CN107556060B - Method for metalizing aluminum nitride ceramic plate - Google Patents
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- CN107556060B CN107556060B CN201710784345.4A CN201710784345A CN107556060B CN 107556060 B CN107556060 B CN 107556060B CN 201710784345 A CN201710784345 A CN 201710784345A CN 107556060 B CN107556060 B CN 107556060B
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Abstract
The invention relates to a method for metalizing an aluminum nitride ceramic plate, which comprises the following steps: cleaning the surface of the aluminum nitride ceramic plate, and forming a titanium conducting layer with a set thickness on the surface of the aluminum nitride ceramic plate; taking an aluminum nitride ceramic plate with a titanium-plated surface as a cathode, placing the aluminum nitride ceramic plate in an electrolytic bath, and taking refined copper as an anode; placing the aluminum nitride ceramic plate in a heat treatment furnace, heating, and enabling the titanium conductive layer to penetrate into aluminum nitride to form a TiN metallurgical transition layer and simple substance aluminum; continuing heating and raising the temperature, and sending ultrasonic waves to the aluminum nitride ceramic plate through an ultrasonic wave generating device to enable liquid simple substance aluminum to vibrate and flow out, so as to stabilize the TiN metallurgy transition layer; further heating and raising the temperature, and enabling the titanium conductive layer to permeate into the copper coating to form a TiCu metallurgical transition layer. Compared with the prior art, the method can lead the liquid-state simple substance aluminum in the TiN metallurgy transition layer to vibrate, lead the liquid-state simple substance aluminum to be fused and discharged out of the aluminum nitride ceramic plate, improve the connection strength of the copper coating and the titanium conducting layer, and improve the product quality and the yield.
Description
Technical Field
The invention relates to the field of ceramic metallization, and relates to a method for metallizing an aluminum nitride ceramic plate.
Background
In the development of power electronic devices, a novel aluminum nitride ceramic (AlN) has gradually replaced the conventional packaging materials of aluminum oxide and beryllium oxide ceramic due to its good thermal conductivity (thermal conductivity can reach 150-.
However, aluminum nitride ceramics are difficult to directly connect with electronic chips, and the surfaces of the aluminum nitride ceramics need to be metalized, and the metallization is generally performed by coating copper on the surfaces. The aluminum nitride ceramic coated with copper has good thermal conductivity of the aluminum nitride ceramic and good electrical conductivity of the metal copper. However, because the difference between the expansion coefficients of aluminum nitride and copper is large, i.e., the difference between the wetting angles is too large, the combination of aluminum nitride and copper is difficult, and therefore, it is very important to select a proper metallization method for aluminum nitride ceramic plates.
At present, a plurality of technical reports about the metallization of aluminum nitride ceramic plates at home and abroad are reported, and the basic principle is improved on the basis of a direct copper-coating method. In the prior art, the surface metallization is realized by combining titanium and copper, for example, the metallization method of the aluminum nitride ceramic plate of the invention patent application No. 201410031911.0, a middle titanium conducting layer of an aluminum nitride and copper coating is mentioned, a TiN metallurgical transition layer (AlN + Ti → TiN + Al) can be formed between the aluminum nitride ceramic plate and the titanium conducting layer, and a TiCu metallurgical transition layer (Cu + Ti → TiCu) can also be formed between the aluminum nitride ceramic plate and the metal copper, and the bonding force between the aluminum nitride and the copper is enhanced by the existence of the two metallurgical transition layers; meanwhile, the aluminum nitride ceramic plate has conductivity after being coated with titanium, so that a copper coating can be directly obtained on the surface of the titanium coated with the aluminum nitride by a chemical plating method to replace a copper foil in a direct copper coating method; however, an aluminum simple substance is generated in the process of forming the TiN metallurgy transition layer (AlN + Ti → TiN + Al), the temperature needs to be increased to 800-900 ℃ in the process of forming the TiCu metallurgy transition layer, Al is heated to be in a liquid state and cannot be removed, the production quality is influenced, and the yield is low.
Disclosure of Invention
The invention aims to provide a method for metalizing an aluminum nitride ceramic plate, which aims to solve the technical problems that: in the process of forming the TiCu metallurgical transition layer, the temperature needs to be heated to 800-900 ℃, Al is heated to be in a liquid state and cannot be removed, the production quality is affected, and the yield is low.
