CN116121696A - Device and method for preparing ceramic-based copper-clad plate - Google Patents

Device and method for preparing ceramic-based copper-clad plate Download PDF

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CN116121696A
CN116121696A CN202211727318.0A CN202211727318A CN116121696A CN 116121696 A CN116121696 A CN 116121696A CN 202211727318 A CN202211727318 A CN 202211727318A CN 116121696 A CN116121696 A CN 116121696A
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ceramic
ion beam
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ceramic substrate
copper
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请求不公布姓名
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Beijing Science And Tech Research Inst
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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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • 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
    • C23C14/221—Ion beam deposition

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Abstract

The invention provides a device and a method for preparing a ceramic-based copper-clad plate, and belongs to the technical field of ceramic substrates. The device provided by the invention realizes micro-reduction of the surface of the ceramic substrate by using the kofmann ion source equipment, realizes metal element injection by using the high-energy ion beam equipment, enables the ceramic substrate and injected metal atoms to form a ceramic-metal mixed layer, and simultaneously forms a transition layer by using the low-energy ion beam equipment, wherein the ceramic-metal mixed layer has good bonding force with the ceramic substrate layer and the transition layer, thereby improving the bonding force between the ceramic substrate and a copper film layer formed by deposition of the subsequent high-pulse low-energy ion beam equipment and enhancing the peeling strength of the copper film layer. The device provided by the invention can solve the problem that the traditional copper-clad technology can not simultaneously meet the requirements of a high-density ultrathin copper-clad layer, high peel strength and low interface roughness of a ceramic-based copper-clad plate, and can meet the requirements of a high frequency ceramic-based copper-clad plate.

Description

Device and method for preparing ceramic-based copper-clad plate
Technical Field
The invention relates to the technical field of ceramic circuit boards, in particular to a device and a method for preparing a ceramic-based copper-clad plate.
Background
The conventional method for manufacturing the alumina ceramic circuit board is to print a conductive coating on a ceramic plate, and then directly bond a copper foil to the surface (single-sided or double-sided) of the alumina ceramic substrate at high temperature using a sintering process. In addition, the existing method also adopts a physical vapor deposition mode to prepare a copper-clad layer, and common modes include a magnetron sputtering method, multi-arc ion plating, electron beam evaporation and the like. However, the interface roughness of the copper-clad layer prepared by the sintering method is higher, and the thinner the copper layer thickness is, the higher the cost is, and the lower the yield is. The magnetron sputtering and electron beam evaporation modes have low ion energy, so that the magnetron sputtering and electron beam evaporation modes have weak bonding force with the ceramic substrate. Although the multi-arc ion plating has higher energy, the plasma led out by the multi-arc ion plating has a plurality of larger particles, and the formed coating has poor compactness and high roughness.
Disclosure of Invention
The invention aims to provide a device and a method for preparing a ceramic-based copper-clad plate, which can simultaneously meet the requirements of a high-density ultrathin copper-clad layer, high peel strength and low interface roughness of the ceramic-based copper-clad plate.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a device for preparing a ceramic-based copper-clad plate, which comprises a vacuum chamber 101, a koufman gas ion source device 102, a high-energy ion beam device 103, a low-energy ion beam device 104 and a high-pulse low-energy ion beam device 105; the kaufman ion source apparatus 102, the high energy ion beam apparatus 103, the low energy ion beam apparatus 104, and the high pulse low energy ion beam apparatus 105 are respectively disposed at four ends of the vacuum chamber 101.
Preferably, a workpiece tray 106 is also included; the workpiece tray 106 is disposed in the vacuum chamber 101.
