CN117003565B - Method for manufacturing composite ceramic substrate and composite ceramic substrate - Google Patents
Method for manufacturing composite ceramic substrate and composite ceramic substrate Download PDFInfo
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- CN117003565B CN117003565B CN202310943667.4A CN202310943667A CN117003565B CN 117003565 B CN117003565 B CN 117003565B CN 202310943667 A CN202310943667 A CN 202310943667A CN 117003565 B CN117003565 B CN 117003565B
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- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention provides a manufacturing method of a composite ceramic substrate and the composite ceramic substrate. The manufacturing method of the composite ceramic substrate comprises the steps of providing a first green film, wherein the first green film is an alumina green film, providing a second green film, wherein the second green film is made of a first mixture comprising alumina and yttrium-stabilized zirconia, providing a third green film, wherein the third green film is made of a second mixture comprising alumina and lanthanum oxide, and manufacturing a composite green body with a multilayer structure through lamination of the first green film, the second green film and the third green film, wherein the first green film is arranged between the second green film and the third green film in the composite green body so as to separate the second green film and the third green film, and performing sintering treatment on the composite green body to obtain the composite ceramic substrate with the laminated structure. According to the manufacturing method of the composite ceramic substrate, the bending strength of the obtained composite ceramic substrate is obviously enhanced, and the mechanical property is excellent.
Description
Technical Field
The invention relates to the technical field of electronic packaging, in particular to a manufacturing method of a composite ceramic substrate and the composite ceramic substrate.
Background
The ceramic heat dissipation substrate has an irreplaceable role in the technical field of electronic packaging, and mainly provides a heat dissipation channel and insulation protection for the bearing chip. Alumina (Al 2O3) ceramic is used as a type of ceramic heat dissipation substrate, and can be widely applied to the technical field of electronic packaging because of the advantages of low cost, rich sources, high chemical stability, low thermal expansion coefficient, high corrosion resistance and the like. With the gradual development of semiconductor packaging devices in the directions of high power, integration, small size and the like, higher requirements on the mechanical properties of alumina-based ceramic substrates are also put forward in the field. Therefore, there is a need to improve the mechanical properties of alumina-based ceramic substrates.
Disclosure of Invention
In view of the above-described problems in the related art, the present invention provides a method of manufacturing a composite ceramic substrate and a composite ceramic substrate, in which a first green film formed of alumina is provided between a second green film comprising yttrium-stabilized zirconia (3Y-ZrO 2) and a third green film comprising lanthanum oxide (La 2O3), so that the second green film comprising yttrium-stabilized zirconia and the third green film comprising lanthanum oxide are separated from each other without contact, thereby avoiding the occurrence of the phenomenon that ZrO 2 is converted from tetragonal phase into cubic phase at high temperature due to the presence of La 2O3, and thus, a composite ceramic substrate having a laminated structure is obtained by stacking the first green film, the second green film and the third green film, whereby simultaneous introduction of lanthanum oxide and yttrium-stabilized zirconia into the composite ceramic substrate can be achieved, and the influence of lanthanum oxide and yttrium-stabilized zirconia on the overall mechanical properties due to mutual contact during high-temperature sintering is avoided.
According to an aspect of the present invention, there is provided a method of manufacturing a composite ceramic substrate including providing a first green film that is an alumina green film, providing a second green film that is made of a first mixture including alumina and yttrium-stabilized zirconia, providing a third green film that is made of a second mixture including alumina and lanthanum oxide, manufacturing a composite green body having a multilayer structure by stacking the first green film, the second green film, and the third green film, wherein in the composite green body having a multilayer structure, the first green film is disposed between the second green film and the third green film to separate the second green film and the third green film, and sintering the composite green body to obtain the composite ceramic substrate having a stacked structure.
In some embodiments, the composite green body having a multilayer structure includes two outer green bodies and an inner green body disposed between the two outer green bodies, the outer green bodies including a first green body layer and a second green body layer disposed between the first green body layers, the inner green body including a third green body layer, wherein the first green body layer is formed from at least one first green body film, the second green body layer is formed from at least one second green body film, and the third green body layer is formed from at least one third green body film.
In other embodiments, the composite green body having a multilayer structure includes an outer green body including a first green body layer formed from at least one first green body film and a third green body layer formed from at least one third green body film, and an inner green body disposed between the outer green bodies, the inner green body including a second green body layer, wherein the first green body layer is formed from at least one first green body film and the second green body layer is formed from at least one second green body film.
In some embodiments, the first green film has a thickness in the range of 100 μm to 500 μm, and/or the second green film has a thickness in the range of 100 μm to 500 μm, and/or the third green film has a thickness in the range of 100 μm to 500 μm.
In some embodiments, the skin layer of the composite green body is a first green layer.
In some embodiments, the step of providing a second green film includes providing the first mixture, providing a second additive including a second binder, forming the first mixture and the second additive into a second slurry, and forming the second slurry into a corresponding second green film.
In some embodiments, the weight ratio of alumina to yttrium-stabilized zirconia is (48-58): 4-14.
In some embodiments, the alumina has a particle size of 0.1 μm to 1 μm and/or the yttrium stabilized zirconia has a particle size of 0.1 μm to 0.5 μm.
