CN110950675A - Novel connection method of AlN ceramic and Cu - Google Patents

Novel connection method of AlN ceramic and Cu Download PDF

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CN110950675A
CN110950675A CN201911104090.8A CN201911104090A CN110950675A CN 110950675 A CN110950675 A CN 110950675A CN 201911104090 A CN201911104090 A CN 201911104090A CN 110950675 A CN110950675 A CN 110950675A
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cuo
aln ceramic
aln
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seed layer
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傅仁利
黄义炼
吴彬勇
吕金玲
何钦江
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B37/00Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/023Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
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    • C04B2237/00Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/12Metallic interlayers
    • C04B2237/125Metallic interlayers based on noble metals, e.g. silver
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32Ceramic
    • C04B2237/36Non-oxidic
    • C04B2237/366Aluminium nitride
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    • C04B2237/00Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40Metallic
    • C04B2237/407Copper
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/55Pre-treatments of a coated or not coated substrate other than oxidation treatment in order to form an active joining layer

Abstract

The invention discloses a novel connection method of AlN ceramic and Cu, which comprises the steps of screen printing a layer of CuO slurry on the surface of AlN ceramic, sintering to form a CuO layer, preserving heat in a reducing atmosphere for a long time, reducing CuO into Cu to prepare a seed layer, using Ag as an intermediate layer, and welding AlN and Cu with the seed layer in a vacuum furnace to realize novel connection of AlN ceramic and Cu. The invention belongs to the field of microelectronic packaging, adopts low-cost CuO and Ag, reduces the welding temperature, utilizes the reaction of the CuO and AlN to generate a reliable connecting layer, uses a solid solution and an eutectic structure formed between the Ag and the Cu, does not generate any hard and brittle compound in a welding seam structure, improves the connecting strength of a joint, and effectively solves the defects of easy generation of holes and the like in the glue discharging process by adopting a multi-step process; the processing conditions are simple, the requirements on processing environment, equipment and the like are low, and the method is favorable for batch production.

Description

Novel connection method of AlN ceramic and Cu
Technical Field
The invention belongs to the field of microelectronic packaging, and particularly relates to a novel connection method of AlN ceramic and Cu.
Background
In the age of rapid development of electronic information technology, ceramic and metal composite materials, i.e., ceramic and metal composite materialsThe ceramic has the advantages of high strength, good insulativity, excellent heat conduction and heat resistance, small thermal expansion coefficient, good chemical stability and the like, and can realize electrical interconnection due to the fact that the metal material is coated on the ceramic, so that the ceramic is widely applied to substrate materials for packaging high-power devices. The physical and chemical properties of ceramics and metals are very different, so that the interconnection of the two has a great problem. The common methods currently applied to interconnection of ceramics and metals include a direct metal coating method, an active metal brazing method, a thick film metallization method, an electroless metallization method and a thin film metallization method, wherein Al is subjected to the interconnection method2O3,AlN,Si3N4The ceramic and the metal Cu, Ag, Al and the like are connected, but the composite material prepared by the method cannot simultaneously meet the requirements of the material in the aspects of process, cost, strength and reliability.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a novel connection method of AlN ceramic and Cu, which adopts the following technical scheme: and printing a layer of CuO slurry on the surface of the AlN ceramic by screen printing, sintering to form a CuO layer, preserving heat in a reducing atmosphere for a long time, reducing the CuO into Cu to prepare a seed layer, using Ag as an intermediate layer, and welding the AlN with the seed layer and the Cu in a vacuum furnace.
Further, the CuO slurry is composed of 86% by mass of CuO and 14% by mass of an organic carrier.
Furthermore, the CuO is nano CuO powder, and the shape of the CuO powder is nearly spherical.
Further, the organic carrier is an organic mixture of a terpineol-ethyl cellulose system, and the organic carrier comprises a solvent, a thickening agent, a thixotropic agent and a surfactant, wherein the solvent is terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, the thickening agent is ethyl cellulose, the thixotropic agent is castor oil, and the surfactant is one of polyethylene glycol and triethanolamine.
