CN110527964B - Diamond-like composite film, preparation method and application thereof, and IGBT module radiating substrate - Google Patents

Diamond-like composite film, preparation method and application thereof, and IGBT module radiating substrate Download PDF

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CN110527964B
CN110527964B CN201910827903.XA CN201910827903A CN110527964B CN 110527964 B CN110527964 B CN 110527964B CN 201910827903 A CN201910827903 A CN 201910827903A CN 110527964 B CN110527964 B CN 110527964B
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diamond
layer
carbon
carbon source
source gas
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殷录桥
张建华
王毅斌
张豆豆
汪飞
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University of Shanghai for Science and Technology
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/367—Cooling facilitated by shape of device
    • H01L23/3672—Foil-like cooling fins or heat sinks
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3731—Ceramic materials or glass
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates

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Abstract

The invention relates to the technical field of transistors, and provides a diamond-like composite film which sequentially comprises a metal base layer, a metal carbide gradient transition layer and a nitrogen and silver co-doped diamond-like thin film layer from bottom to top. The problem of overlarge contact angle between the diamond-like carbon film and metal is solved by arranging the metal carbide gradient transition layer; according to the invention, nitrogen and silver are doped in the diamond-like carbon film, so that the thermal stability of the diamond-like carbon film is improved, the internal stress of the diamond-like carbon film can be reduced, and the heat dissipation performance of the diamond-like carbon composite film is improved. The invention provides a preparation method of a diamond-like carbon composite film, which has simple steps and high quality of the obtained composite film. The invention also provides an IGBT module heat dissipation substrate and an IGBT module, wherein the diamond-like carbon composite film is prepared on the surface of the copper substrate of the traditional IGBT module, so that the heat conduction performance of the heat dissipation copper plate can be obviously improved, and the heat transfer capacity of the whole IGBT module is further improved.

Description

Diamond-like composite film, preparation method and application thereof, and IGBT module radiating substrate
Technical Field
The invention relates to the technical field of transistors, in particular to a diamond-like composite film, a preparation method and application thereof, and an IGBT module heat dissipation substrate.
Background
The IGBT (insulated gate bipolar transistor chip) is a power type semiconductor device consisting of a bipolar triode and an insulated gate field effect transistor, has the excellent characteristics of small driving power and low saturation voltage drop, and the IGBT module is a modular semiconductor product formed by bridging and packaging the IGBT and the FWD (freewheeling diode chip) through a specific circuit; the packaged IGBT module is directly applied to the fields of alternating current motors, traction transmission, switching power supplies, frequency converters, UPS and the like. The main work of the IGBT is to control and transmit electric energy, the IGBT composed of chips with the size of a nail cover can process over 6500W of ultrahigh voltage, the IGBT chips can realize 10 ten thousand times of current switching actions within 1 second of short time when working, so that high-speed running of high-speed rails is driven, however, the high-power and high-speed current switching of the IGBT modules causes huge heat productivity of the modules, the higher junction temperature can cause the fault rate of the chips to rise, the temperature rises by 10 ℃, the fault rate of the IGBT modules doubles, and the service life of the modules is seriously influenced.
When the chip works, the generated heat is conducted onto the heat dissipation substrate through the DBC substrate (ceramic copper clad substrate), and then is transmitted to the radiator through the heat conduction silica gel for heat dissipation, however, as the heat dissipation substrate is made of a material (generally copper), the heat conductivity is general, so that a large amount of heat is accumulated inside the module and cannot be timely transmitted out, and junction temperature is increased.
The diamond-like film is a hard coating with high thermal conductivity, high hardness, high wear resistance, high chemical stability and water lubricity, and is widely applied to the fields of heat dissipation, machining, electronic devices, optics, medicine and the like. The heat conductivity of the diamond-like film can reach 480W/m, and compared with 320W/mK of a traditional copper radiating substrate, the covering of the diamond-like film can improve the heat conducting performance of the whole radiating substrate, so that the heat conduction from the chip to the radiator is accelerated. But the diamond-like film and the substrate have low bonding force and large stress during deposition, so that the bonding interface is easy to peel off, and the service life is greatly shortened.
Disclosure of Invention
The invention aims to provide a diamond-like composite film, a preparation method and application thereof, and an IGBT module heat dissipation substrate. The diamond-like carbon film provided by the invention has strong binding force with a substrate and good heat conducting property, and can be applied to an IGBT module, so that the heat radiation performance of the IGBT module can be obviously improved.