The invention provides a method for preparing a ceramic-based copper-clad plate by using the device for preparing the ceramic-based copper-clad plate, which comprises the following steps:
performing surface reduction on the ceramic substrate placed in the vacuum chamber 101 by adopting the kaufman gas ion source equipment 102 to obtain a first processed ceramic substrate;
injecting metal on the surface of the first processed ceramic substrate by adopting high-energy ion beam equipment 103, and connecting keys to obtain a second processed ceramic substrate;
performing first surface deposition on the second processed ceramic substrate by using a low-energy ion beam device 104 to form a transition layer;
and (3) carrying out second surface deposition on the transition layer by adopting high-pulse low-energy ion beam equipment 105 to form a copper layer, thereby obtaining the ceramic-based copper-clad plate.
Preferably, the flow rate of the argon gas for surface reduction is 20-80 sccm, the flow rate of the hydrogen gas is 0-40 sccm, the voltage is 20-40 KV, the beam intensity is 1-50 mA, and the treatment time is 20-60 min.
Preferably, after the surface reduction is performed, the surface roughness of the ceramic substrate varies by 0.1 μm or less.
Preferably, the metal element used for the injection metal includes Ti, al, ni, cr or Cu.
Preferably, the beam intensity of the connecting key is 10-100 mA, the energy is 10-40 keV, and the injection dosage is 1× (10 15 ～10 17 )ions/cm 2 。
Preferably, the element of the transition layer is Ni and/or Cr, the arcing current deposited on the first surface is 60-150A, the bias voltage is 0-300V, the duty ratio is 20-95%, and the deposition thickness is 10-100 nm.
Preferably, the arcing current of the second surface deposition is 60-150A, the bias voltage is 0-7 kV and is not 0, the frequency is 0-200 Hz and is not 0, and the deposition thickness is 1-9 mu m.
Preferably, the surface roughness of the ceramic-based copper-clad plate is less than 0.2 mu m.
The invention provides a device for preparing a ceramic-based copper-clad plate, which comprises a vacuum chamber 101, a koufman gas ion source device 102, a high-energy ion beam device 103, a low-energy ion beam device 104 and a high-pulse low-energy ion beam device 105; the kaufman ion source apparatus 102, the high energy ion beam apparatus 103, the low energy ion beam apparatus 104, and the high pulse low energy ion beam apparatus 105 are respectively disposed at four ends of the vacuum chamber 101. The device provided by the invention realizes micro-reduction of the surface of the ceramic substrate by using the kofmann ion source equipment, realizes metal element injection by using the high-energy ion beam equipment, enables the ceramic substrate and injected metal atoms to form a ceramic-metal mixed layer, and simultaneously forms a transition layer by using the low-energy ion beam equipment, wherein the ceramic-metal mixed layer has good bonding force with the ceramic substrate layer and the transition layer, thereby improving the bonding force between the ceramic substrate and a copper film layer formed by deposition of the subsequent high-pulse low-energy ion beam equipment and enhancing the peeling strength of the copper film layer.
The deposited copper-clad plate prepared by the device disclosed by the invention does not increase the original interface roughness of ceramics, can keep the surface roughness of the original ceramics, has low interface roughness, can avoid skin effect caused by copper teeth generated in a traditional mode, and reduces loss in the high-frequency signal transmission process; the copper-clad plate prepared by the device has low interface roughness, and the copper layer is thin, so that the preparation of a fine circuit board with the line width and line distance smaller than 15/15 micrometers can be realized; the invention can lead out ion beam spots with the ionization rate higher than 90% by using high-pulse low-energy ion beam equipment, thereby obtaining a high-density ultrathin copper-clad layer (the thickness of the copper layer is 1-9 mu m). Therefore, the device provided by the invention can solve the problem that the traditional copper-clad technology can not simultaneously meet the requirements of a high-density ultrathin copper-clad layer, high peel strength and low interface roughness of a ceramic-based copper-clad plate, and can obtain the ceramic-based copper-clad plate meeting the high-frequency requirements.