The technical scheme for solving the technical problems is as follows: the method for metalizing the aluminum nitride ceramic plate comprises the following steps of:
step S1: cleaning the surface of the aluminum nitride ceramic plate, and plating a titanium conducting layer with a set thickness on the surface of the aluminum nitride ceramic plate through vacuum magnetron sputtering;
step S2: taking an aluminum nitride ceramic plate with a titanium-plated surface as a cathode, placing the aluminum nitride ceramic plate in an electrolytic tank containing an acidic copper sulfate plating solution, taking refined copper as an anode, and controlling the current density of the cathode and the electroplating time to obtain a copper plating layer with a corresponding thickness;
step S3: placing the aluminum nitride ceramic plate with the surface coated with the titanium conducting layer and the copper coating in sequence in a heat treatment furnace, filling argon into the heat treatment furnace, heating, keeping the temperature for 25-30 min when the temperature reaches 300-400 ℃, and allowing the titanium conducting layer to penetrate into aluminum nitride to form a TiN metallurgy transition layer and simple substance aluminum;
step S4: continuing heating and raising the temperature, keeping the temperature for 10-15 min when the temperature reaches 600-700 ℃, simultaneously sending ultrasonic waves to the aluminum nitride ceramic plate through an ultrasonic wave generating device, and continuing for 10-15 min to enable liquid simple substance aluminum to vibrate and flow out, so that a TiN metallurgy transition layer is stabilized;
step S5: and further heating to 800-900 ℃, preserving the heat for 30-60 min, and enabling the titanium conductive layer to permeate into the copper coating to form a TiCu metallurgical transition layer.
The invention has the beneficial effects that: the refined copper is used as the anode, so that other metals can be effectively prevented from being electroplated on the aluminum nitride ceramic plate, and the product quality is improved; send the ultrasonic wave to the aluminium nitride ceramic plate through ultrasonic wave generating device, enable the titanium conducting layer to form the liquid simple substance aluminium vibration that produces in the metallurgical transition layer in-process of TiN to aluminium nitride infiltration for liquid simple substance aluminium fuses and discharges outside aluminium nitride ceramic plate, promotes the joint strength of copper cladding material and titanium conducting layer, promotes product quality and yield.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in step S1, the surface of the aluminum nitride ceramic plate is cleaned with 10% hydrochloric acid, then cleaned with clean water, and dried after cleaning.
The beneficial effect of adopting the further scheme is that: the aluminum nitride ceramic plate is cleaned by 10% hydrochloric acid, so that the cleaning cleanliness of the aluminum nitride ceramic plate is improved, and other metals are prevented from being attached to the aluminum nitride ceramic plate to influence the surface metallization quality of the aluminum nitride ceramic plate; furthermore, the hydrochloric acid is easy to volatilize, and the subsequent electroplating is not influenced.
Further, in the step 2, the aluminum nitride ceramic plate with the titanium conducting layer plated on the surface is placed in an acid copper sulfate plating solution for copper electroplating, and the formula of the acid copper sulfate plating solution is as follows: 150-220 g/L CuSO4·5H2O, 50-80 g/L of concentrated H with mass concentration of 98%2SO4The solvent is water.
The beneficial effect of adopting the further scheme is that: the process is mature, the control condition is simple, the equipment is ready, the precision and the efficiency of the copper electroplating of the aluminum nitride ceramic plate can be improved, and the yield is improved.
Further, in the step 2, the electrolytic copper plating takes the refined copper as an anode, and the cathode current density is controlled to be 3-8A/dm2And the temperature is 30-50 ℃, and the time is 10-30 min, so that a copper coating with the thickness of 5-100 microns is formed on the surface of the aluminum nitride ceramic plate with the titanium conducting layer coated on the surface.
The beneficial effect of adopting the further scheme is that: the process is mature, the control condition is simple, the equipment is ready, the precision and the efficiency of the copper electroplating of the aluminum nitride ceramic plate can be improved, and the yield is improved.
Further, in the step S4, the frequency of the ultrasonic wave generated by the ultrasonic wave generator to the aluminum nitride ceramic plate is 1 mhz to 30 mhz.
The beneficial effect of adopting the further scheme is that: the frequency of ultrasonic wave is 1 megahertz ~ 30 megahertz, can make the liquid simple substance aluminium vibration on the aluminium nitride ceramic plate, and then fuses the aluminium nitride ceramic plate that flows, promotes the joint strength of copper coating and titanium conducting layer, promotes product quality and yield.
Further, argon gas is filled into the heat treatment furnace, so that the air pressure in the heat treatment furnace reaches 3 standard atmospheric pressure to 4 standard atmospheric pressure.