In some embodiments, the step of providing a third green film includes providing the second mixture, providing a third additive including a third binder, forming the first mixture and the third additive into a third slurry, and forming the third slurry into a corresponding third green film.
In some embodiments, the weight ratio of alumina to lanthanum oxide is (48-58): 4-14.
In some embodiments, the alumina has a particle size of 0.1 μm to 1 μm and/or the lanthanum oxide has a particle size of 0.05 μm to 0.5 μm.
In some embodiments, the sintering process includes the steps of heating the composite green body to 800-1200 ℃ at a heating rate of 5-10 ℃ per minute, heating to 1550-1650 ℃ at a heating rate of 2-5 ℃ per minute, maintaining for 1-2 hours, cooling to 800-1200 ℃ at a cooling rate of 2-5 ℃ per minute, and finally cooling to room temperature with a furnace.
According to a second aspect of the present invention, there is provided a composite ceramic substrate having a laminated structure, the composite ceramic substrate having a laminated structure including a first material layer, a second material layer and a third material layer, the first material layer being an alumina layer, the second material layer being a mixed layer of alumina and yttrium-stabilized zirconia, the third material layer being a mixed layer of alumina and lanthanum oxide, wherein the first material layer is disposed between the second material layer and the third material layer so as to separate the second material layer and the third material layer.
In some embodiments, the surface layer of the composite ceramic substrate is a first material layer.
In some embodiments, the composite ceramic substrate includes an outer cladding layer including a first material layer and a second material layer disposed between the first material layers, and a core disposed between the outer cladding layers, the core including a third material layer.
In other embodiments, the composite ceramic substrate includes an outer cladding layer including a first material layer and a third material layer disposed between the first material layers and a core disposed between the outer cladding layers, the core including a second material layer.
According to the manufacturing method of the composite ceramic substrate and the composite ceramic substrate, the rod-shaped reinforcing effect of LaAl 11O18 is reserved, and the phase change reinforcing effect of yttrium stabilized zirconia is ensured, so that the bending strength of the alumina-based composite ceramic substrate is obviously enhanced (the mechanical property is excellent).
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings.
FIG. 1 is a schematic structural diagram of a composite green body according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a composite ceramic substrate according to an embodiment of the present invention.
In the drawings, like parts are given like reference numerals, and the drawings are not drawn to scale.
Symbol description
10. The composite green body, 11, an outer green body, 111, a first green body layer, 112, a second green body layer, 12, an inner green body, 121, a third green body layer;
20. The composite ceramic substrate comprises 21 parts of an outer coating layer, 211 parts of a first material layer, 212 parts of a second material layer, 22 parts of a core part, 221 parts of a third material layer.
Detailed Description
The present application will be further described in detail with reference to the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present application more apparent, and the described embodiments should not be construed as limiting the present application, and all other embodiments obtained by those skilled in the art without making any inventive effort are within the scope of the present application.
In the following description, reference is made to "some embodiments" which describe a subset of all possible embodiments, but it is to be understood that "some embodiments" can be the same subset or different subsets of all possible embodiments and can be combined with one another without conflict.
If a similar description of "first\second\third" appears in the application document, the following description is added, in which the terms "first\second\third" are merely distinguishing between similar objects and do not represent a particular ordering of the objects, it being understood that the "first\second\third" may be interchanged in a particular order or precedence, where allowed, to enable embodiments of the application described herein to be practiced in an order other than that illustrated or described herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing embodiments of the application only and is not intended to be limiting of the application.
In the present invention, the terms "upper", "lower", "top" and "bottom" are defined based on the orientation of the product when the product is in normal use and is placed upright. And should not be construed as limiting the embodiments of the invention in any way. In the context of the present invention, it is to be understood that when an element is referred to as being connected to another element, it can be directly or indirectly connected unless it is explicitly stated that the element is directly connected to the other element.
The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more.
While certain embodiments have been shown and described, it would be appreciated by those skilled in the art that changes and modifications may be made without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.
In the field of ceramic substrate manufacturing, the introduction of other phases (for example, lanthanum oxide) into an alumina ceramic matrix is a common reinforcing means for alumina ceramics, and the reinforcing mechanism mainly comprises fine-grain reinforcement, phase-change reinforcement, whisker reinforcement and the like. Lanthanum oxide is a common rare earth oxide, the lanthanum oxide is introduced into the alumina ceramic matrix to effectively reduce the grain size of the alumina ceramic and realize fine grain strengthening, and Al 2O3 and La 2O3 can generate rod-shaped LaAl 11O18 at high temperature to effectively enhance the bending strength of the alumina ceramic.
The crystalline forms of ZrO 2 are mainly classified into monoclinic, tetragonal and cubic, pure ZrO 2 is mainly classified into monoclinic crystalline forms, and the crystalline form of ZrO 2 is transformed at a certain temperature by introducing rare earth elements into ZrO 2. However, the tetragonal ZrO 2 has the best mechanical properties, so that yttrium doping is carried out on the zirconia to obtain the tetragonal yttrium-stabilized zirconia (3Y-ZrO 2). The yttrium-stabilized zirconia has the characteristics of phase change reinforcement and toughening, and the crystal form of the yttrium-stabilized zirconia can undergo phase change from tetragonal to monoclinic in the fracture process of the ceramic, so that a large amount of fracture energy is consumed, and the ceramic has the effect of phase change reinforcement. And the yttrium-stabilized zirconia doped in the alumina ceramic matrix can also effectively inhibit the growth of alumina grains, and has the function of fine grain strengthening.