Drawings
FIG. 1 is a top view of an apparatus for producing a ceramic-based copper-clad plate according to the present invention;
FIG. 2 is a flow chart of the preparation of a ceramic-based copper clad laminate according to the present invention;
FIG. 3 is a surface topography of a ceramic-based copper clad laminate prepared in example 1;
FIG. 4 is a graph showing the results of roughness test of the ceramic-based copper clad laminates prepared in examples 1 to 3 and comparative examples 1 to 3;
fig. 5 is a graph showing the bonding force test results of the ceramic-based copper clad laminates prepared in examples 1 to 3 and comparative examples 1 to 3.
Detailed Description
As shown in fig. 1, the present invention provides an apparatus for preparing a ceramic-based copper-clad plate, which comprises a vacuum chamber 101, a kaufman gas ion source device 102, a high-energy ion beam device 103, a low-energy ion beam device 104 and a high-pulse low-energy ion beam device 105; the kaufman ion source apparatus 102, the high energy ion beam apparatus 103, the low energy ion beam apparatus 104, and the high pulse low energy ion beam apparatus 105 are respectively disposed at four ends of the vacuum chamber 101.
In the present invention, the required equipment is commercially available equipment well known to those skilled in the art unless specified otherwise.
The device for preparing the ceramic-based copper-clad plate provided by the invention comprises a vacuum chamber 101. The present invention utilizes a vacuum chamber 101 to provide a vacuum environment.
The device for preparing the ceramic-based copper-clad plate provided by the invention comprises a kaufman gas ion source device 102. The present invention utilizes the kaufman gas ion source apparatus 102 to perform kaufman gas ion source processing on a workpiece.
The device for preparing the ceramic-based copper-clad plate provided by the invention comprises high-energy ion beam equipment 103. The present invention utilizes a high energy ion beam apparatus 103 to perform metal implantation on a workpiece.
The apparatus for preparing a ceramic-based copper-clad plate provided by the invention comprises a low-energy ion beam device 104. The present invention utilizes a low energy ion beam apparatus 104 for surface deposition of a workpiece.
The device for preparing the ceramic-based copper-clad plate comprises high-pulse low-energy ion beam equipment 105. The present invention utilizes a high pulse low energy ion beam apparatus 105 for surface deposition of a workpiece.
As an embodiment of the present invention, the apparatus for preparing a ceramic-based copper-clad plate provided by the present invention further includes a workpiece tray 106; the workpiece tray 106 is disposed in the vacuum chamber 101. The present invention utilizes a workpiece tray 106 to hold the workpieces to be prepared.
As shown in fig. 2, the invention provides a method for preparing a ceramic-based copper-clad plate by using the device for preparing a ceramic-based copper-clad plate, which comprises the following steps:
performing surface reduction on the ceramic substrate placed in the vacuum chamber 101 by adopting the kaufman gas ion source equipment 102 to obtain a first processed ceramic substrate;
injecting metal on the surface of the first processed ceramic substrate by adopting high-energy ion beam equipment 103, and connecting keys to obtain a second processed ceramic substrate;
performing first surface deposition on the second processed ceramic substrate by using a low-energy ion beam device 104 to form a transition layer;
and (3) carrying out second surface deposition on the transition layer by adopting high-pulse low-energy ion beam equipment 105 to form a copper layer, thereby obtaining the ceramic-based copper-clad plate.
In the present invention, the preparation materials are commercially available as known to those skilled in the art unless otherwise specified.
The present invention employs a kaufman gas ion source apparatus 102 for surface reduction of a ceramic substrate placed in a vacuum chamber 101 to obtain a first processed ceramic substrate.
In the present invention, the ceramic substrate is preferably an alumina ceramic plate or an aluminum nitride ceramic plate.
In the present invention, the flow rate of the surface-reduced argon gas is preferably 20 to 80sccm, more preferably 20 to 60sccm; the flow rate of the hydrogen gas is preferably 0 to 40sccm, more preferably 30sccm; the voltage is preferably 20-40 KV, more preferably 30KV; the beam intensity is preferably 1-50 mA, more preferably 30mA; the treatment time is preferably 20 to 60 minutes, more preferably 40 minutes.