The beneficial effect of adopting the further scheme is that: 3 standard atmospheric pressure to 4 standard atmospheric pressure's argon gas can effectively realize extrudeing aluminium nitride ceramic plate for liquid simple substance aluminium flows out, promotes production efficiency.
Drawings
FIG. 1 is a flow chart of the method for metallizing an aluminum nitride ceramic plate according to the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1:
as shown in fig. 1, the method for metallizing an aluminum nitride ceramic plate comprises the following steps:
step S1: cleaning the surface of the aluminum nitride ceramic plate, cleaning the surface of the aluminum nitride ceramic plate by 10% hydrochloric acid, cleaning by clean water, and drying after cleaning; forming a titanium conducting layer with a set thickness on the surface of the aluminum nitride ceramic plate through vacuum magnetron sputtering plating;
step S2: the aluminum nitride ceramic plate with the titanium plated surface is used as a cathode and is placed in an electrolytic bath containing acidic copper sulfate plating solution, refined copper is used as an anode, and the acidic copper sulfate plating solution comprises the following components in percentage by weight: 150g/L CuSO4·5H2O, 50g/L concentrated H with mass concentration of 98%2SO4The solvent is water; controlling cathode current density to be 3A/dm2Forming a copper plating layer with the thickness of 5 microns on the surface of the aluminum nitride ceramic plate with the titanium conducting layer plated on the surface at the temperature of 30 ℃ for 30 min;
step S3: placing the aluminum nitride ceramic plate with the surface coated with the titanium conductive layer and the copper coating in sequence in a heat treatment furnace, filling argon into the heat treatment furnace, heating, keeping the temperature for 25min when the temperature reaches 300 ℃, and allowing the titanium conductive layer to penetrate into aluminum nitride to form a TiN metallurgical transition layer and simple substance aluminum;
step S4: continuing heating and warming, keeping the temperature for 15min when the temperature reaches 600 ℃, simultaneously sending ultrasonic waves to the aluminum nitride ceramic plate through an ultrasonic wave generating device, enabling the frequency of the ultrasonic waves sent by the ultrasonic wave generating device to be 1 MHz, enabling the ultrasonic wave generating device to rotate around the heat treatment furnace, realizing that the ultrasonic waves are sent to the aluminum nitride ceramic plate in the heat treatment furnace at 360 degrees, enabling liquid elemental aluminum on the aluminum nitride ceramic plate to vibrate and last for 15min, filling argon into the heat treatment furnace, enabling the air pressure in the heat treatment furnace to reach 4 standard atmospheric pressures, enabling the liquid elemental aluminum to vibrate and flow out, and stabilizing a TiN metallurgy transition layer;
step S5: further heating to 800 ℃, and preserving heat for 60min, wherein the titanium conductive layer permeates into the copper coating to form a TiCu metallurgy transition layer.
The refined copper is used as the anode, so that other metals can be effectively prevented from being electroplated on the aluminum nitride ceramic plate, and the product quality is improved; ultrasonic waves are sent to the aluminum nitride ceramic plate through an ultrasonic wave generating device, so that liquid simple substance aluminum generated in the process that the titanium conductive layer penetrates into the aluminum nitride to form a TiN metallurgical transition layer can vibrate, and the liquid simple substance aluminum is fused and discharged out of the aluminum nitride ceramic plate; 3 standard atmospheric pressure to 4 standard atmospheric pressure's argon gas can effectively realize extrudeing aluminium nitride ceramic plate for liquid simple substance aluminium flows out, promotes production efficiency.