In order to achieve the above object, the present invention provides the following technical solutions:
a diamond-like composite film comprises a metal base layer, a metal carbide gradient transition layer and a nitrogen-silver co-doped diamond-like thin film layer from bottom to top in sequence;
the metal elements in the metal base layer and the metal carbide gradient transition layer are the same;
the carbon content of the metal carbide gradient transition layer is gradually increased from bottom to top.
Preferably, the metal carbide gradient transition layer is plated by a direct-current magnetron sputtering method, the plating process comprises four stages, the flow ratio of carbon source gas and argon gas in the first stage is (1-3): 12-14), the flow ratio of carbon source gas and argon gas in the second stage is (2-4): 11-13), the flow ratio of carbon source gas and argon gas in the third stage is (3-5): 10-12, and the flow ratio of carbon source gas and argon gas in the fourth stage is (4-6): 9-11; in the four stages, the flow ratio of the carbon source gas gradually increases from the first stage to the fourth stage, and the sum of the flow rates of the carbon source gas and the argon gas is 15 sccm.
Preferably, the metal base layer is a chromium layer, a titanium layer or an aluminum layer; the metal carbide in the metal carbide gradient transition layer is chromium carbide, titanium carbide or aluminum carbide.
Preferably, the thickness of the metal base layer is 0.2-3 mu m, the thickness of the metal carbide gradient transition layer is 0.5-5 mu m, and the thickness of the nitrogen and silver co-doped diamond-like thin film layer is 8-20 mu m.
The invention provides a preparation method of the diamond-like carbon composite film, which comprises the following steps:
plating a metal base layer on the surface of the substrate by adopting direct current sputtering;
plating a metal carbide gradient transition layer on the surface of the metal base layer by adopting direct-current magnetron sputtering;
and plating a nitrogen-silver co-doped diamond-like carbon film layer on the surface of the metal carbide gradient transition layer by adopting radio frequency sputtering, and obtaining the diamond-like carbon composite film after the plating is finished.
Preferably, the atmosphere during plating the metal base layer is argon, the sputtering current during plating is 0.2-0.5A, and the deposition time is 45-300 min;
the process comprises four stages, wherein the flow ratio of carbon source gas to argon gas in the first stage is (1-3): 12-14, the plating time is 10-75 min, the flow ratio of carbon source gas to argon gas in the second stage is (2-4): 11-13), the plating time is 10-75 min, the flow ratio of carbon source gas to argon gas in the third stage is (3-5): 10-12, the plating time is 10-75 min, and the flow ratio of carbon source gas to argon gas in the fourth stage is (4-6): 9-11; the plating time is 10-75 min; in the four stages, the flow proportion of the carbon source gas is gradually increased from the first stage to the fourth stage, and the sum of the flow of the carbon source gas and the flow of the argon gas is 15 sccm; the sputtering current for plating the metal carbide gradient transition layer is 0.2-0.5A;
the atmosphere of the nitrogen and silver co-doped diamond-like carbon thin film layer is a mixed atmosphere of nitrogen and a carbon source gas, the plating comprises two stages, the flow ratio of the nitrogen to the carbon source gas in the first stage is (8-12): 13-17), the plating time is 5-20 min, the flow ratio of the nitrogen to the carbon source gas in the second stage is (8-12): 18-22), and the plating time is 4-20 h; the target material used in the process of plating the nitrogen and silver co-doped diamond-like carbon thin film layer is a silver target, and the sputtering current is 0.2-0.5A.
The invention provides application of the diamond-like carbon composite film in the scheme in heat dissipation of power electronic devices.
The invention provides an IGBT module radiating substrate which comprises a copper substrate and a diamond-like carbon composite film arranged on the surface of the copper substrate.
The invention also provides an IGBT module which comprises a radiator, a radiating substrate, a conductive substrate and an IGBT chip from bottom to top; the radiating substrate is the IGBT module radiating substrate in the scheme.
The invention provides a diamond-like composite film, which sequentially comprises a metal base layer, a metal carbide gradient transition layer and a nitrogen-silver co-doped diamond-like thin film layer from bottom to top; the metal elements in the metal base layer and the metal carbide gradient transition layer are the same; the carbon content of the metal carbide gradient transition layer is gradually increased from bottom to top. According to the invention, the problem of overlarge contact angle between the diamond-like carbon film and the metal base layer is solved by arranging the metal carbide gradient transition layer, so that the problem that the bonding interface of the diamond-like carbon film is easy to fall off is solved; the invention dopes nitrogen and silver in the diamond-like carbon film, which can reduce the internal stress while improving the thermal stability of the diamond-like carbon film, so that the diamond-like carbon composite film of the invention has good performance in heat dissipation.