The two reinforcing means for adding other phases into the alumina ceramic matrix can obtain the alumina composite ceramic with certain mechanical properties. However, with the gradual development of semiconductor packaging devices in the directions of high power, integration, small size and the like, higher requirements on the mechanical properties of alumina-based ceramic substrates will be also put forward in the field. Therefore, there is a need to improve the mechanical properties of alumina-based ceramic substrates.
When lanthanum oxide and yttrium stabilized zirconia are doped in alumina ceramic at the same time, the obtained alumina ceramic substrate has limited reinforcing effect, which is found to be because La 2O3 can promote the transformation of 3Y-ZrO 2 from tetragonal phase to cubic phase at high temperature, the mechanical property of cubic phase ZrO 2 is poor, and the phase transformation reinforcement cannot be realized in the fracture process, so that the mechanical property of the alumina ceramic substrate is poor.
According to a first aspect of an embodiment of the present application, there is provided a method for manufacturing a composite ceramic substrate, wherein the method for manufacturing a composite ceramic substrate includes providing a first green film that is an alumina green film, providing a second green film that is made of a first mixture including alumina and yttrium-stabilized zirconia, providing a third green film that is made of a second mixture including alumina and lanthanum oxide, and manufacturing a composite green body having a multilayer structure by stacking the first green film, the second green film, and the third green film, wherein in the composite green body having a multilayer structure, the first green film is disposed between the second green film and the third green film to separate the second green film and the third green film, and performing a sintering process on the composite green body to obtain the corresponding composite ceramic substrate having a stacked structure.
In the present embodiment, the green film is a green film which is not sintered and is formed into a film shape by pressing powder (powder).
According to the manufacturing method of the composite ceramic substrate provided by the embodiment of the application, when the first green film, the second green film and the third green film are laminated in the thickness direction, the first green film formed by alumina is arranged between the second green film with yttrium-stabilized zirconia and the third green film with lanthanum oxide, so that the second green film with yttrium-stabilized zirconia and the third green film with lanthanum oxide are separated from each other in the thickness direction and are not contacted, the situation that ZrO 2 is converted into a cubic phase from a tetragonal phase at a high temperature due to the existence of La 2O3 is avoided, and the composite ceramic substrate with a laminated structure is obtained through compounding of the first green film, the second green film and the third green film, the lanthanum oxide and the yttrium-stabilized zirconia can be simultaneously introduced into the composite ceramic substrate, and the phenomenon that the lanthanum oxide and the yttrium-stabilized zirconia are contacted with each other in a high-temperature sintering process to influence the overall mechanical performance is avoided.
According to the composite ceramic substrate, the rod-shaped reinforcing effect of LaAl 11O18 is reserved, and the phase change reinforcing effect of yttrium-stabilized zirconia is ensured, so that the bending strength of the alumina-based composite ceramic substrate is obviously enhanced (the mechanical property is excellent).
Hereinafter, a method of manufacturing a composite ceramic substrate according to the present application will be specifically described with reference to specific embodiments.
Providing a first green film
In an embodiment, the step of providing a first green film comprises preparing a first green film. Wherein the step of preparing the first green film comprises providing an alumina powder, providing a first additive comprising a first binder, preparing the alumina powder with the first additive into a first slurry, and preparing the first slurry into the first green film.
According to the application, the alumina powder has a preset particle size, and the particle size of the powder affects the overall strength of the formed composite green body. If the particle size is too large, the pores of the formed composite green body are too large, the whole structure of the green body is loose, and the strength of the composite green body is affected, and if the particle size is too small, the cost is increased due to the large difficulty of the powder process. In some embodiments, the particle size of the alumina powder is in the range of 0.1 μm to 1 μm. Here, the particle size difference of the alumina powder is smaller (more uniform), so that the structures at different areas of the first green film are more uniform, and the strength of the formed composite green body is further ensured. The particle size of the above-mentioned material may be the maximum length of the particles of the material, and the material is not particularly limited to have a spherical or spheroid shape. For example, but not limited to, when a material has an oval shape, the particle size dimension of the material may refer to the length of its major axis.
In some embodiments, a first additive is provided that includes a first binder, which in exemplary embodiments may be polyvinyl butyral, which has a high bond strength and good abrasion, oil, and heat resistance. The weight ratio of the alumina powder to the first binder may be (60-70): 3-4.
According to the application, the first additive may comprise, in addition to the first binder, an auxiliary agent. Wherein the auxiliary agent comprises a plasticizer and/or a dispersant. In an exemplary embodiment, the plasticizer may be butyl benzyl phthalate and the dispersant may be triolein. The weight ratio of the alumina powder to the plasticizer may be (60-70): 3-4, and the weight ratio of the alumina powder to the dispersant may be (60-70): 1-2.