Further, the organic carrier is an organic mixture of a terpineol-ethyl cellulose system, and comprises the following components in parts by weight: 62 parts of terpineol, 5 parts of dibutyl phthalate, 22 parts of diethylene glycol butyl ether acetate, 4 parts of castor oil, 2 parts of triethanolamine and 5 parts of ethyl cellulose.
Further, the reducing atmosphere is H accounting for 20 percent of the volume2And 80% of N2The mixed gas of (1).
Further, the intermediate layer was flake Ag having a purity of 99.99% and a thickness of 20 μm.
The novel connection method of the AlN ceramic and the Cu specifically comprises the following steps:
1) preparation of organic vehicle
Adding ethyl cellulose into a mixed solvent of terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, heating to 90 ℃ for water bath stirring, adding castor oil and triethanolamine after the ethyl cellulose is completely dissolved, and continuously heating and stirring for 1-2 hours to prepare a uniform organic carrier;
2) preparation of CuO slurry
Firstly, 86 mass percent of CuO powder and 14 mass percent of organic carrier are weighed by a beaker and put into a constant-temperature magnetic stirring water bath kettle, and the mixture is stirred for 2 hours at constant temperature in the environment of 30 ℃ so that the CuO powder is fully dispersed into the organic carrier;
3) CuO paste for screen printing
Cleaning a silk screen, adjusting the height of a screen plate from a printing table, opening a mechanical pump, moving a scraper at an angle of 45 degrees, printing CuO slurry on an AlN ceramic plate, firstly placing the AlN ceramic plate in air, leveling for 10min, then placing the AlN ceramic plate in a drying box at 60 ℃, and drying for 30 min;
4) sintered CuO layer
Putting the AlN ceramic plate brushed with the CuO slurry into a muffle furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, discharging the organic carrier, heating to 1075 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, and enabling the CuO slurry and the AlN ceramic plate to fully react to generate the CuAlO compound composite substrate;
5) reducing the CuO layer to form a seed layer
Placing the sintered CuAlO compound composite substrate into a box-type atmosphere furnace, preserving the heat at 400 ℃ for 2h, then cooling the furnace, and reducing all CuO layers on the CuAlO compound composite substrate into Cu to obtain a required seed layer, wherein the thickness of the seed layer is about 50 mu m;
6) interconnecting AlN with seed layer and Cu
Stacking a single layer of Ag sheet and a Cu plate on the seed layer, putting the seed layer into a vacuum tube furnace, and vacuumizing to 3 x 10-3pa, heating to 810-850 ℃, preserving heat for 10-30 min, and then cooling in a furnace, wherein the highest connection strength of AlN and Cu can reach 44 Mpa.
The beneficial effects obtained by adopting the scheme are as follows: according to the invention, CuO and Ag with lower cost are adopted, the welding temperature is reduced, a reliable connecting layer is generated by utilizing the reaction of the CuO and AlN, a solid solution and an eutectic structure formed between the Ag and the Cu are used, no hard and brittle compound is generated in a welding seam structure, the connecting strength of a joint is improved, and meanwhile, the defects that holes are easy to generate in the glue discharging process and the like are effectively overcome by adopting a multi-step process mode; the processing conditions are simple, the requirements on processing environment, equipment and the like are low, and the method is favorable for batch production.