The invention provides the preparation method of the diamond-like carbon composite film, which has the advantages of simple steps, easy operation and high quality of the prepared composite film.
The invention also provides an IGBT module heat dissipation substrate and an IGBT module, wherein the IGBT module heat dissipation substrate comprises a copper substrate and a diamond-like carbon composite film arranged on the surface of the copper substrate; the diamond-like composite film is prepared on the surface of the copper substrate of the traditional IGBT module, so that the heat conduction performance of the heat-radiating copper plate can be obviously improved, and the heat-radiating copper plate is protected to a certain extent. The heat dissipation substrate is applied to the IGBT module, so that the heat transfer capacity of the whole IGBT module can be remarkably improved, and the conduction of a large amount of heat generated by the chip during working from an IGBT device to a radiator is accelerated, so that the temperature and the chip junction temperature of the IGBT module during working are reduced, the failure rate of the IGBT module is reduced, and the service life of the IGBT module is prolonged. The embodiment result shows that when the composite film is applied to an IGBT module, the junction temperature of an IGBT chip can be reduced by 27 ℃.
Drawings
Fig. 1 is a schematic structural diagram of a copper substrate with a diamond-like carbon composite film plated on a single-side surface, wherein in fig. 1: 1 is a copper substrate, 2 is a metal base layer, 3 is a metal carbide gradient transition layer, and 4 is a nitrogen and silver co-doped diamond-like carbon film layer;
FIG. 2 is a schematic structural diagram of an IGBT module according to the present invention; in fig. 2: 5 is a solder layer, 6 is an IGBT chip, 7 is a conductive substrate, 8 is a heat dissipation substrate, 9 is a heat conduction silica gel layer, and 10 is a radiator.
Detailed Description
The invention provides a diamond-like composite film which sequentially comprises a metal base layer, a metal carbide gradient transition layer and a nitrogen and silver co-doped diamond-like thin film layer from bottom to top.
In the present invention, the metal base layer is preferably a chromium layer, a titanium layer or an aluminum layer, and the thickness of the metal base layer is preferably 0.2 to 3 μm, more preferably 0.5 to 2.5 μm, and further preferably 1 to 2 μm.
In the invention, the metal carbide in the metal carbide gradient transition layer is chromium carbide, titanium carbide or aluminum carbide; the metal elements in the metal base layer and the metal carbide gradient transition layer are the same; the thickness of the metal carbide gradient transition layer is preferably 0.5-5 μm, more preferably 1-4 μm, and even more preferably 2-3 μm.
In the invention, the carbon content of the metal carbide gradient transition layer is gradually increased from bottom to top, the lower part of the metal carbide gradient transition layer has low carbon content, so that the metal carbide gradient transition layer has good bonding force with a metal base layer, and the upper part of the metal carbide gradient transition layer has high carbon content, so that the metal carbide gradient transition layer has good bonding force with a nitrogen-silver co-doped diamond-like thin film layer.
In the invention, the metal carbide gradient transition layer is preferably plated by a direct current magnetron sputtering method, the plating process comprises four stages, the flow ratio of the carbon source gas and the argon gas in the first stage is preferably (1-3): 12-14), more preferably 2:13, the flow ratio of the carbon source gas and the argon gas in the second stage is preferably (2-4): 11-13, more preferably 3:12, the flow ratio of the carbon source gas and the argon gas in the third stage is preferably (3-5): 10-12, more preferably 4:11, and the flow ratio of the carbon source gas and the argon gas in the fourth stage is preferably (4-6): 9-11, more preferably 5: 10; the carbon source gas is preferably toluene; in the four stages, the flow ratio of the carbon source gas gradually increases from the first stage to the fourth stage, and the sum of the flow rates of the carbon source gas and the argon gas is 15 sccm. The proportion of carbon source gas is gradually increased in the plating process, so that the carbon content of the obtained metal carbide is gradually increased, and a metal carbide gradient transition layer is obtained; according to the invention, the problem of overlarge contact angle between the diamond-like carbon film and the metal base layer is solved by arranging the metal carbide gradient transition layer, and the problem that the bonding interface of the diamond-like carbon film is easy to fall off is further solved.
