitride-based ceramic substrate biscuit with an inner flow channel can be obtained;
and 8: degreasing the obtained ceramic substrate biscuit;
and step 9: putting the degreased ceramic substrate biscuit into a tool and embedding Al 2 O 3 And (3) heating the powder to 1250 ℃ at the heating rate of 1.2 ℃/min, preserving heat for 1.5h, then heating to 1650 ℃ at the heating rate of 6.5 ℃/min, preserving heat for 2h, and cooling along with the furnace after the heating is finished, thereby finally obtaining the high-thermal-conductivity aluminum nitride-based ceramic substrate with the inner flow channel.
According to the method, the ceramic substrate structure is prepared by adopting the conventional process and the method of the invention, the experiment comparison is carried out by adopting powder materials with different proportions, the specific test is shown in the following table 1, and the thermal shock performance and the thermal conductivity parameters of the ceramic substrate structure prepared by adopting the conventional process and the method of the invention are shown in the following table 2.
Table 1 shows the ratio of ceramic substrates prepared in different proportions
Table 2 shows the thermal shock performance and thermal conductivity parameters of the ceramic substrate prepared in the above example
As shown in table 2, the thermal shock performance and the heat conductivity parameters of the ceramic substrate structure prepared in example 1 and the conventional process show that the ceramic substrate with the inner flow channel prepared by using the aluminum nitride-based ceramic slurry of the present invention is improved in performance in various aspects compared with the aluminum nitride-based ceramic substrate prepared by using the conventional process material.
Claims (10)
1. The additive manufacturing ceramic slurry for the aluminum nitride ceramic substrate is characterized by comprising the following components in parts by weight: 50 to 65 portions of aluminum nitride powder, 1 to 7 portions of powder surface modifier, 35 to 55 portions of photosensitive resin, 0.8 to 3.5 portions of photoinitiator, 1.5 to 3.5 portions of dispersant and 3 to 4 portions of viscosity regulator.
2. The additive manufacturing ceramic slurry for the aluminum nitride ceramic substrate according to claim 1, wherein the aluminum nitride powder has a particle size of 0.5-5 μm and a purity of 99.9% or higher.
3. The aluminum nitride ceramic substrate additive manufacturing ceramic slurry of claim 1, wherein the powder surface modifier is one or more of dimer acid, fatty acid, pentaerythritol oleate, and the like.
4. The additive manufacturing ceramic slurry for the aluminum nitride ceramic substrate according to claim 1, wherein the photosensitive resin is one or more of aliphatic epoxy resin, polyacrylic resin and epoxy acrylate.
5. The additive manufacturing ceramic slurry for the aluminum nitride ceramic substrate according to claim 1, wherein the photoinitiator is one or a mixture of TPO and DMPA; the dispersant is a hyper-dispersant, and the viscosity regulator is one or a mixture of glycerol and PEG 200.
6. The preparation method of the ceramic slurry for the additive manufacturing of the aluminum nitride ceramic substrate is characterized by comprising the following steps of:
s1, taking 45-65 parts of aluminum nitride powder, 1-7 parts of powder surface modifier, 35-55 parts of photosensitive resin, 0.8-3.5 parts of photoinitiator, 1.5-3.5 parts of dispersant and 3-4 parts of viscosity regulator according to parts by weight;
s2, uniformly mixing the aluminum nitride powder in absolute ethyl alcohol to obtain a mixed powder solution;
s3, ball-milling the mixed powder solution, uniformly mixing, carrying out vacuum defoaming, drying and crushing on the uniformly mixed powder solution, and screening by using a screen to obtain powder A with the particle size of 15-53 mu m;
s4, adding a powder surface modifier into the powder A, adding zirconia ball grinding beads for uniform dispersion, and crushing and screening the uniformly mixed powder A to obtain powder B with the grain size of 15-35 mu m;
s5, uniformly mixing the photosensitive resin, the photoinitiator, the dispersant and the viscosity regulator to obtain a resin mixture; and adding the powder B into the resin mixture, uniformly mixing, defoaming, and filtering to obtain the ceramic slurry.
7. A preparation method of a high-thermal-conductivity aluminum nitride-based ceramic substrate is characterized by comprising the following steps:
carrying out photocuring forming on the ceramic slurry of claim 1 or the ceramic slurry obtained by the preparation method of claim 6 to obtain a ceramic substrate biscuit, and carrying out degreasing treatment on the obtained ceramic substrate biscuit; putting the degreased ceramic substrate biscuit into a tool and embedding Al 2 O 3 And (3) cooling the powder along with the furnace after high-temperature treatment to finally obtain the high-thermal-conductivity aluminum nitride-based ceramic substrate with the inner flow channel.
8. The method for preparing the high-thermal-conductivity aluminum nitride-based ceramic substrate as claimed in claim 7, wherein the obtained ceramic slurry is placed in a photocuring device, and is shaped by a photocuring method to obtain a ceramic substrate biscuit; the laser power of the light curing equipment is 800-2400 mW, the laser scanning speed is 2000-5000mm/s, and the scanning layer thickness is 0.03-0.05mm.
9. The preparation method of the high-thermal-conductivity aluminum nitride-based ceramic substrate according to claim 7, wherein the degreased ceramic substrate biscuit is loaded into a tool, aluminum oxide powder embedding treatment is carried out, the temperature is increased to 1200-1300 ℃ according to the temperature increase rate of 1-1.5 ℃/min, the temperature is kept for 1-2h, then the temperature is increased to 1600-1700 ℃ according to the temperature increase rate of 5-10 ℃/min, the temperature is kept for 1-3h, furnace cooling is carried out after the temperature is increased, and finally the high-thermal-conductivity aluminum nitride-based ceramic substrate with a complex configuration can be obtained.
10. The method as claimed in claim 7, wherein the thermal conductivity of the prepared aluminum nitride substrate is 150-180W/(m.k), and the prepared aluminum nitride substrate has internal flow channels.
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