In some embodiments, the step of forming the alumina powder and the first additive into a first slurry includes mixing the alumina powder and the first additive in a solvent and then forming the slurry by ball milling. In an exemplary embodiment, the solvent is a mixed solvent of polyols, which can increase the solvency of the material and can improve the control of drying speed, slurry rheology, cost and safety. Specifically, the mixed solvent of the polyalcohol can comprise n-butanol, isopropanol and absolute ethyl alcohol, wherein the volume ratio of the n-butanol to the isopropanol to the absolute ethyl alcohol is (0.5-1): 1-2. The weight ratio of the alumina powder to the mixed solvent can be (60-70): 25-35.
In an exemplary embodiment, 62 parts by mass of alumina powder, 1.2 parts by mass of triolein, 3.1 parts by mass of polyvinyl butyral, and 3.7 parts by mass of butyl benzyl phthalate are weighed, 30 parts by mass of a mixed solvent of polyols (the volume ratio of n-butanol to isopropanol to absolute ethanol is 1:2:2) are weighed, the above materials are mixed in the above solvents, and then ball milling media are added and uniformly mixed by a planetary ball mill (the ball milling speed is set to be 250r/min-350r/min for 6h-10 h), so that the alumina ceramic casting slurry, namely the first slurry, is prepared. Pouring the first slurry into a trough of a casting machine, setting the height of a scraper to be 100-500 mu m, the baseband speed to be 0.1-0.3 m/min and the drying temperature to be 40-55 ℃, volatilizing the solvent and preparing the alumina ceramic green sheet, namely the first green film.
According to the application, the thickness of the first green film is in the range of 100 μm to 500 μm. The thickness of the green film is determined according to the height of the scraper, when the thickness of the green film is lower than 100 mu m, the thickness is too thin, so that the strength of the green film is lower, cracking easily occurs when the base band is peeled off, and when the thickness of the green film is greater than 500 mu m, the thickness is too thick, so that the surface and the inner drying speeds of the green film are inconsistent, and the green film is easy to crack and defect.
Providing a second green film
In an embodiment, the step of providing a second green film comprises preparing the second green film. Wherein the step of preparing the second green film comprises providing a first mixture comprising alumina powder and yttrium-stabilized zirconia powder, providing a second additive comprising a second binder, forming the first mixture and the second additive into a second slurry, and forming the second slurry into the second green film.
In the first mixture, the weight ratio of the alumina powder to the yttrium-stabilized zirconia powder is (48-58): 4-14.
According to the application, the powder forming the first mixture has a preset particle size, and the particle size of the powder influences the overall strength of the formed composite green body. If the particle size is too large, the pores of the formed composite green body are too large, the whole structure of the green body is loose, and the strength of the composite green body is affected, and if the particle size is too small, the cost is increased due to the large difficulty of the powder process. In some embodiments, the alumina powder has a particle size in the range of 0.1 μm to 1 μm and the yttrium stabilized zirconia has a particle size in the range of 0.1 μm to 0.5 μm. Here, the particle size of the alumina powder and the particle size of the yttrium-stabilized zirconia powder can be made to be small (relatively uniform), so that the structures at different areas of the second green film are relatively uniform, and the strength of the formed composite green body is further ensured. The particle size of the above-mentioned material may be the maximum length of the particles of the material, and the material is not particularly limited to have a spherical or spheroid shape. For example, but not limited to, when a material has an oval shape, the particle size dimension of the material may refer to the length of its major axis.
In some embodiments, a second additive is provided that includes a second binder, which may or may not be the same as the first binder, and in some exemplary embodiments, may also be polyvinyl butyral, which has a high bond strength and good abrasion, oil, and heat resistance. The weight ratio of the first mixture to the second binder may be (60-70): 3-4.
According to the application, the second additive may comprise, in addition to the second binder, an auxiliary agent. Wherein the auxiliary agent comprises an enhancer and/or a dispersant. May be the same as or different from the additive used to form the first green film. In an exemplary embodiment, the plasticizer may be butyl benzyl phthalate and the dispersant may be triolein. The weight ratio of the first mixture to the plasticizer may be (60-70): 3-4, and the weight ratio of the first mixture to the dispersant may be (60-70): 1-2.
In some embodiments, the step of forming the first mixture and the second additive into a second slurry includes mixing the first mixture and the second additive in a solvent and then forming the second slurry by ball milling. In an exemplary embodiment, the solvent is a mixed solvent of polyols, which can increase the solvency of the material and can improve the control of drying speed, slurry rheology, cost and safety. In an exemplary embodiment, the mixed solvent includes n-butanol to isopropanol to absolute ethanol, wherein the volume ratio of n-butanol to isopropanol to absolute ethanol is (0.5-1): 1-2.