Drawings
FIG. 1 is a micro-topography of a seed layer in example 1 of a novel AlN ceramic and Cu connecting method according to the present invention;
FIG. 2 is a micro-topography of a seed layer according to an embodiment 3 of the novel connection method of AlN ceramic and Cu;
FIG. 3 is a view showing the interface connection morphology of example 1 of the novel AlN ceramic and Cu connecting method of the present invention;
FIG. 4 is a view showing the interface connection morphology of the novel AlN ceramic and Cu connecting method of example 2 according to the present invention;
FIG. 5 is a schematic view of the interface connection of example 3 of the novel AlN ceramic and Cu connecting method of the present invention;
FIG. 6 is a graphical representation of the interface connection morphology of the novel connection method of AlN ceramic and Cu of example 4 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1:
1) preparation of organic vehicle
Adding ethyl cellulose into a mixed solvent of terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, heating to 90 ℃ for water bath stirring, adding castor oil and triethanolamine after the ethyl cellulose is completely dissolved, and continuously heating and stirring for 1-2 hours to prepare a uniform organic carrier, wherein the organic carrier comprises the following components in parts by weight: 62 parts of terpineol, 5 parts of dibutyl phthalate, 22 parts of diethylene glycol butyl ether acetate, 4 parts of castor oil, 2 parts of triethanolamine and 5 parts of ethyl cellulose;
2) preparation of CuO slurry
Firstly, 86 mass percent of CuO powder and 14 mass percent of organic carrier are weighed by a beaker and put into a constant-temperature magnetic stirring water bath kettle, and the mixture is stirred for 2 hours at constant temperature in the environment of 30 ℃ so that the CuO powder is fully dispersed into the organic carrier;
3) CuO paste for screen printing
Cleaning a silk screen, adjusting the height of the screen plate from a printing table, opening a mechanical pump, moving a scraper at an angle of 45 degrees, printing CuO slurry on an AlN ceramic plate, firstly placing the AlN ceramic plate in air for leveling for 10min, then placing the AlN ceramic plate in a drying box at 60 ℃, drying for 30min, and repeating the step twice;
4) sintered CuO layer
Putting the AlN ceramic plate brushed with the CuO slurry into a muffle furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, discharging the organic carrier, heating to 1075 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, and enabling the CuO slurry and the AlN ceramic plate to fully react to generate the CuAlO compound composite substrate;
5) reducing the CuO layer to form a seed layer
Placing the sintered CuAlO compound composite substrate into a box-type atmosphere furnace, preserving the heat at 400 ℃ for 2h, then cooling the furnace, and reducing the CuO layer on the CuAlO compound composite substrate into Cu to prepare a seed layer with the thickness of about 50 mu m;
6) interconnecting AlN with seed layer and Cu
Stacking a single layer of Ag sheet and a Cu plate on the seed layer, putting the seed layer into a vacuum tube furnace, and vacuumizing to 3 x 10-3pa, heating to 830 ℃, preserving heat for 10min, and then cooling in a furnace;
7) and (3) performance testing: and measuring the shearing strength of the prepared AlN ceramic and Cu composite substrate by using a shearing machine, and observing the microscopic appearance and measuring the thickness of the interface connecting layer after embedding the sample.
Example 2:
1) preparation of organic vehicle
Adding ethyl cellulose into a mixed solvent of terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, heating to 90 ℃ for water bath stirring, adding castor oil and triethanolamine after the ethyl cellulose is completely dissolved, and continuously heating and stirring for 1-2 hours to prepare a uniform organic carrier, wherein the organic carrier comprises the following components in parts by weight: 62 parts of terpineol, 5 parts of dibutyl phthalate, 22 parts of diethylene glycol butyl ether acetate, 4 parts of castor oil, 2 parts of triethanolamine and 5 parts of ethyl cellulose;
2) preparation of CuO slurry
Firstly, 86 mass percent of CuO powder and 14 mass percent of organic carrier are weighed by a beaker and put into a constant-temperature magnetic stirring water bath kettle, and the mixture is stirred for 2 hours at constant temperature in the environment of 30 ℃ so that the CuO powder is fully dispersed into the organic carrier;
3) CuO paste for screen printing
Cleaning a silk screen, adjusting the height of the screen plate from a printing table, opening a mechanical pump, moving a scraper at an angle of 45 degrees, printing CuO slurry on an AlN ceramic plate, firstly placing the AlN ceramic plate in air for leveling for 10min, then placing the AlN ceramic plate in a drying box at 60 ℃, drying for 30min, and repeating the step twice;
4) sintered CuO layer
Putting the AlN ceramic plate brushed with the CuO slurry into a muffle furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, discharging the organic carrier, heating to 1075 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, and enabling the CuO slurry and the AlN ceramic plate to fully react to generate the CuAlO compound composite substrate;
5) reducing the CuO layer to form a seed layer
Placing the sintered CuAlO compound composite substrate into a box-type atmosphere furnace, preserving the heat at 400 ℃ for 2h, then cooling the furnace, and reducing the CuO layer on the CuAlO compound composite substrate into Cu to prepare a seed layer with the thickness of about 50 mu m;
6) interconnecting AlN with seed layer and Cu
Stacking a single layer of Ag sheet and a Cu plate on the seed layer, putting the seed layer into a vacuum tube furnace, and vacuumizing to 3 x 10-3pa, heating to 840 ℃, preserving heat for 10min, and then furnace cooling;
7) and (3) testing the performance, namely measuring the shearing strength of the prepared AlN ceramic and Cu composite substrate by using a shearing machine, and observing the microscopic appearance and measuring the thickness of the interface connecting layer after embedding the sample.