Example 2:
as shown in fig. 1, the method for metallizing an aluminum nitride ceramic plate comprises the following steps:
step S1: cleaning the surface of the aluminum nitride ceramic plate, cleaning the surface of the aluminum nitride ceramic plate by 10% hydrochloric acid, cleaning by clean water, and drying after cleaning; forming a titanium conducting layer with a set thickness on the surface of the aluminum nitride ceramic plate through vacuum magnetron sputtering plating;
step S2: the aluminum nitride ceramic plate with the titanium plated surface is used as a cathode and is placed in an electrolytic bath containing acidic copper sulfate plating solution, refined copper is used as an anode, and the acidic copper sulfate plating solution comprises the following components in percentage by weight: 180g/L CuSO4·5H2O, and concentrated H with the mass concentration of 65g/L of 98 percent2SO4The solvent is water; controlling cathode current density to be 5A/dm2Forming a copper plating layer with the thickness of 55 microns on the surface of the aluminum nitride ceramic plate with the titanium conducting layer plated on the surface at the temperature of 40 ℃ for 20 min;
step S3: placing the aluminum nitride ceramic plate with the surface coated with the titanium conductive layer and the copper coating in sequence in a heat treatment furnace, filling argon into the heat treatment furnace, heating, keeping the temperature for 28min when the temperature reaches 350 ℃, and allowing the titanium conductive layer to penetrate into aluminum nitride to form a TiN metallurgical transition layer and simple substance aluminum;
step S4: continuing heating and warming, keeping the temperature for 13min when the temperature reaches 650 ℃, simultaneously sending ultrasonic waves to the aluminum nitride ceramic plate through an ultrasonic wave generating device, enabling the frequency of the ultrasonic waves sent by the ultrasonic wave generating device to be 15 MHz, enabling the ultrasonic wave generating device to rotate around the heat treatment furnace, realizing that the ultrasonic waves are sent to the aluminum nitride ceramic plate in the heat treatment furnace at 360 degrees, enabling liquid elemental aluminum on the aluminum nitride ceramic plate to vibrate and last for 10min, filling argon into the heat treatment furnace, enabling the air pressure in the heat treatment furnace to reach 3.5 standard atmospheric pressures, enabling the liquid elemental aluminum to vibrate and flow out, and stabilizing a TiN metallurgy transition layer;
step S5: further heating to 850 ℃, keeping the temperature for 45min, and enabling the titanium conductive layer to permeate into the copper plating layer to form a TiCu metallurgical transition layer.
The refined copper is used as the anode, so that other metals can be effectively prevented from being electroplated on the aluminum nitride ceramic plate, and the product quality is improved; ultrasonic waves are sent to the aluminum nitride ceramic plate through an ultrasonic wave generating device, so that liquid simple substance aluminum generated in the process that the titanium conductive layer penetrates into the aluminum nitride to form a TiN metallurgical transition layer can vibrate, and the liquid simple substance aluminum is fused and discharged out of the aluminum nitride ceramic plate; 3 standard atmospheric pressure to 4 standard atmospheric pressure's argon gas can effectively realize extrudeing aluminium nitride ceramic plate for liquid simple substance aluminium flows out, promotes production efficiency.
Example 3:
as shown in fig. 1, the method for metallizing an aluminum nitride ceramic plate comprises the following steps:
step S1: cleaning the surface of the aluminum nitride ceramic plate, cleaning the surface of the aluminum nitride ceramic plate by 10% hydrochloric acid, cleaning by clean water, and drying after cleaning; forming a titanium conducting layer with a set thickness on the surface of the aluminum nitride ceramic plate through vacuum magnetron sputtering plating;
step S2: the aluminum nitride ceramic plate with the titanium plated surface is used as a cathode and is placed in an electrolytic bath containing acidic copper sulfate plating solution, refined copper is used as an anode, and the acidic copper sulfate plating solution comprises the following components in percentage by weight: 220g/L CuSO4·5H2O, 80g/L concentrated H with mass concentration of 98%2SO4The solvent is water; controlling the cathode current density to be 8A/dm2Forming a copper plating layer with the thickness of 100 microns on the surface of the aluminum nitride ceramic plate with the titanium conducting layer plated on the surface at the temperature of 50 ℃ for 10 min;
step S3: placing the aluminum nitride ceramic plate with the surface coated with the titanium conductive layer and the copper coating in sequence in a heat treatment furnace, filling argon into the heat treatment furnace, heating, keeping the temperature for 25min when the temperature reaches 400 ℃, and allowing the titanium conductive layer to penetrate into the aluminum nitride to form a TiN metallurgical transition layer and simple aluminum;
step S4: continuing heating and warming, keeping the temperature for 10min when the temperature reaches 700 ℃, simultaneously sending ultrasonic waves to the aluminum nitride ceramic plate through an ultrasonic wave generating device, enabling the frequency of the ultrasonic waves sent by the ultrasonic wave generating device to be 30 MHz, enabling the ultrasonic wave generating device to rotate around the heat treatment furnace, realizing that the ultrasonic waves are sent to the aluminum nitride ceramic plate in the heat treatment furnace at 360 degrees, enabling liquid elemental aluminum on the aluminum nitride ceramic plate to vibrate and last for 15min, filling argon into the heat treatment furnace, enabling the air pressure in the heat treatment furnace to reach 4 standard atmospheric pressures, enabling the liquid elemental aluminum to vibrate and flow out, and stabilizing a TiN metallurgy transition layer;
step S5: further heating to 900 ℃, and preserving heat for 30min, wherein the titanium conductive layer permeates into the copper coating to form a TiCu metallurgy transition layer.