In the invention, the thickness of the nitrogen-silver co-doped diamond-like carbon film layer is preferably 8-20 μm, more preferably 10-18 μm, and further preferably 15 μm; the total doping amount of nitrogen and silver in the nitrogen and silver co-doped diamond-like carbon thin film layer is preferably 2-8 wt.%, and more preferably 3-5 wt.%, and the nitrogen and silver co-doped diamond-like carbon thin film layer has no special requirement on the doping ratio of nitrogen and silver, and can be doped at any ratio; according to the invention, the thermal stability of the diamond-like carbon film is improved through nitrogen and silver codoping, and meanwhile, the internal stress of the diamond-like carbon film can be reduced, and the heat conductivity of the diamond-like carbon film is improved.
In the invention, the thermal conductivity of the diamond-like carbon composite film can reach 400W/(m.K).
The invention provides a preparation method of a diamond-like carbon composite film, which comprises the following steps:
plating a metal base layer on the surface of the substrate by adopting direct current sputtering;
plating a metal carbide gradient transition layer on the surface of the metal base layer by adopting direct-current magnetron sputtering;
and plating a nitrogen-silver co-doped diamond-like carbon film layer on the surface of the metal carbide gradient transition layer by adopting radio frequency sputtering, and obtaining the diamond-like carbon composite film after the plating is finished.
The device used by the invention preferably comprises radio frequency sputtering and direct current sputtering at the same time, in the sputtering process, the direct current sputtering power supply and the radio frequency sputtering power supply are switched according to actual needs, and the switch of magnetron sputtering is controlled according to the actual needs.
The present invention does not require the substrate to be specially designed, and any metal substrate known to those skilled in the art can be used as the heat dissipation plate, specifically, a copper plate. Before the substrate is placed into a sputtering device, the substrate is preferably cleaned to remove impurities on the surface of the substrate, so that the growth of a thin film is facilitated; the cleaning is preferably ultrasonic cleaning using acetone, ethanol and deionized water in sequence.
After the cleaning is finished, the cleaned matrix is preferably loaded into a vacuum chamber of a sputtering device; prior to sputtering, the present invention preferably performs sputter cleaning of the target and substrate surfaces, said sputter cleaning preferably comprising the steps of:
(1) and (3) vacuumizing by using a mechanical pump, introducing Ar gas for 5min when the pressure in the vacuum cavity is reduced to be below 5Pa, cleaning the valve, closing the valve after the gas flowmeter is stabilized, closing an Ar gas switch, repeating for 5 times, and exhausting the air in the Ar gas pipeline. Then introducing nitrogen and carbon source gas toluene, pumping the valve to clean, closing the valve after the gas flowmeter is stable, closing the two gas switches, repeating for 5 times, and exhausting the air in the nitrogen and carbon source gas pipelines;
(2) continuing to vacuumize, turning on the molecular pump after the pressure in the vacuum cavity is reduced to below 5Pa, exhausting the air in the vacuum cavity and the gas pipeline according to the method in the step (1), and finally turning off the nitrogen N2And a switch of the carbon source gas, and continuously utilizing the mechanical pump and the molecular pump to vacuumize the vacuum chamber;
(3) the pressure in the vacuum chamber dropped to 4 × 10-4Introducing Ar gas after Pa is less than Pa, and opening a switch to control the valve to control the gas flow to be 20 sccm; when the air pressure in the vacuum chamber is 0.3Pa, a radio frequency power source of the base station is turned on, the current is adjusted to be 0.3A, the voltage is 320V, and the radio frequency power is 96W;
(4) after 10min, the DC sputtering power supply is turned on, the current is adjusted to be 0.2A, the DC sputtering voltage is 330V, and the power is 66W. Ar under the action of electric field+Bombarding the target material to remove pollutants and oxide layers on the surface of the target material and the substrate, wherein the whole surface cleaning process lasts for about 5 min.
After the sputtering cleaning is finished, the invention adopts direct current sputtering to plate a metal base layer on the surface of the substrate. In the invention, the atmosphere of the metal base layer is preferably argon, the direct current of the metal base layer during plating is preferably 0.2-0.5A, more preferably 0.3A, and the deposition time is preferably 45-300 min, more preferably 60-250 min; in the specific embodiment of the invention, the sputtering target material is selected according to the material of the target metal layer, and specifically comprises a chromium target, an aluminum target or a titanium target; the invention has no special requirement on the purity of the target material, and the target material with the purity commonly used in the field can be used; when the metal base layer is plated, the power supply is a direct current sputtering power supply, and the magnetic control switch is kept closed.