Example 3:
1) preparation of organic vehicle
Adding ethyl cellulose into a mixed solvent of terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, heating to 90 ℃ for water bath stirring, adding castor oil and triethanolamine after the ethyl cellulose is completely dissolved, and continuously heating and stirring for 1-2 hours to prepare a uniform organic carrier, wherein the organic carrier comprises the following components in parts by weight: 62 parts of terpineol, 5 parts of dibutyl phthalate, 22 parts of diethylene glycol butyl ether acetate, 4 parts of castor oil, 2 parts of triethanolamine and 5 parts of ethyl cellulose;
2) preparation of CuO slurry
Firstly, 86 mass percent of CuO powder and 14 mass percent of organic carrier are weighed by a beaker and put into a constant-temperature magnetic stirring water bath kettle, and the mixture is stirred for 2 hours at constant temperature in the environment of 30 ℃ so that the CuO powder is fully dispersed into the organic carrier;
3) CuO paste for screen printing
Cleaning a silk screen, adjusting the height of the screen plate from a printing table, opening a mechanical pump, moving a scraper at an angle of 45 degrees, printing CuO slurry on an AlN ceramic plate, firstly placing the AlN ceramic plate in air for leveling for 10min, then placing the AlN ceramic plate in a drying box at 60 ℃, drying for 30min, and repeating the step for three times;
4) sintered CuO layer
Putting the AlN ceramic plate brushed with the CuO slurry into a muffle furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, discharging the organic carrier, heating to 1075 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, and enabling the CuO slurry and the AlN ceramic plate to fully react to generate the CuAlO compound composite substrate;
5) reducing the CuO layer to form a seed layer
Placing the sintered CuAlO compound composite substrate into a box-type atmosphere furnace, preserving the heat at 400 ℃ for 2h, then cooling the furnace, and reducing the CuO layer on the CuAlO compound composite substrate into Cu to prepare a seed layer with the thickness of about 80 mu m;
6) interconnecting AlN with seed layer and Cu
Stacking a single layer of Ag sheet and a Cu plate on the seed layer, putting the seed layer into a vacuum tube furnace, and vacuumizing to 3 x 10-3pa, heating to 830 ℃, preserving heat for 10min, and then cooling in a furnace;
7) and (3) testing the performance, namely measuring the shearing strength of the prepared AlN ceramic and Cu composite substrate by using a shearing machine, and observing the microscopic appearance and measuring the thickness of the interface connecting layer after embedding the sample.