The refined copper is used as the anode, so that other metals can be effectively prevented from being electroplated on the aluminum nitride ceramic plate, and the product quality is improved; ultrasonic waves are sent to the aluminum nitride ceramic plate through an ultrasonic wave generating device, so that liquid simple substance aluminum generated in the process that the titanium conductive layer penetrates into the aluminum nitride to form a TiN metallurgical transition layer can vibrate, and the liquid simple substance aluminum is fused and discharged out of the aluminum nitride ceramic plate; 3 standard atmospheric pressure to 4 standard atmospheric pressure's argon gas can effectively realize extrudeing aluminium nitride ceramic plate for liquid simple substance aluminium flows out, promotes production efficiency.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The method for metalizing the aluminum nitride ceramic plate is characterized by comprising the following steps of:
step S1: cleaning the surface of the aluminum nitride ceramic plate, and plating a titanium conducting layer with a set thickness on the surface of the aluminum nitride ceramic plate through vacuum magnetron sputtering;
step S2: taking an aluminum nitride ceramic plate with a titanium-plated surface as a cathode, placing the aluminum nitride ceramic plate in an electrolytic tank containing an acidic copper sulfate plating solution, taking refined copper as an anode, and controlling the current density of the cathode and the electroplating time to obtain a copper plating layer with a corresponding thickness;
step S3: placing the aluminum nitride ceramic plate with the surface coated with the titanium conducting layer and the copper coating in sequence in a heat treatment furnace, filling argon into the heat treatment furnace, heating, keeping the temperature for 25-30 min when the temperature reaches 300-400 ℃, and allowing the titanium conducting layer to penetrate into aluminum nitride to form a TiN metallurgy transition layer and simple substance aluminum;
step S4: continuing heating and raising the temperature, keeping the temperature for 10-15 min when the temperature reaches 600-700 ℃, simultaneously sending ultrasonic waves to the aluminum nitride ceramic plate through an ultrasonic wave generating device, and continuing for 10-15 min to enable liquid simple substance aluminum to vibrate and flow out, so that a TiN metallurgy transition layer is stabilized;
step S5: and further heating to 800-900 ℃, preserving the heat for 30-60 min, and enabling the titanium conductive layer to permeate into the copper coating to form a TiCu metallurgical transition layer.
2. The method of claim 1, wherein in step S1, the surface of the aluminum nitride ceramic plate is cleaned with 10% hydrochloric acid, then cleaned with clean water, and dried.
3. The method of claim 1, wherein the aluminum nitride ceramic plate having the titanium conductive layer plated on the surface thereof is subjected to copper electroplating in an acidic copper sulfate plating solution according to the following formula in step S2: 150-220 g/LCuSO4·5H2O, 50-80 g/L of concentrated H with mass concentration of 98%2SO4The solvent is water.
4. The method of claim 1 or 3, wherein the step S2, the electrolytic copper plating is performed by using fine copper as an anode and controlling the cathode current density to 3-8A/dm2The temperature is 30-50 ℃, and the time is 10-30 min, so that the aluminum nitride ceramics with the titanium conducting layer plated on the surface can be obtainedAnd forming a copper plating layer with the thickness of 5-100 microns on the surface of the porcelain plate.
5. The method of metallizing an aluminum nitride ceramic plate according to any one of claims 1 to 3, wherein the ultrasonic wave generator emits the ultrasonic wave to the aluminum nitride ceramic plate at a frequency of 1 MHz to 30 MHz in step S4.
6. The method of metallizing an aluminum nitride ceramic plate according to claim 5, wherein in step S4, argon gas is introduced into the heat treatment furnace so that the pressure in the heat treatment furnace can reach 3 to 4 standard atmospheres.
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| CN109136848B (en) * | 2018-07-17 | 2020-04-28 | 西安交通大学 | Method for connecting aluminum nitride ceramic plate and metal based on PVD (physical vapor deposition) deposition method |
| CN115286415A (en) * | 2022-06-28 | 2022-11-04 | 中国科学院合肥物质科学研究院 | Aluminum nitride copper-clad ceramic and preparation method and application thereof |
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| JPH07114316B2 (en) * | 1989-09-28 | 1995-12-06 | 電気化学工業株式会社 | Method for manufacturing aluminum nitride substrate having copper circuit |
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| JP2005272858A (en) * | 2004-03-22 | 2005-10-06 | Campus Create Co Ltd | Surface pretreatment method for light metal material |
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