CN112738988A - Ceramic copper-clad plate, preparation method thereof and ceramic circuit board - Google Patents
Ceramic copper-clad plate, preparation method thereof and ceramic circuit board Download PDFInfo
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- CN112738988A CN112738988A CN202011645344.XA CN202011645344A CN112738988A CN 112738988 A CN112738988 A CN 112738988A CN 202011645344 A CN202011645344 A CN 202011645344A CN 112738988 A CN112738988 A CN 112738988A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 145
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000010949 copper Substances 0.000 claims abstract description 288
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 278
- 229910052802 copper Inorganic materials 0.000 claims abstract description 276
- 239000013078 crystal Substances 0.000 claims abstract description 98
- 239000000758 substrate Substances 0.000 claims abstract description 56
- 238000000137 annealing Methods 0.000 claims abstract description 40
- 238000009713 electroplating Methods 0.000 claims description 16
- 229910000679 solder Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000008719 thickening Effects 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 139
- 238000000034 method Methods 0.000 description 10
- 238000005336 cracking Methods 0.000 description 9
- 238000005219 brazing Methods 0.000 description 8
- 239000000945 filler Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 230000008646 thermal stress Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0306—Inorganic insulating substrates, e.g. ceramic, glass
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/022—Processes for manufacturing precursors of printed circuits, i.e. copper-clad substrates
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/06—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed chemically or electrolytically, e.g. by photo-etch process
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
A ceramic copper-clad plate, a preparation method thereof and a ceramic circuit board belong to the technical field of copper-clad plates. At least one side of the ceramic substrate is provided with a conductive copper plate, and the conductive copper plate comprises a single crystal domain copper layer; the single crystal domain copper layer has no crystal boundary, and still has high single crystal orientation and high conductivity after being thickened by electroplated copper and treated by secondary annealing. The ceramic copper-clad plate is formed by directly bonding the ceramic substrate and the conductive copper plate at high temperature, so that the problems of cracks and warping and peeling of the conductive copper layer of the ceramic circuit board can be obviously solved, the conductive performance and reliability are improved, and the performance requirements in the fields of high-current power modules, power electronic components and the like are better met.
Description
Technical Field
The application relates to the technical field of copper-clad plates, in particular to a ceramic copper-clad plate, a preparation method thereof and a ceramic circuit board.
Background
Compared with an organic copper-clad plate, the ceramic copper-clad plate material has better heat-resistant stability, dimensional stability and heat dissipation capability. In the prior art, a ceramic substrate and a conductive copper plate are directly bonded into a ceramic copper-clad plate at high temperature, in the high-temperature bonding process, the temperature is conducted to the ceramic copper-clad plate, and the thermal expansion difference (copper 17 multiplied by 10) between the copper and the ceramic is added-6K, 3-8 x 10 of ceramic-6and/K) is large, thermal stress is generated on the interface of the ceramic copper-clad plate, and the reliability problem of crack and warping peeling of the copper layer is aggravated.
Disclosure of Invention
The application provides a ceramic copper-clad plate, a preparation method thereof and a ceramic circuit board, which can solve the problems of cracking, warping and peeling of copper layers in the ceramic copper-clad plate and the ceramic circuit board.
The embodiment of the application is realized as follows:
in a first aspect, an embodiment of the present application provides a ceramic copper-clad plate, including: the ceramic substrate and the conductive copper plate are arranged in a laminated manner, and the conductive copper plate is arranged on at least one side of the ceramic substrate; the conductive copper plate comprises a single crystal domain copper layer; the single crystal domain copper layer is arranged close to the surface of the ceramic substrate.
In a second aspect, an embodiment of the present application provides a method for preparing a ceramic copper-clad plate in an embodiment of the first aspect, including:
and directly bonding the ceramic substrate and the conductive copper plate under the heating condition.
In a third aspect, an embodiment of the present application provides a ceramic circuit board, which is obtained by etching the ceramic copper-clad plate of the embodiment of the first aspect through a line.