In an exemplary embodiment, 48 to 58 parts by mass of alumina powder having a particle diameter of 0.1 μm to 1 μm, 4 to 14 parts by mass of yttrium-stabilized zirconia powder having a particle diameter of 0.1 μm to 0.5 μm, 1.2 parts by mass of glyceryl trioleate, 3.1 parts by mass of polyvinyl butyral and 3.7 parts by mass of butyl benzyl phthalate are weighed, 30 parts by mass of a mixed solvent of polyhydric alcohols (volume ratio of n-butanol to isopropanol to absolute ethanol is 1:2) are weighed, the above materials are mixed into the above solvents, and then ball milling media are added and mixed uniformly by a planetary ball mill (set at a ball milling rotation speed of 250r/min to 350r/min for 6h to 10 h), thereby obtaining an alumina/yttrium-stabilized zirconia ceramic casting slurry, i.e., a second slurry. Pouring the second slurry into a trough of a casting machine, setting the height of a scraper to be 100-500 mu m, the baseband speed to be 0.1-0.3 m/min, the drying temperature to be 40-55 ℃, volatilizing the solvent and obtaining the alumina/yttrium stabilized zirconia ceramic green sheet, namely the second green film.
According to the application, the thickness of the second green film is in the range of 100 μm to 500 μm. The thickness of the green film is determined according to the height of the scraper, when the thickness of the green film is lower than 100 mu m, the thickness is too thin, so that the strength of the green film is lower, cracking easily occurs when the base band is peeled off, and when the thickness of the green film is greater than 500 mu m, the thickness is too thick, so that the surface and the inner drying speeds of the green film are inconsistent, and the green film is easy to crack and defect.
Providing a third green film
In an embodiment, the step of providing a third green film comprises preparing the third green film. The method for preparing the third green film comprises the steps of providing a second mixture comprising alumina powder and lanthanum oxide powder, providing a third additive comprising a third binder, preparing the second mixture and the third additive into third slurry, and preparing the third slurry into the third green film.
In the first mixture, the weight ratio of the alumina powder to the lanthanum oxide powder is (48-58) to (4-14).
According to the application, the powder forming the second mixture has a preset particle size, and the particle size of the powder influences the overall strength of the formed composite green body. If the particle size is too large, the pores of the formed composite green body are too large, the whole structure of the green body is loose, and the strength of the composite green body is affected, and if the particle size is too small, the cost is increased due to the large difficulty of the powder process. In the examples, the particle size of the alumina powder was in the range of 0.1 μm to 1 μm, and the particle size of the lanthanum oxide was in the range of 0.05 μm to 0.5 μm. Here, the particle size of the alumina powder and the particle size of the lanthanum oxide powder are not greatly different (are relatively uniform), so that the structures of the third green film in different areas are relatively uniform, and the strength of the formed composite green body is further ensured. The particle size of the above-mentioned material may be the maximum length of the particles of the material, and the material is not particularly limited to have a spherical or spheroid shape. For example, but not limited to, when a material has an oval shape, the particle size dimension of the material may refer to the length of its major axis.
In some embodiments, a third additive is provided that includes a third binder, which may or may not be the same as the first binder, and which may be polyvinyl butyral, which has a high bond strength and good abrasion, oil, and heat resistance. The weight ratio of the second mixture to the second binder may be (60-70): 3-4.
According to the application, the third additive may comprise, in addition to the third binder, an auxiliary agent. Wherein the auxiliary agent comprises an enhancer and/or a dispersant. May be the same as or different from the additive used to form the first green film. In an exemplary embodiment, the plasticizer may be butyl benzyl phthalate and the dispersant may be triolein. The weight ratio of the second mixture to the plasticizer may be (60-70): 3-4, and the weight ratio of the second mixture to the dispersant may be (60-70): 1-2.
In some embodiments, the step of forming the second mixture with the third additive into a third slurry includes mixing the second mixture with the third additive in a solvent and then forming the third slurry by ball milling. In an exemplary embodiment, the solvent is a mixed solvent of polyols, which can increase the solvency of the material and can improve the control of drying speed, slurry rheology, cost and safety. In an exemplary embodiment, the mixed solvent includes n-butanol to isopropanol to absolute ethanol, wherein the volume ratio of n-butanol to isopropanol to absolute ethanol is (0.5-1): 1-2.
In an exemplary embodiment, 48 to 58 parts by mass of alumina powder having a particle diameter of 0.1 μm to 1 μm, 4 to 14 parts by mass of lanthanum oxide powder having a particle diameter of 0.05 μm to 0.5 μm, 1.2 parts by mass of glyceryl trioleate, 3.1 parts by mass of polyvinyl butyral and 3.7 parts by mass of butyl benzyl phthalate are weighed, 30 parts by mass of a mixed solvent of polyhydric alcohols (n-butanol: isopropanol: absolute ethanol in a volume ratio of 1:2:2) are weighed, the above materials are mixed into the above solvents, and then ball milling medium is added and mixed uniformly by a planetary ball mill (set at a ball milling rotation speed of 250r/min to 350r/min for 6h to 10 h), thereby obtaining an alumina/lanthanum oxide ceramic tape casting slurry, i.e., a third slurry. Pouring the third slurry into a trough of a casting machine, setting the height of a scraper to be 100-500 mu m, the baseband speed to be 0.1-0.3 m/min, the drying temperature to be 40-55 ℃, and volatilizing the solvent to obtain the alumina/lanthanum oxide ceramic green sheet, namely the third green film.