In the embodiment of the invention, the carbon source gas switch is preferably opened (the carbon source gas valve is kept closed) 20min before the end of the metal layer plating, so that the carbon source gas is filled in the pipeline, and the subsequent metal carbide gradient transition layer plating is facilitated.
After the metal base layer is obtained, the invention adopts direct current magnetron sputtering to plate a metal carbide gradient transition layer on the surface of the metal base layer. In the invention, the atmosphere for plating the metal carbide gradient transition layer is preferably a mixed atmosphere of argon and a carbon source gas, and the carbon source gas is preferably toluene; the plating process preferably comprises four stages, the flow ratio of the carbon source gas and the argon gas in the first stage is preferably (1-3): 12-14), more preferably 2:13, the plating time is preferably 10-75 min, the flow ratio of the carbon source gas and the argon gas in the second stage is preferably (2-4): 11-13), more preferably 3:12, the plating time is preferably 10-75 min, the flow ratio of the carbon source gas and the argon gas in the third stage is preferably (3-5): 10-12, more preferably 4:11, the plating time is preferably 10-75 min, the flow ratio of the carbon source gas and the argon gas in the fourth stage is preferably (4-6): 9-11, more preferably 5:10, and the plating time is preferably 10-75 min; in the four stages, the flow proportion of the carbon source gas is gradually increased from the first stage to the fourth stage, and the sum of the flow of the carbon source gas and the flow of the argon gas is 15 sccm; in the whole plating process, the direct current is preferably kept at 0.2-0.5A, more preferably 0.3A, the metal target is continuously sputtered, and the used metal target is consistent with the target when the metal base layer is plated. When the metal carbide gradient transition layer is plated, the power supply is a direct current sputtering power supply, and the magnetic control switch is turned on.
After the metal carbide gradient transition layer is obtained, the invention adopts radio frequency sputtering to plate a nitrogen and silver co-doped diamond-like carbon film layer on the surface of the metal carbide gradient transition layer, and the diamond-like carbon composite film is obtained after the plating is finished. In the invention, the atmosphere for plating the nitrogen-silver co-doped diamond-like thin film layer is a mixed atmosphere of nitrogen and a carbon source gas, wherein the carbon source gas is preferably toluene; the plating preferably comprises two stages, the flow ratio of nitrogen to carbon source gas in the first stage is preferably (8-12): 13-17), more preferably 10:15, the plating time is preferably 5-20 min, more preferably 10min, the flow ratio of nitrogen to carbon source gas in the second stage is preferably (8-12): 18-22, more preferably 10:20, and the plating time is preferably 4-20 h, more preferably 8 h. According to the invention, the plating is firstly carried out for a period of time (namely the first stage) under the condition that the flow proportion of the carbon source gas is low, so that the yield of the nitrogen-silver co-doped diamond-like carbon film layer can be improved; the invention controls the thickness of the nitrogen-silver co-doped diamond-like carbon film layer by controlling the plating time of the second stage. When the metal carbide gradient is plated, the used target material is a silver target, the power supply is a radio frequency sputtering power supply, the magnetic control switch is turned off, and the current in the whole plating process is preferably 0.2-0.5A, more preferably 0.3A.
The invention provides application of the diamond-like carbon composite film in the scheme in heat dissipation of power electronic devices. The invention has no special requirements on the types of the power electronic devices, the power electronic devices with large power and limited heat dissipation modes in the field can be applied with the diamond-like composite film to improve the heat dissipation efficiency, and the diamond-like composite film can be directly plated on the surface of a heat dissipation plate of the power electronic device during application.
The invention also provides an IGBT module radiating substrate which comprises a copper substrate and the diamond-like carbon composite film arranged on the surface of the copper substrate; in the invention, the diamond-like carbon composite film can be arranged on one side surface of the copper substrate, and also can be arranged on two side surfaces of the copper substrate; in the embodiment of the invention, the diamond-like carbon film is preferably arranged on the surfaces of the two sides of the copper substrate, so that the heat dissipation efficiency of the heat dissipation substrate can be further improved. During preparation, the diamond-like carbon composite film is directly plated on the surface of the copper substrate, and the plating method is consistent with the scheme and is not repeated. The schematic diagram of the copper substrate with the diamond-like carbon composite film plated on the single-side surface is shown in fig. 1, wherein in fig. 1, 1 is a copper substrate, 2 is a metal base layer, 3 is a metal carbide gradient transition layer, and 4 is a nitrogen and silver co-doped diamond-like carbon film layer.