The ceramic copper-clad plate, the preparation method thereof and the ceramic circuit board have the beneficial effects that:
the applicant researches and discovers that the crystal grain size of the copper plate is small, the number of crystal boundaries is large, the dislocation of the thermal stress to the copper layer of the ceramic copper-clad plate can not be inhibited, and the problems of crack, warping and stripping reliability of the copper layer can be aggravated; therefore, the ceramic copper-clad plate in the embodiment of the application adopts the conductive copper plate with the single crystal domain copper layer, the copper in the single crystal domain copper layer is the single crystal domain copper, the single crystal domain copper does not have a crystal boundary, the problems of copper layer cracks and easy warping and stripping of the ceramic circuit board can be obviously improved, the conductive performance and the reliability are improved, and the performance requirements in the fields of high-current power modules, power electronic components and the like are better met.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a schematic structural diagram of a first ceramic copper-clad plate according to an embodiment of the present application;
FIG. 2 is a schematic structural diagram of a second ceramic copper-clad plate according to an embodiment of the present application;
FIG. 3 is a schematic structural diagram of a third ceramic copper-clad plate according to an embodiment of the present application;
FIG. 4 is a schematic structural diagram of a fourth ceramic copper-clad plate according to an embodiment of the present application;
FIG. 5 is an electron microscope photograph of a single crystal domain copper layer of example 1 of the present application;
fig. 6 is an electron microscope photograph of the polycrystalline copper plate of example 1 of the present application.
Icon: 10-a ceramic copper-clad plate; 11-a ceramic substrate; 12-a conductive copper plate; 121-single crystal domain copper layer; 122-annealing the electroplated copper layer; 13-solder layer.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The ceramic copper clad laminate generally comprises a ceramic substrate and a conductive copper plate, wherein the ceramic copper clad laminate is easy to generate thermal stress due to high temperature in the preparation process, in addition, the ceramic copper clad laminate is repeatedly electrified and powered off to generate heating and cooling heat to be conducted to the ceramic copper clad laminate in the use process, in addition, the thermal expansion difference between copper and ceramic is large, and the thermal stress is repeatedly generated on the interface of the ceramic copper clad laminate.
Based on this, the embodiment of the application provides a ceramic copper-clad plate 10, a preparation method thereof and a ceramic circuit board, so as to solve the problems of cracks and warping and peeling of copper layers in the ceramic copper-clad plate 10 and the ceramic circuit board.
The following description specifically explains the ceramic copper-clad plate 10, the preparation method thereof, and the ceramic circuit board according to the embodiment of the present application:
in a first aspect, an embodiment of the present application provides a ceramic copper-clad plate 10, please refer to fig. 1 to 4, which includes: the conductive copper plate 12 is arranged on at least one side of the ceramic substrate 11, the conductive copper plate 12 comprises a single crystal domain copper layer 121, and the single crystal domain copper layer 121 is arranged close to the surface of the ceramic substrate 11.
The conductive copper plate 12 may be provided on one side of the ceramic substrate 11 (see fig. 1 and 3), or the conductive copper plate 12 may be provided on both opposite sides of the ceramic substrate 11 (see fig. 2 and 4). When the conductive copper plate 12 is provided on at least one side of the ceramic substrate 11, the single crystal domain copper layer 121 of the conductive copper plate 12 may be in direct contact with the surface of the ceramic substrate 11, or other functional layers may be provided on the ceramic substrate 11 and the conductive copper plate 12.
In the embodiment of the application, the conductive copper plate 12 with the single crystal domain copper layer 121 is adopted, the copper in the single crystal domain copper layer 121 is the single crystal domain copper, and no crystal boundary exists, so that the problems of cracking and warping peeling of the copper layer in the ceramic copper-clad plate 10 can be obviously solved, and the conductivity of the ceramic copper-clad plate 10 can be improved.