According to the application, the thickness of the third green film is in the range of 100 μm to 500 μm. The thickness of the green film is determined according to the height of the scraper, when the thickness of the green film is lower than 100 mu m, the thickness is too thin, so that the strength of the green film is lower, cracking easily occurs when the base band is peeled off, and when the thickness of the green film is greater than 500 mu m, the thickness is too thick, so that the surface and the inner drying speeds of the green film are inconsistent, and the green film is easy to crack and defect.
Forming a composite green body
According to the present application, a composite green body having a multilayer structure is obtained by laminating a first green film, a second green film, and a third green film in the thickness direction, and disposing the first green film between the second green film and the third green film such that the second green film and the third green film are spaced apart from each other in the thickness direction;
According to the present application, the first green film, the second green film, and the third green film may be laminated in the thickness direction in various ways, thereby forming an initial green body. In exemplary embodiments, the thickness of each layer in the initial green body may be set based on the thickness of the desired composite ceramic substrate, and in some exemplary embodiments, each layer may be formed from one or more corresponding green films. In an exemplary embodiment, when the thickness of the composite ceramic substrate is 0.5mm to 1mm, in the initial green body, one alumina green body layer may be formed in1 to 4 first green body films, preferably, one alumina green body layer may be formed in2 to 3 first green body films, and respective composite green body layers may be formed in2 to 6 second green body films or third green body films, preferably, respective composite green body layers may be formed in 3 to 4 second green body films or third green body films.
In order to make the strength of the composite substrate higher, the thickness of the composite green layer may be made thicker than the thickness of the aluminum oxide-only green layer. After the initial blank is formed, the initial blank is pressed, specifically, the initial blank is placed in a warm isostatic press, the temperature is set to be 100 ℃, the holding pressure is set to be 30MPa, and the holding time is set to be 10 minutes, so that a composite blank with good interlayer bonding is obtained.
In some embodiments, the composite green body 10 having a multi-layer structure includes an outer green body 11 and an inner green body 12 disposed between the outer green bodies 11, wherein the outer green body 11 includes a first green layer 111 and a second green layer 112 disposed between the first green layers 111, and the inner green body 12 includes a third green layer 121. Wherein the first green layer is formed from at least one first green film, the second green layer is formed from at least one second green film, and the third green layer is formed from at least one third green film.
In other embodiments, a composite green body having a multilayer structure includes an outer green body including a first green film and a third green film disposed between the first green films, and an inner green body disposed between the outer green bodies, the inner green body including a second green film. Wherein the first green layer is formed from at least one first green film, the second green layer is formed from at least one second green film, and the third green layer is formed from at least one third green film.
As shown in fig. 1, the composite green body 10 having the multi-layered structure includes two outer-layer green bodies 11 and an inner-layer green body 12 disposed between the two outer-layer green bodies 11, wherein the outer-layer green body 11 includes two first green body layers 111 and a second green body layer 112 disposed between the two first green body layers 111, and the inner-layer green body 12 includes a third green body layer 121. Wherein the first green layer 111 is formed from two first green films, the second green layer 112 is formed from three second green films, and the third green layer 113 is formed from three third green films.
The layered structure involves a problem of internal stress, and because of the different thermal expansion coefficients of the different material layers, the junction between the different material layers is correspondingly subjected to tensile stress or compressive stress, the thermal expansion coefficient of 3Y-ZrO 2 is larger than that of Al 2O3, and the surface layer of the composite blank is set as the first green layer, i.e., the alumina layer. On one hand, the aluminum oxide layer on the surface layer is subjected to compressive stress, and compared with the situation that the surface layer is subjected to tensile stress, the bending strength of the substrate can be greatly increased due to the fact that the surface layer is subjected to compressive stress, so that the internal stress of the formed composite ceramic substrate is enhanced, on the other hand, copper is required to be coated on the surface of the composite ceramic substrate applied to packaging components, the thermal expansion coefficients of the aluminum oxide layer and the copper layer on the surface layer of the composite ceramic substrate are closer, and the interlayer binding force is better, so that the packaging components are mounted.
Degreasing process
After forming the composite green body, the composite green body needs to be subjected to degreasing treatment in advance, and the composite green body is subjected to degreasing treatment at a relatively low temperature and a relatively low temperature, so that additives in the composite green body are removed as much as possible, and the influence of residues of the materials on the overall performance of the composite ceramic substrate is reduced. The degreasing treatment comprises the steps of heating to 300-400 ℃ at a rate of 0.5-2 ℃ per minute in an air atmosphere, preserving heat for 1h, heating to 550-700 ℃ at a heating rate of 0.5-2 ℃ per minute, preserving heat for 30-2 h, and finally cooling to room temperature along with a furnace.
Sintering process
According to the application, the initial blank is sintered in a stepwise heating mode. The sintering treatment method comprises the steps of heating the composite blank to 800-1200 ℃ at a temperature rising speed of 5-10 ℃ per minute, heating to 1550-1650 ℃ at a temperature rising speed of 2-5 ℃ per minute, preserving heat for 1-2 h, cooling to 800-1200 ℃ at a cooling speed of 2-5 ℃ per minute, and finally cooling to room temperature along with a furnace.