In the present invention, the change in the surface roughness of the ceramic substrate after the surface reduction is preferably 0.1 μm or less. The invention cleans the dirty surface of the ceramic substrate by the koufman gas ion source, and performs bond breaking and micro-reduction on the surface to realize surface activation and improve the binding force.
After the first processed ceramic substrate is obtained, the high-energy ion beam equipment 103 is adopted to inject metal on the surface of the first processed ceramic substrate, and bonding is carried out, so that the second processed ceramic substrate is obtained. In the present invention, the metal element used for the injection metal preferably includes Ti, al, ni, cr or Cu.
In the invention, the beam intensity of the bonding is preferably 10-100 mA, more preferably 20mA; the energy is preferably 10 to 40keV, more preferably 20keV; the implantation dose is preferably 1× (10 15 ～10 17 )ions/cm 2 More preferably 1X 10 16 ions/cm 2 . The invention uses the high-energy ion beam technology to bond the broken bonds and the micro-reduction surfaces of the ceramic substrate after the metal elements are treated by the kaufman gas ion source to form a ceramic-metal mixed layer combined by chemical bonds, thereby improving the bonding force of the ceramic substrate and the transition layer and further improving the bonding force of the ceramic substrate and the subsequent copper-clad layerForce. For example, ni is formed on the ceramic surface layer by Ni compounds (NiO and NiAl 2 O 4 ) Is present in the form of (c).
After the second processed ceramic substrate is obtained, the invention adopts the low-energy ion beam equipment 104 to carry out first surface deposition on the second processed ceramic substrate to form a transition layer. In the invention, the target material used for the first surface deposition is preferably Ni, cr or NiCr alloy target material with any proportion; the elements of the transition layer are preferably Ni and/or Cr, and when the elements of the transition layer are Ni and Cr, the proportion of Ni and Cr is not particularly limited, and any proportion can be adopted; in the embodiment of the invention, the NiCr alloy with the atomic mass ratio of 8:2 is specifically adopted; the arcing current of the first surface deposition is preferably 60-150A, more preferably 100A; the bias voltage is preferably 0 to 300V, more preferably 200V; the duty cycle is preferably 20 to 95%, more preferably 90%; the deposition thickness is preferably 10 to 100nm, more preferably 50 to 80nm. The invention uses the transition layer as the connecting layer of the ceramic substrate and Cu, and the transition layer has good bonding force with the Cu layer.
After the transition layer is formed, the invention adopts the high-pulse low-energy ion beam equipment 105 to deposit the second surface on the transition layer to form a copper layer, and the ceramic-based copper-clad plate is obtained.
In the present invention, the target used for the second surface deposition is preferably a pure copper target; the arcing current of the second surface deposition is preferably 60-150A, more preferably 100A; the bias voltage is preferably 0 to 7kV and is not 0, more preferably 5kV; the frequency is preferably 0 to 200Hz and not 0, more preferably 20 to 100Hz; the deposition thickness is preferably 1 to 9. Mu.m, more preferably 3. Mu.m.
The invention can reduce the internal stress in the deposition process by using the high-pulse low-energy ion beam method on the basis of ensuring the compactness of the copper layer, thereby reducing the warpage and obtaining high reliability.