In a possible embodiment, the size of the single crystal domain copper layer 121 is more than or equal to 200 x 200mm, and the grain size is larger, so that the probability of cracking and warping peeling of the copper layer in the ceramic copper-clad plate 10 can be better reduced. Optionally, the single-crystal domain size of the single-crystal domain copper layer 121 is 200 × 200mm to 400 × 400mm, such as 200 × 200mm, 210 × 230mm, 220 × 250mm, 250 × 250mm, 300 × 250mm, 280 × 280mm, 300 × 300mm, 350 × 280mm, 330 × 330mm, 350 × 300mm, 350 × 350mm, 350 × 380mm, 350 × 400mm, and 400 × 400 mm.
Illustratively, the single-crystal-domain copper layer 121 is obtained by annealing a polycrystalline copper plate. Polycrystalline copper is contained in the polycrystalline copper plate, the grain size of the polycrystalline copper becomes large after annealing treatment, the grain boundaries contained in the copper plate of the same area become small, and the copper plate may contain only one single crystal. Optionally, after the annealing treatment of the polycrystalline copper plate, the polycrystalline copper plate can be cut to retain large-size crystal-boundary-free single crystal copper, and the rest part of the polycrystalline copper plate is cut off, so that the single crystal copper with only one crystal domain is ensured to be contained in the single crystal domain copper layer 121, and the problems of cracking and warping peeling of the copper layer in the ceramic copper-clad plate 10 are obviously solved.
Alternatively, the conductive copper plate 12 includes an annealed electroplated copper layer 122 in addition to the single-crystal-domain copper layer 121. When the polycrystalline copper plate is thick, the annealing process for increasing the grain size and eliminating the copper grain boundary has great difficulty, and the difficulty for eliminating the reliability risk is greater. Under the condition that the thickness of the conductive copper plate 12 is the same, compared with the scheme that the conductive copper plate 12 only comprises the single crystal domain copper layer 121, the conductive copper plate 12 comprises the single crystal domain copper layer 121 and the annealing copper electroplating layer 122, the difficulty of obtaining the single crystal domain copper layer 121 can be reduced, in addition, the copper electroplating layer can also enlarge copper crystal grains after annealing, and the problems of cracking and warping and stripping of the copper layer in the ceramic copper clad plate 10 can also be obviously improved.
Illustratively, the thickness of the single crystal domain copper layer 121 is 25-75 um. The single crystal domain copper layer 121 with the thickness of 25-75 um is relatively easily obtained by annealing a polycrystalline copper plate due to the relatively thin thickness. Optionally, the thickness of the single-domain copper layer 121 is any one of 25um, 30um, 35um, 40um, 45um, 50um, 55um, 60um, 65um, 70um, and 75um or a range between any two.
Further, the thickness of the conductive copper plate 12 is preferably 100 to 600 um. When the thickness of the conductive copper plate 12 is 100 to 600um, since the thickness is thick, if the conductive copper plate 12 only contains the single crystal domain copper layer 121, it is very difficult to obtain the single crystal domain copper layer 121 with the thickness due to the annealing difficulty. The conductive copper plate 12 with the thickness of 100-600 um comprises a single crystal domain copper layer 121 and an annealing copper electroplating layer 122, so that the annealing difficulty is reduced, the annealing copper electroplating layer 122 is obtained after the annealing of the copper electroplating layer, copper crystal grains can be enlarged in the annealing process, and the conductive copper plate 12 containing the single crystal domain copper layer 121 and the annealing copper electroplating layer 122 can also remarkably improve the problems of cracking and warping and peeling of the copper layer in the ceramic copper clad plate 10.
Optionally, the ceramic substrate 11 comprises Al2O3、AlN、Si3N4BeO, SiC and BN.
Illustratively, the copper lattice of the conductive copper plate 12 is oriented to any one of Cu (111), Cu (110), Cu (211), and Cu (100). It is understood that, when the conductive copper plate 12 includes the single-crystal-domain copper layer 121 and the annealed copper plating layer 122, the lattice orientation of copper in the single-crystal-domain copper layer 121 and the annealed copper plating layer 122 is any one of Cu (111), Cu (110), Cu (211), and Cu (100). The crystal lattices of the copper in the single-crystal-domain copper layer 121 and the annealed copper plating layer 122 are preferably in the same crystal lattice orientation.