In the invention, the diamond-like carbon composite film is plated on the surface of the copper substrate, so that the heat conducting property of the copper substrate can be obviously improved, the nitrogen and silver co-doped diamond-like carbon thin film layer in the diamond-like carbon composite film is not directly contacted with the copper substrate but is indirectly combined with the copper substrate through the metal base layer and the metal carbide gradient transition layer, the metal base layer and the copper substrate have strong bonding force, and the nitrogen and silver co-doped diamond-like carbon thin film layer and the metal carbide gradient have strong bonding force, so that the problems of poor bonding force and easy falling of the diamond-like carbon thin film and the substrate in the prior art can be solved, and the service life is prolonged.
The invention also provides an IGBT module which comprises a radiator, a radiating substrate, a conductive substrate and an IGBT chip from bottom to top; the radiating substrate is the IGBT module radiating substrate in the scheme. The invention has no special requirements on the radiator, the conductive substrate and the IGBT chip, and the radiator, the conductive substrate and the IGBT chip can be manufactured by using the components which are well known by the technical personnel in the field; in a specific embodiment of the present invention, the conductive substrate is preferably a PCB panel (printed circuit board) or a DBC substrate (copper clad ceramic substrate).
In a specific embodiment of the present invention, the IGBT chip is preferably soldered on a conductive substrate by ultrasonic bonding and soldering techniques, the conductive substrate is soldered on a heat dissipation substrate, and the heat dissipation substrate is bonded to the heat sink by a heat conductive silicone grease.
In the present invention, the specific structure of the IGBT module is shown in fig. 2, where 5 is a solder layer, 6 is an IGBT chip, 7 is a conductive substrate, 8 is a heat dissipation substrate, 9 is a heat conductive silica gel layer, and 10 is a heat sink.
The diamond-like composite film is applied to the IGBT module, so that the heat transfer capacity of the whole IGBT module can be improved, and the conduction of a large amount of heat generated by the chip during working from an IGBT device to a radiator is accelerated, so that the temperature and the junction temperature of the chip during working of the IGBT module are reduced, the failure rate of the IGBT module is reduced, and the service life of the IGBT module is prolonged.
The embodiments of the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Preparing an IGBT module radiating substrate, plating a diamond-like composite film on the surface of a copper substrate, wherein a metal base layer is a chromium layer, and a metal carbide in a metal carbide gradient transition layer is chromium carbide, and the preparation method comprises the following specific steps:
the method comprises the following steps of (A) respectively carrying out ultrasonic cleaning on a copper substrate by using acetone, ethanol and deionized water, putting the copper substrate into a vacuum chamber after airing, and then carrying out sputtering cleaning on the surfaces of a target material and the copper substrate, wherein the cleaning steps are as follows:
(1) firstly, using a mechanical pump to pump vacuum, when the pressure in a vacuum cavity is reduced to be below 5Pa, introducing Ar gas for 5min, cleaning a valve, closing the valve after a gas-carrying flowmeter is stabilized, closing an Ar gas switch, repeating for 5 times, and evacuating the air in an Ar gas pipeline. Then nitrogen N is introduced2And cleaning the carbon source gas toluene, closing the valve after the gas flowmeter is stabilized, closing the two gas switches, repeating the operation for 5 times, and emptying the air in the pipeline.
(2) Continuing to vacuumize, after the pressure in the cavity is reduced to below 5Pa, opening the molecular pump, continuing to remove the air in the vacuum cavity and the gas pipeline as in the step (1), and finally closing the nitrogen N2And a carbon source gas toluene switch, and continuously utilizing a mechanical pump and a molecular pump to vacuumize the vacuum chamber.
(3) The pressure in the vacuum chamber dropped to 4 × 10-4And after Pa is less than Pa, introducing Ar gas, and opening a switch to control the valve to control the gas flow to be 20 sccm. When the air pressure in the vacuum chamber is 0.3Pa, the RF power source of the base station is turned on, the current is adjusted to 0.3A, the voltage is 320V, and the RF power is 96W.
(4) After 10min, the DC sputtering power supply is turned on, the current is adjusted to be 0.2A, the DC sputtering voltage is 330V, and the power is 66W. Under the action of electric fieldAr+Bombarding the target material to remove pollutants and oxide layers on the surface of the target material and the substrate, wherein the whole surface cleaning process lasts for about 5 min.