In these examples, the temperature is raised to between 1550 ℃ and 1650 ℃ and kept at a temperature, so that not only can Al 2O3 and La 2O3 generate rod-shaped LaAl 11O18, but also adjacent layers can be combined with each other, and densification of the structure of the composite substrate can be ensured.
According to a second aspect of the present application, there is provided a composite ceramic substrate manufactured by the manufacturing method of a composite ceramic substrate provided in each of the above embodiments, which has all the advantages of each of the above embodiments, and therefore, will not be described herein.
In some embodiments, the composite ceramic substrate has a laminated structure, and the composite ceramic substrate with the laminated structure comprises a first material layer, a second material layer and a third material layer, wherein the first material layer is an alumina layer, the second material layer is a mixed layer of alumina and yttrium stabilized zirconia, and the third material layer is a mixed layer of alumina and lanthanum oxide, and the first material layer is arranged between the second material layer and the third material layer to separate the second material layer and the third material layer.
In some embodiments, the surface layer of the composite ceramic substrate is a first material layer.
In these embodiments, the surface layer of the composite ceramic substrate is the first material layer, on one hand, the aluminum oxide layer on the surface layer is subjected to compressive stress, and compared with the case that the surface layer is subjected to tensile stress, the bending strength of the substrate can be greatly increased by the compressive stress on the surface layer, so that the internal stress of the formed composite ceramic substrate is enhanced, on the other hand, copper is required to be coated on the surface of the composite ceramic substrate applied to the packaging component, and the thermal expansion coefficients of the aluminum oxide layer and the copper layer on the surface layer of the composite ceramic substrate are closer, so that the interlayer bonding force is better, and the mounting of the packaging component is facilitated.
In some embodiments, a composite ceramic substrate includes an outer cladding layer and a core disposed between the outer cladding layers, wherein the outer cladding layer includes a first material layer and a second material layer disposed between the first material layers, the core including a third material layer, wherein the first material layer is formed from a first green layer formed from at least one first green film by a sintering process, the second green layer is formed from a second green layer formed from at least one second green film by a sintering process, and the third green layer is formed from a third green layer formed from at least one third green film by a sintering process.
In other embodiments, a composite ceramic substrate includes an outer cladding layer and a core disposed between the plurality of outer cladding layers, wherein the outer cladding layer includes a first material layer and a third material layer disposed between the first material layers, the core including a second material layer, wherein the first material layer is formed from a first green layer formed from at least one first green film by a sintering process, the second green layer is formed from a second green layer formed from at least one second green film by a sintering process, and the third green layer is formed from a third green layer formed from at least one third green film by a sintering process.
As shown in fig. 2, the composite ceramic substrate 20 includes two outer coating layers 21 and a core 22 disposed between the two outer coating layers 21, wherein the outer coating layers 21 include two first material layers 211 and a second material layer 212 disposed between the two first material layers 211, and the core 22 includes a third material layer 221.
In these embodiments, the second material layer 212 with yttrium-stabilized zirconia is sandwiched between the first material layers 211 formed of two aluminas to form the outer coating layers 21, and the third material layer 221 with lanthanum oxide is disposed between the two outer coating layers 21, and the layered structure is disposed based on the coefficient of thermal expansion between the different materials, so that the internal stress at the junction of the layers in the layered structure can be ensured, thereby ensuring better effect of internal stress enhancement and higher strength.
According to the present application, the flexural strength of the composite ceramic substrate is not less than 711MPa.
It should be appreciated that reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present application. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. It should be understood that, in various embodiments of the present application, the sequence numbers of the foregoing processes do not mean the order of execution, and the order of execution of the processes should be determined by the functions and internal logic thereof, and should not constitute any limitation on the implementation process of the embodiments of the present application. The foregoing embodiment numbers of the present application are merely for the purpose of description, and do not represent the advantages or disadvantages of the embodiments.
It should be noted that, in this document, 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.
The above-described embodiments of the apparatus are merely illustrative, and for example, the division of the units is merely a logical function division, and there may be additional divisions of actual implementation, such as multiple units or components may be combined or integrated into another system, or some features may be omitted or not performed. In addition, the various components shown or discussed may be coupled or directly coupled or communicatively coupled to each other via some interface, whether indirectly coupled or communicatively coupled to devices or units, whether electrically, mechanically, or otherwise.
The units described as separate components may or may not be physically separate, and components displayed as units may or may not be physical units, may be located in one place or distributed on a plurality of network units, and may select some or all of the units according to actual needs to achieve the purpose of the embodiment.
In addition, each functional unit in each embodiment of the present application may be integrated in one processing unit, or each unit may be separately used as a unit, or two or more units may be integrated in one unit, where the integrated units may be implemented in a form of hardware or a form of hardware plus a form of software functional unit.
It will be appreciated by those of ordinary skill in the art that implementing all or part of the steps of the above method embodiments may be implemented by hardware associated with program instructions, where the above program may be stored in a computer readable storage medium, where the program when executed performs the steps comprising the above method embodiments, where the above storage medium includes various media that may store program code, such as a removable storage device, a Read Only Memory (ROM), a magnetic disk, or an optical disk.