The applicant researches and finds that the copper lattice orientations can relieve lattice dislocation of the conductive copper plate 12 layer caused by thermal stress, so that the probability of cracks and warping of the copper layer in the ceramic copper-clad plate 10 is reduced.
Further, in a possible embodiment, a solder layer 13 is further provided between the ceramic substrate 11 and the conductive copper plate 12 (refer to fig. 3 and 4). Compared with the scheme that the conductive copper plate 12 is formed on the surface of the ceramic substrate 11, the brazing filler metal layer 13 is further arranged between the ceramic substrate 11 and the conductive copper plate 12, and the brazing filler metal layer 13 can reduce the direct bonding temperature, so that the generation of high-temperature thermal stress is further reduced. In addition, the existence of the solder layer 13 can reduce the problem of thermal stress caused by the overlarge difference of the thermal expansion coefficients between the ceramic substrate 11 and the conductive copper plate 12, thereby improving the thermal stability of the ceramic copper-clad plate 10. Illustratively, the solder in the solder layer 13 comprises at least one of silver, copper and titanium, and the electronic paste made of the solder is coated on one side or two side surfaces of the ceramic substrate 11, dried and then made into the ceramic copper clad laminate 10 with the conductive copper plate 12 at a high temperature in vacuum.
In a second aspect, an embodiment of the present application provides a method for preparing a ceramic copper-clad plate 10, including: the ceramic substrate 11 and the conductive copper plate 12 are directly bonded under heating.
The ceramic copper clad laminate 10 obtained by bonding the ceramic substrate 11 and the conductive copper plate 12 under the heating condition has the advantages that the conductive copper plate 12 comprises the single crystal domain copper layer 121, the copper in the single crystal domain copper layer 121 is single crystal domain copper, and each single crystal domain has no crystal boundary, so that the problems of cracking and warping and stripping of the copper layer in the ceramic copper clad laminate 10 can be obviously improved, and the conductivity of the ceramic copper clad laminate 10 can be improved. The heating temperature during bonding is, for example, 1050 to 1100 ℃, for example, 1050 ℃, 1060 ℃, 1070 ℃, 1080 ℃, 1090 ℃, and 1100 ℃, or a range between any two of them.
In one possible embodiment, the process for manufacturing the conductive copper plate 12 comprises: and annealing the polycrystalline copper plate for the first time to obtain a single crystal domain copper layer 121, electroplating the single crystal domain copper layer 121 to thicken, forming an electroplated copper layer on the surface of the single crystal domain copper layer 121, and annealing for the second time to obtain the conductive copper plate 12.
After annealing, the polycrystalline copper plate has larger copper grain size and less crystal boundary, and finally, the copper plate only contains one copper single crystal. The electroplated copper layer is formed on the surface of the single crystal domain copper layer 121 in an electroplating thickening mode, secondary annealing is carried out, the grain size of the single crystal domain copper layer 121 is further increased, copper grains are increased after the electroplated copper layer is annealed, the grain sizes of the single crystal domain copper layer 121 and the annealed electroplated copper layer 122 are increased, the single crystal domain copper layer 121 has no crystal boundary, the problems of cracking and warping stripping of the copper layer in the ceramic copper-clad plate 10 can be obviously improved, and meanwhile, the annealing difficulty of the single crystal domain copper layer 121 is also reduced.
Illustratively, the current density of the electroplating process is 0.3-4 ASD. In the process of electroplating thickening, if the current density is too large, thickening is easy to be uneven, if the current density is too small, copper can not be plated successfully, and the current density is selected to be 0.3-4ASD, so that the surface of the single crystal domain copper layer 121 can be relatively uniformly formed into an electroplated copper layer.
In addition, the temperature range of the first annealing is 800-1075 ℃, such as 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃ and 1075 ℃ or the range between any two. Optionally, the time of the first annealing is in a range of 1 to 4 hours, such as 1 hour, 2 hours, 3 hours, or 4 hours.