In the invention, the surface roughness of the ceramic-based copper-clad plate is preferably less than 0.2 mu m, and more preferably 0.11-0.19 mu m.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
S1: carrying out surface reduction on the surface of the aluminum nitride ceramic substrate by using a kofmann gas ion source, wherein the argon flow is 60sccm, the hydrogen flow is 30sccm, the voltage is 30kV, the beam intensity is 30mA, and the treatment time is 40min, so as to obtain a first treated ceramic substrate;
s2: ni element is injected on the surface of the first treated ceramic substrate by adopting a high-energy ion beam technology, bonding is carried out, the beam intensity is 20mA, the energy is 20keV, and the injection dosage is 1 multiplied by 10 16 ions/cm 2 Obtaining a second treated ceramic substrate;
s3, depositing a transition layer on the surface of the second treated ceramic substrate by using an NiCr (atomic mass ratio of 8:2) alloy as a target material and adopting a low-energy ion beam technology, wherein the transition layer is the NiCr (atomic mass ratio of 8:2) alloy, the arcing current is 100A, the bias voltage is 200V, the duty ratio is 90%, and the deposition thickness is 50nm;
s4: and (3) taking pure copper (99.95%) as a target material, depositing a copper layer on the surface of the transition layer by adopting a high-pulse low-energy ion beam technology, wherein the arcing current is 100A, the bias voltage is 5kV, the frequency is 100Hz, and the deposition thickness is 3 mu m, so that the ceramic-based copper-clad plate is obtained.
Example 2
S1: carrying out surface reduction on the surface of the aluminum nitride ceramic substrate by using a kofmann gas ion source, wherein the argon flow is 60sccm, the hydrogen flow is 30sccm, the voltage is 30kV, the beam intensity is 30mA, and the treatment time is 40min, so as to obtain a first treated ceramic substrate;
s2: ni element is injected on the surface of the first treated ceramic substrate by adopting a high-energy ion beam technology, bonding is carried out, the beam intensity is 20mA, the energy is 20keV, and the injection dosage is 1 multiplied by 10 15 ions/cm 2 Obtaining a second treated ceramic substrate;
s3, depositing a transition layer on the surface of the second treated ceramic substrate by using an NiCr (atomic mass ratio of 8:2) alloy as a target material and adopting a low-energy ion beam technology, wherein the transition layer is the NiCr (atomic mass ratio of 8:2) alloy, the arcing current is 100A, the bias voltage is 200V, the duty ratio is 90%, and the deposition thickness is 50nm;
s4: and (3) taking pure copper (99.95%) as a target material, depositing a copper layer on the surface of the transition layer by adopting a high-pulse low-energy ion beam technology, wherein the arcing current is 100A, the bias voltage is 5kV, the frequency is 20Hz, and the deposition thickness is 3 mu m, so that the ceramic-based copper-clad plate is obtained.
Example 3
S1: carrying out surface reduction on the surface of the aluminum nitride ceramic substrate by using a kofmann gas ion source, wherein the argon flow is 60sccm, the hydrogen flow is 30sccm, the voltage is 30kV, the beam intensity is 30mA, and the treatment time is 40min, so as to obtain a first treated ceramic substrate;
s2: al element is injected on the surface of the first treated ceramic substrate by adopting a high-energy ion beam technology, bonding is carried out, the beam intensity is 20mA, the energy is 20keV, and the injection dosage is 1 multiplied by 10 16 ions/cm 2 Obtaining a second treated ceramic substrate;
s3, depositing a transition layer on the surface of the second treated ceramic substrate by using an NiCr (atomic mass ratio of 8:2) alloy as a target material and adopting a low-energy ion beam technology, wherein the transition layer is the NiCr (atomic mass ratio of 8:2) alloy, the arcing current is 100A, the bias voltage is 200V, the duty ratio is 90%, and the deposition thickness is 80nm;
s4: and (3) taking pure copper (99.95%) as a target material, depositing a copper layer on the surface of the transition layer by adopting a high-pulse low-energy ion beam technology, wherein the arcing current is 100A, the bias voltage is 5kV, the frequency is 100Hz, and the deposition thickness is 3 mu m, so that the ceramic-based copper-clad plate is obtained.