And (II) after the sputtering cleaning of the target and the substrate surface is finished, opening an Ar gas switch, opening a valve to control the valve, controlling the flow of the Ar gas to be stable at 15sccm, setting the direct current at 0.3A, and depositing for 25 min. And opening a carbon source gas toluene switch, keeping a valve in a closed state, and continuing to deposit for 20 min. To this end, a pure chromium layer was prepared with a thickness of 0.3 μm.
(III) introducing carbon source gas toluene, controlling the valve to be valve-controlled, controlling the gas flow to be 2sccm, regulating the Ar gas flow to be 13sccm, and depositing for 10 min; regulating the flow rate of toluene gas to be 3sccm, regulating the flow rate of Ar gas to be 12sccm, and depositing for 10 min; regulating the flow rate of toluene gas to 4sccm, regulating the flow rate of Ar gas to 11sccm, and depositing for 10 min; regulating the flow rate of toluene gas to 5sccm, regulating the flow rate of Ar gas to 10sccm, and depositing for 10 min; during this process, the direct current was kept at 0.3A, and the sputtering of the chromium target was continued. To this end, a graded transition layer of chromium carbide compound was prepared to a thickness of 0.8 μm.
And (IV) cleaning a valve of carbon source gas toluene, opening a silver target baffle, opening a nitrogen valve, enabling the gas flow to be 10sccm, closing a chromium target baffle, switching a direct current power supply, and keeping the current of a sputtering power supply of the silver target at 0.3A. And (3) pumping a toluene gas valve to a valve control mode, controlling the gas flow to be 15sccm, depositing for 10min, then controlling the toluene gas flow to be 20sccm, and depositing for 8h, so that the preparation of the nitrogen-silver co-doped diamond-like thin film layer is completed, and the thickness is 9.6 microns.
Plating the same diamond-like composite film on the other surface of the copper substrate under the same conditions as the steps from the first step to the fourth step.
Example 2
Other conditions were the same as in example 1 except that only the metal base layer was replaced with a titanium layer, the metal carbide in the metal carbide gradient transition layer was replaced with titanium carbide, and the thickness of each layer was the same as in example 1.
Example 3
Other conditions were the same as in example 1 except that only the metal base layer was replaced with the aluminum layer, the metal carbide in the metal carbide gradient transition layer was replaced with aluminum carbide, and the thickness of each layer was the same as in example 1.
Example 4
The other conditions were the same as those of example 1, and the thickness of the chromium layer in the step (II) was controlled to be 3 μm, the thickness of the metal carbide gradient transition layer in the step (III) was controlled to be 5 μm, and the thickness of the nitrogen-silver co-doped diamond-like thin film layer in the step (IV) was controlled to be 15 μm, by changing only the sputtering time.
Example 5
Other conditions were the same as those in example 1, and only the surface of one side of the copper substrate was coated with the diamond-like composite film.
And (3) testing thermal conductivity:
the thermal conductivity of the copper substrates plated with the diamond-like composite films in examples 1, 3 and 5 was measured, and the results are shown in table 1:
TABLE 1 thermal conductivity of copper substrates before and after coating
Figure BDA0002189709380000101
Figure BDA0002189709380000111
As can be seen from table 1, the thermal conductivity of the copper substrate was significantly improved after plating the diamond-like composite film of the present invention.
In addition, the thermal conductivity of the copper substrate plated with the diamond-like carbon composite film in the examples 2 and 4 is tested, and the test result shows that the thermal conductivity of the copper substrate is also obviously improved.
Example 6
In this embodiment, an IGBT module is prepared, and the heat dissipation substrate prepared in embodiment 1 is applied to the IGBT module, and the specific steps are as follows:
the IGBT chip is soldered to the copper clad ceramic substrate DBC by ultrasonic bonding and soldering techniques, the circuit substrate is soldered to the heat dissipation substrate prepared in example 1, and then the heat conduction substrate of the IGBT module and the heat sink are bonded together by the heat conduction silicone grease.
Comparative example 1
Other conditions were the same as in example 6, and an IGBT module was prepared using only a general copper substrate as a heat dissipation plate.
Junction temperatures of the IGBT chips in the IGBT modules prepared in example 6 and comparative example 1 were tested, and the results showed: the junction temperature of the IGBT chip in the IGBT module prepared in comparative example 1 was 132 ℃, the junction temperature of the IGBT chip in the IGBT module obtained in example 6 was 105 ℃, and decreased by 27 ℃ compared to comparative example 1. The diamond-like carbon composite film disclosed by the invention is applied to the IGBT module, so that the heat dissipation capability of the IGBT module can be improved, and the service life of the IGBT module is further prolonged.