Example 4:
1) preparation of organic vehicle
Adding ethyl cellulose into a mixed solvent of terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, heating to 90 ℃ for water bath stirring, adding castor oil and triethanolamine after the ethyl cellulose is completely dissolved, and continuously heating and stirring for 1-2 hours to prepare a uniform organic carrier, wherein the organic carrier comprises the following components in parts by weight: 62 parts of terpineol, 5 parts of dibutyl phthalate, 22 parts of diethylene glycol butyl ether acetate, 4 parts of castor oil, 2 parts of triethanolamine and 5 parts of ethyl cellulose;
2) preparation of CuO slurry
Firstly, 86 mass percent of CuO powder and 14 mass percent of organic carrier are weighed by a beaker and put into a constant-temperature magnetic stirring water bath kettle, and the mixture is stirred for 2 hours at constant temperature in the environment of 30 ℃ so that the CuO powder is fully dispersed into the organic carrier;
3) CuO paste for screen printing
Cleaning a silk screen, adjusting the height of the screen plate from a printing table, opening a mechanical pump, moving a scraper at an angle of 45 degrees, printing CuO slurry on an AlN ceramic plate, firstly placing the AlN ceramic plate in air for leveling for 10min, then placing the AlN ceramic plate in a drying box at 60 ℃, drying for 30min, and repeating the step for three times;
4) sintered CuO layer
Putting the AlN ceramic plate brushed with the CuO slurry into a muffle furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, discharging the organic carrier, heating to 1075 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, and enabling the CuO slurry and the AlN ceramic plate to fully react to generate the CuAlO compound composite substrate;
5) reducing the CuO layer to form a seed layer
Placing the sintered CuAlO compound composite substrate into a box-type atmosphere furnace, preserving the heat at 400 ℃ for 2h, cooling the furnace, and reducing the CuO layer into Cu to prepare a seed layer with the thickness of about 80 mu m;
6) interconnecting AlN with seed layer and Cu
Stacking a single layer of Ag sheet and a Cu plate on the seed layer, putting the seed layer into a vacuum tube furnace, and vacuumizing to 3 x 10-3pa, heating to 840 ℃, preserving heat for 10min, and then furnace cooling;
7) and (3) performance testing: and measuring the shearing strength of the prepared AlN ceramic and Cu composite substrate by using a shearing machine, and observing the microscopic appearance and measuring the thickness of the interface connecting layer after embedding the sample.
The performance test results are shown in table 1:
TABLE 1
Example 1 Example 2 Example 3 Example 4
Shear strength (Mpa) 21.0 20.5 30.4 34.8
Thickness of interface connecting layer (mum) 38.46 40.47 71.22 75.92
As can be seen from Table 1, the change of the processing temperature when AlN and Cu are interconnected has no significant influence on the shear strength performance of the AlN ceramic and Cu composite substrate; with the increase of the repetition times of silk-screen printing of the CuO slurry, the shearing strength of the obtained AlN ceramic and Cu composite substrate is remarkably increased, and the thickness of an interface connecting layer is remarkably increased.
Fig. 1 and 2 are microstructure diagrams of the seed layers of examples 1 and 3, respectively, and it can be seen from fig. 1-2 that the loose and porous seed layer prepared after reduction is favorable for diffusion of Ag atoms in the subsequent connection process, and the thickness of the seed layer is significantly increased along with the number of screen printing.
Fig. 3 to 6 are respectively a morphology diagram of interface connection in examples 1 to 4, and it can be seen from fig. 3 to 6 that, after reaching a certain temperature, Ag and Cu diffuse each other to form an alloy liquid phase with a low melting point to fill in the pores, and a dense connection layer with bulk Cu as a framework and an Ag-Cu eutectic structure as a filling is formed in the cooling process. Along with the increase of the screen printing times, the thickness of the interface connection layer is remarkably increased, and simultaneously, the bulk copper in the interface connection layer is remarkably increased, so that a net structure taking Cu as a framework is favorably formed, the residual stress can be alleviated to a certain extent, and the joint strength is improved. The increase of the processing temperature when AlN and Cu are interconnected has little influence on the appearance and the structure of the interface.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (8)

1. A novel connection method of AlN ceramic and Cu is characterized in that a CuO slurry is screen-printed on the surface of AlN ceramic, a CuO layer is prepared by sintering and film forming, the temperature is kept for a long time in a reducing atmosphere, CuO is reduced to Cu to prepare a seed layer, Ag is used as an intermediate layer, and AlN and Cu with the seed layer are welded in a vacuum furnace.