Comparative example 1
S1: ni element is injected on the surface of the aluminum nitride ceramic substrate by adopting a high-energy ion beam technology, the beam intensity is 20mA, the energy is 20keV, and the injection dosage is 1 multiplied by 10 16 ions/cm 2 ；
S2, taking NiCr (atomic mass ratio is 8:2) alloy as a target material, adopting a low-energy ion beam technology to deposit a transition layer, wherein the transition layer is the NiCr (atomic mass ratio is 8:2) alloy, the arcing current is 100A, the bias voltage is 200V, the duty ratio is 90%, and the deposition thickness is 50nm;
s3: and (3) taking pure copper (99.95%) as a target material, adopting a high-pulse low-energy ion beam technology to deposit a copper layer, and obtaining the ceramic-based copper-clad plate, wherein the arcing current is 100A, the bias voltage is 5kV, the frequency is 100Hz and the deposition thickness is 3 mu m.
Comparative example 2
S1: carrying out surface reduction on the surface of the aluminum nitride ceramic substrate by using a kofmann gas ion source, wherein the argon flow is 60sccm, the hydrogen flow is 30sccm, the voltage is 30kV, the beam intensity is 30mA, and the treatment time is 40min, so as to obtain a first treated ceramic substrate;
s2, taking NiCr (atomic mass ratio is 8:2) alloy as a target material, adopting a low-energy ion beam technology to deposit a transition layer on the surface of the first treated ceramic substrate, wherein the transition layer is the NiCr (atomic mass ratio is 8:2) alloy, the arcing current is 100A, the bias voltage is 200V, the duty ratio is 90%, and the deposition thickness is 50nm;
s3: and (3) taking pure copper (99.95%) as a target material, depositing a copper layer on the surface of the transition layer by adopting a high-pulse low-energy ion beam technology, wherein the arcing current is 100A, the bias voltage is 5kV, the frequency is 20Hz, and the deposition thickness is 3 mu m, so that the ceramic-based copper-clad plate is obtained.
Comparative example 3
S1: carrying out surface reduction on the aluminum nitride ceramic surface by using a koufman gas ion source, wherein the argon is 60sccm, the hydrogen is 30sccm, the voltage is 30kV, the beam intensity is 30mA, and the treatment time is 40min, so that a first treated ceramic substrate is obtained;
s2: ni element is injected on the surface of the first processed ceramic substrate by adopting a high-energy ion beam technology, bonding is carried out, the beam intensity is 20mA, the energy is 20keV, and the injection dosage is 1 x 10 16 ions/cm 2 Obtaining a second treated ceramic substrate;
s3, depositing a transition layer on the surface of the second treated ceramic substrate by using an NiCr (atomic mass ratio of 8:2) alloy as a target material and adopting a low-energy ion beam technology, wherein the transition layer is the NiCr (atomic mass ratio of 8:2) alloy, the arcing current is 100A, the bias voltage is 200V, the duty ratio is 90%, and the deposition thickness is 50nm;
s4: and (3) taking pure copper (99.95%) as a target material, depositing a copper layer on the surface of the transition layer by adopting a high-pulse low-energy ion beam technology, wherein the arcing current is 100A, the bias voltage is 0kV, the frequency is 0Hz, and the deposition thickness is 3 mu m, so that the ceramic-based copper-clad plate is obtained.
Characterization and performance testing
1) The ceramic-based copper-clad plate prepared in example 1 was subjected to surface topography test, and the obtained results are shown in fig. 3; as can be seen from fig. 3, the prepared copper-clad layer has low surface roughness and few defects.
2) The ceramic-based copper clad laminate surfaces prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to roughness test (Ra) using a roughness profiler by stylus method, and the obtained results are shown in fig. 4; from the test data of examples 1-3 and comparative examples 1-3 in fig. 4, it is clear that the high pulse low energy ion beam technique can effectively reduce the roughness of the coating, and the higher the frequency, the greater the roughness.