Or the above-described integrated units of the application may be stored in a computer-readable storage medium if implemented in the form of software functional modules and sold or used as separate products. Based on such understanding, the technical solutions of the embodiments of the present application may be embodied essentially or in part in the form of a software product stored in a storage medium, including instructions for causing a controller to perform all or part of the methods described in the embodiments of the present application. The storage medium includes various media capable of storing program codes such as a removable storage device, a ROM, a magnetic disk, or an optical disk.
The foregoing is merely an embodiment of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art can easily think about changes or substitutions within the technical scope of the present application, and the changes and substitutions are intended to be covered by the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (14)
1. A method for manufacturing a composite ceramic substrate, comprising:
providing a first green film, the first green film being an alumina green film;
providing a second green film made from a first mixture comprising alumina and yttrium-stabilized zirconia;
Providing a third green film made from a second mixture comprising alumina and lanthanum oxide;
manufacturing a composite green body having a multilayer structure by stacking a first green body film, a second green body film, and a third green body film, wherein in the composite green body having a multilayer structure, the first green body film is disposed between the second green body film and the third green body film to separate the second green body film and the third green body film;
and sintering the composite green body to obtain the composite ceramic substrate with the laminated structure.
2. The method of manufacturing a composite ceramic substrate according to claim 1, wherein the composite green body having a multilayer structure comprises an outer green body and an inner green body disposed between the outer green bodies, the outer green body comprising a first green body layer and a second green body layer disposed between the first green body layers, the inner green body comprising a third green body layer, wherein the first green body layer is formed of at least one first green body film, the second green body layer is formed of at least one second green body film, the third green body layer is formed of at least one third green body film, or
The composite blank with the multilayer structure comprises an outer layer blank and an inner layer blank arranged between the outer layer blanks, wherein the outer layer blank comprises a first green body layer and a third green body layer arranged between the first green body layers, the inner layer blank comprises a second green body layer, the first green body layer is formed by at least one first green body film, the second green body layer is formed by at least one second green body film, and the third green body layer is formed by at least one third green body film.
3. The method of manufacturing a composite ceramic substrate according to claim 1, wherein the thickness of the first green film is in the range of 100 μm to 500 μm, and/or the thickness of the second green film is in the range of 100 μm to 500 μm, and/or the thickness of the third green film is in the range of 100 μm to 500 μm.
4. The method of manufacturing a composite ceramic substrate according to claim 2, wherein the surface layer of the composite green body is a first green body layer.
5. The method of manufacturing a composite ceramic substrate according to claim 1, wherein the step of providing a second green film comprises:
Providing the first mixture;
providing a second additive comprising a second binder;
preparing a second slurry from the first mixture and the second additive;
and preparing the second slurry into a corresponding second green film.
6. The method of manufacturing a composite ceramic substrate according to claim 5, wherein the weight ratio of the alumina to the yttrium-stabilized zirconia is (48-58): 4-14.
7. The method according to claim 5, wherein the alumina has a particle size of 0.1 μm to 1 μm and/or the yttrium-stabilized zirconia has a particle size of 0.1 μm to 0.5 μm.
8. The method of manufacturing a composite ceramic substrate according to claim 1, wherein the step of providing a third green film comprises:
Providing the second mixture;
providing a third additive comprising a third binder;
preparing a third slurry from the first mixture and the third additive;
and preparing the third slurry into a corresponding third green film.
9. The method of manufacturing a composite ceramic substrate according to claim 8, wherein the weight ratio of alumina to lanthanum oxide is (48-58): 4-14.
10. The method according to claim 8, wherein the alumina has a particle size of 0.1 μm to 1 μm and/or the lanthanum oxide has a particle size of 0.05 μm to 0.5 μm.
11. The method according to claim 1, wherein the sintering process comprises heating the composite green body to 800 to 1200 ℃ at a temperature rising rate of 5 to 10 ℃ per minute, heating the composite green body to 1550 to 1650 ℃ at a temperature rising rate of 2 to 5 ℃ per minute, maintaining the temperature for 1 to 2 hours, cooling the composite green body to 800 to 1200 ℃ at a cooling rate of 2 to 5 ℃ per minute, and finally cooling the composite green body to room temperature with a furnace.
12. The composite ceramic substrate is characterized by having a laminated structure, and comprises a first material layer, a second material layer and a third material layer, wherein the first material layer is an aluminum oxide layer, the second material layer is a mixed layer of aluminum oxide and yttrium-stabilized zirconium oxide, and the third material layer is a mixed layer of aluminum oxide and lanthanum oxide, and the first material layer is arranged between the second material layer and the third material layer so as to separate the second material layer from the third material layer.
13. The composite ceramic substrate according to claim 12, wherein the surface layer of the composite ceramic substrate is a first material layer.
14. The composite ceramic substrate of claim 12, wherein the composite ceramic substrate comprises an overcoat layer and a core disposed between the overcoat layers, the overcoat layer comprising a first material layer and a second material layer disposed between the first material layers, the core comprising a third material layer, or
The composite ceramic substrate includes an outer cladding layer including a first material layer and a third material layer disposed between the first material layers, and a core disposed between the outer cladding layers, the core including a second material layer.
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