2. The novel connection method of AlN ceramic and Cu according to claim 1, wherein said CuO slurry is composed of 86% CuO by mass and 14% organic vehicle by mass.
3. The novel connection method of AlN ceramic and Cu according to claim 1, wherein the CuO is nano CuO powder, and the CuO powder has a nearly spherical shape.
4. The novel connection method of AlN ceramic and Cu according to claim 1, wherein the organic carrier is an organic mixture of terpineol-ethyl cellulose system, and the components of the organic mixture comprise a solvent, a thickening agent, a thixotropic agent and a surfactant, the solvent is terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, the thickening agent is ethyl cellulose, the thixotropic agent is castor oil, and the surfactant is one of polyethylene glycol and triethanolamine.
5. The novel connection method of AlN ceramic and Cu as claimed in claim 1, wherein said organic vehicle is an organic mixture of terpineol-ethyl cellulose system comprising the following components in parts by weight: 62 parts of terpineol, 5 parts of dibutyl phthalate, 22 parts of diethylene glycol butyl ether acetate, 4 parts of castor oil, 2 parts of triethanolamine and 5 parts of ethyl cellulose.
6. The method of claim 1, wherein the reducing atmosphere is 20 vol.% H2And 80% of N2The mixed gas of (1).
7. The novel connection method of AlN ceramic and Cu according to claim 1, wherein said intermediate layer is Ag flakes having a purity of 99.99% and a thickness of 20 μm.
8. The novel connection method of AlN ceramic and Cu according to claim 1, characterized by comprising the following steps:
1) preparation of organic vehicle
Adding ethyl cellulose into a mixed solvent of terpineol, diethylene glycol butyl ether acetate and dibutyl phthalate, heating to 90 ℃ for water bath stirring, adding castor oil and triethanolamine after the ethyl cellulose is completely dissolved, and continuously heating and stirring for 1-2 hours to prepare a uniform organic carrier;
2) preparation of CuO slurry
Firstly, 86 mass percent of CuO powder and 14 mass percent of organic carrier are weighed by a beaker and put into a constant-temperature magnetic stirring water bath kettle, and the mixture is stirred for 2 hours at constant temperature in the environment of 30 ℃ so that the CuO powder is fully dispersed into the organic carrier;
3) CuO paste for screen printing
Cleaning a silk screen, adjusting the height of a screen plate from a printing table, opening a mechanical pump, moving a scraper at an angle of 45 degrees, printing CuO slurry on an AlN ceramic plate, firstly placing the AlN ceramic plate in air, leveling for 10min, then placing the AlN ceramic plate in a drying box at 60 ℃, and drying for 30 min;
4) sintered CuO layer
Putting the AlN ceramic plate brushed with the CuO slurry into a muffle furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, discharging the organic carrier, heating to 1075 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, and enabling the CuO slurry and the AlN ceramic plate to fully react to generate the CuAlO compound composite substrate;
5) reducing the CuO layer to form a seed layer
Placing the sintered CuAlO compound composite substrate into a box-type atmosphere furnace, preserving the heat at 400 ℃ for 2h, then cooling the furnace, and reducing all CuO layers on the CuAlO compound composite substrate into Cu to prepare a required seed layer;
6) interconnecting AlN with seed layer and Cu
Stacking a single layer of Ag sheet and a Cu plate on the seed layer, putting the seed layer into a vacuum tube furnace, and vacuumizing to 3 x 10-3pa, heating to 810-850 ℃, preserving heat for 10-30 min, and then cooling in a furnace, wherein the highest connection strength of AlN and Cu can reach 44 Mpa.
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CN114163259A (en) * 2021-12-14 2022-03-11 东莞智昊光电科技有限公司 Method for metallizing ceramic surfaces and metallized ceramics

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