3) The ceramic-based copper clad laminates prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to a bonding force test by using a tensile peeling test, copper wires with widths of 5mm were etched from different ceramic-based copper clad laminates, and then the average force of the copper wires when peeled from the ceramic substrate was recorded by using a peeling strength machine, and the obtained results are shown in fig. 5; from the test data of the binding forces of examples 1 to 3 and comparative examples 1 to 3 in fig. 5, the kaufman ion source treatment can effectively improve the binding force between the substrate and the copper layer, while the high-energy ion beam treatment is the key to improve the binding force. The implantation dosage and the implantation element also affect the binding force, the binding force is increased along with the increase of the implantation dosage, and the implantation of Ni element is obviously superior to the implantation of Al element.
4) The ceramic-based copper clad laminates prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to compactness test by using a two-dimensional measuring instrument, and the number of pinholes smaller than 0.1mm was marked on any 250mmx250mm area, and the obtained results are shown in table 1.
Table 1 number of pinholes of less than 0.1mm over any 250mmx250mm area
Figure BDA0004030601080000081
Figure BDA0004030601080000091
From the test data of examples 1 to 3 and comparative examples 1 to 3 in table 1, it is understood that the pulse frequency in the high pulse low energy ion beam technique affects the compactness of the copper layer, and the higher the frequency, the better the compactness.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (10)

1. The device for preparing the ceramic-based copper-clad plate is characterized by comprising a vacuum chamber (101), a kaufman gas ion source device (102), a high-energy ion beam device (103), a low-energy ion beam device (104) and a high-pulse low-energy ion beam device (105); the kofuman ion source device (102), the high-energy ion beam device (103), the low-energy ion beam device (104) and the high-pulse low-energy ion beam device (105) are respectively distributed at four ends of the vacuum chamber 101.
2. The apparatus of claim 1, further comprising a workpiece tray (106); the workpiece tray (106) is disposed in the vacuum chamber (101).
3. The method for preparing the ceramic-based copper-clad plate by using the device for preparing the ceramic-based copper-clad plate according to claim 1 or 2, which is characterized by comprising the following steps:
adopting a kaufman gas ion source device (102) to perform surface reduction on a ceramic substrate arranged in a vacuum chamber (101) to obtain a first processed ceramic substrate;
injecting metal into the surface of the first treated ceramic substrate by adopting high-energy ion beam equipment (103) to carry out bonding so as to obtain a second treated ceramic substrate;
performing first surface deposition on the second processed ceramic substrate by using low-energy ion beam equipment (104) to form a transition layer;
and (3) adopting high-pulse low-energy ion beam equipment (105) to deposit a second surface on the transition layer to form a copper layer, and obtaining the ceramic-based copper-clad plate.
4. A method according to claim 3, wherein the flow rate of the argon gas for surface reduction is 20-80 sccm, the flow rate of the hydrogen gas is 0-40 sccm, the voltage is 20-40 KV, the beam intensity is 1-50 mA, and the treatment time is 20-60 min.
5. The method according to claim 3, wherein the ceramic substrate has a surface roughness change of 0.1 μm or less after the surface reduction is performed.
6. A method according to claim 3, wherein the metal element used for the injection of the metal comprises Ti, al, ni, cr or Cu.
7. A method according to claim 3, wherein the beam intensity of the bond is 10-100 mA, the energy is 10-40 keV, and the implantation dose is 1× (10 15 ～10 17 )ions/cm 2 。
8. A method according to claim 3, wherein the elements of the transition layer are Ni and/or Cr, the first surface is deposited with an arc current of 60-150A, a bias voltage of 0-300V, a duty cycle of 20-95% and a deposition thickness of 10-100 nm.
9. A method according to claim 3, wherein the second surface is deposited with an arc current of 60 to 150A, a bias voltage of 0 to 7kV and not 0, a frequency of 0 to 200Hz and not 0, and a deposition thickness of 1 to 9 μm.
10. A method according to claim 3, wherein the ceramic-based copper clad laminate has a surface roughness of < 0.2 μm.
CN202211727318.0A 2022-12-30 2022-12-30 Device and method for preparing ceramic-based copper-clad plate Pending CN116121696A (en)

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