The embodiment shows that the diamond-like composite film provided by the invention has good thermal conductivity and strong bonding force with the substrate, can be applied to the IGBT module, can obviously improve the heat dissipation capability of the IGBT module, and has wide application prospect in the heat dissipation of power electronic devices.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A diamond-like composite film is characterized by sequentially comprising a metal base layer, a metal carbide gradient transition layer and a nitrogen-silver co-doped diamond-like thin film layer from bottom to top;
the metal elements in the metal base layer and the metal carbide gradient transition layer are the same;
the carbon content of the metal carbide gradient transition layer is gradually increased from bottom to top; the thickness of the nitrogen and silver co-doped diamond-like carbon film layer is 8-20 mu m; the total doping amount of nitrogen and silver in the nitrogen and silver co-doped diamond-like carbon thin film layer is 2-8 wt.%.
2. A diamond-like composite film as in claim 1, wherein the metal carbide gradient transition layer is coated by a DC magnetron sputtering method, the coating process comprises four stages, the flow ratio of carbon source gas and argon gas in the first stage is (1-3): 12-14), the flow ratio of carbon source gas and argon gas in the second stage is (2-4): 11-13), the flow ratio of carbon source gas and argon gas in the third stage is (3-5): 10-12, and the flow ratio of carbon source gas and argon gas in the fourth stage is (4-6): 9-11); in the four stages, the flow ratio of the carbon source gas gradually increases from the first stage to the fourth stage, and the sum of the flow rates of the carbon source gas and the argon gas is 15 sccm.
3. The diamond-like composite film according to claim 1, wherein the metal base layer is a chromium layer, a titanium layer, or an aluminum layer; the metal carbide in the metal carbide gradient transition layer is chromium carbide, titanium carbide or aluminum carbide.
4. The diamond-like composite film according to claim 1, wherein the metal base layer has a thickness of 0.2 to 3 μm, and the metal carbide gradient transition layer has a thickness of 0.5 to 5 μm.
5. A method for preparing a diamond-like composite film according to any one of claims 1 to 4, comprising the steps of:
plating a metal base layer on the surface of the substrate by adopting direct current sputtering;
plating a metal carbide gradient transition layer on the surface of the metal base layer by adopting direct-current magnetron sputtering;
and plating a nitrogen-silver co-doped diamond-like carbon film layer on the surface of the metal carbide gradient transition layer by adopting radio frequency sputtering, and obtaining the diamond-like carbon composite film after the plating is finished.
6. The method according to claim 5, wherein the atmosphere for plating the metal substrate is argon, the sputtering current for plating is 0.2 to 0.5A, and the deposition time is 45 to 300 min;
the process comprises four stages, wherein the flow ratio of carbon source gas to argon gas in the first stage is (1-3) - (12-14), the plating time is 10-75 min, the flow ratio of carbon source gas to argon gas in the second stage is (2-4) - (11-13), the plating time is 10-75 min, the flow ratio of carbon source gas to argon gas in the third stage is (3-5) - (10-12), the plating time is 10-75 min, the flow ratio of carbon source gas to argon gas in the fourth stage is (4-6) - (9-11), and the plating time is 10-75 min; in the four stages, the flow proportion of the carbon source gas is gradually increased from the first stage to the fourth stage, and the sum of the flow of the carbon source gas and the flow of the argon gas is 15 sccm; the sputtering current for plating the metal carbide gradient transition layer is 0.2-0.5A;
the atmosphere of the nitrogen and silver co-doped diamond-like carbon thin film layer is a mixed atmosphere of nitrogen and a carbon source gas, the plating comprises two stages, the flow ratio of the nitrogen to the carbon source gas in the first stage is (8-12): 13-17), the plating time is 5-20 min, the flow ratio of the nitrogen to the carbon source gas in the second stage is (8-12): 18-22), and the plating time is 4-20 h; the target material used in the process of plating the nitrogen and silver co-doped diamond-like carbon thin film layer is a silver target, and the sputtering current is 0.2-0.5A.
7. Use of the diamond-like composite film according to any one of claims 1 to 4 for heat dissipation in power electronic devices.
8. An IGBT module heat dissipation substrate, characterized by comprising a copper substrate and the diamond-like carbon composite film of any one of claims 1 to 4 arranged on the surface of the copper substrate.
9. An IGBT module is characterized by comprising a radiator, a radiating substrate, a conductive substrate and an IGBT chip from bottom to top; the heat dissipation substrate is the IGBT module heat dissipation substrate according to claim 8.
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