Illustratively, the temperature range of the second annealing is 500-1075 ℃, such as 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ and 1075 ℃ or any range between any two. The annealing difficulty of the annealed electroplated copper layer 122 is less than that of the single-crystal-domain copper layer 121, and thus, the second annealing temperature may be less than the first annealing temperature. Optionally, the second annealing time is 1-2 h.
Further, when the ceramic copper clad laminate 10 includes the solder layer 13, the electronic slurry made of the solder is coated on one side or both sides of the ceramic substrate 11 to form the solder layer 13, and after drying, the conductive copper plate 12 is bonded with the ceramic substrate 11 having the solder layer 13 on the surface under the heating condition.
In a third aspect, an embodiment of the present application further provides a ceramic circuit board, which is obtained by etching the ceramic copper-clad plate 10 of the first aspect through a line.
The ceramic copper-clad plate 10 is etched through a circuit, part of the conductive copper plate 12 is removed, a conductive copper wire is formed on the surface of the ceramic substrate 11, and the problems of cracking, warping and peeling of the copper layer in the ceramic circuit board can be obviously improved due to the fact that a single crystal domain copper layer 121 of the conductive copper wire does not have a crystal boundary.
The ceramic copper clad laminate 10, the preparation method thereof and the ceramic circuit board of the present application are further described in detail with reference to the following embodiments.
Example 1
The embodiment provides a ceramic copper-clad plate, it includes ceramic substrate and the electrically conductive copper board of range upon range of setting, and one side of ceramic substrate sets up the electrically conductive copper layer, and its preparation technology includes:
carrying out first annealing on a polycrystalline copper plate with the thickness of 50 mu m at 1050 ℃ to obtain a single crystal domain copper layer, electroplating the single crystal domain copper layer to thicken, forming an electroplated copper layer with the thickness of 200 mu m on the surface of the single crystal domain copper layer, and then carrying out second annealing at 700 ℃ to obtain the conductive copper plate with the single crystal domain copper layer and the annealed electroplated copper layer.
And bonding the conductive copper plate and the ceramic substrate with the thickness of 200um at the temperature of 1050 ℃ so that the single crystal domain copper layer is in contact with the ceramic substrate.
Example 2
The embodiment provides a ceramic copper-clad plate, its ceramic substrate and the electrically conductive copper board including range upon range of setting, and ceramic substrate's both sides all set up electrically conductive copper layer, and its preparation technology includes:
the method comprises the steps of annealing a polycrystalline copper plate with the thickness of 75 microns for the first time at the temperature of 1000 ℃ to obtain a single crystal domain copper layer, electroplating the single crystal domain copper layer for thickening, forming an electroplated copper layer with the thickness of 400 microns on the surface of the single crystal domain copper layer 121, and annealing for the second time at the temperature of 800 ℃ to obtain the conductive copper plate with the single crystal domain copper layer and the annealed electroplated copper layer.
And bonding the conductive copper plate and the ceramic substrate with the thickness of 400 mu m at the temperature of 1050 ℃ so that the single crystal domain copper layer is in contact with the ceramic substrate.
Example 3
The embodiment provides a ceramic copper-clad plate, it is including ceramic substrate and the electrically conductive copper board of range upon range of setting, and one side of ceramic substrate sets up the electrically conductive copper layer, sets up the brazing filler metal layer between ceramic substrate and the electrically conductive copper board, and its preparation technology includes:
carrying out first annealing on a polycrystalline copper plate with the thickness of 50 mu m at 1050 ℃ to obtain a single crystal domain copper layer, electroplating the single crystal domain copper layer to thicken, forming an electroplated copper layer with the thickness of 200 mu m on the surface of the single crystal domain copper layer, and then carrying out second annealing at 700 ℃ to obtain the conductive copper plate with the single crystal domain copper layer and the annealed electroplated copper layer.
Brazing the silver-containing brazing filler metal on the surface of one side of a ceramic substrate with the thickness of 200 mu m to form a brazing filler metal layer, and then bonding the ceramic substrate with the brazing filler metal layer and a conductive copper plate at the temperature of 1050 ℃ to enable a single crystal domain copper layer to be in contact with the brazing filler metal layer.
Example 4
The embodiment provides a ceramic copper-clad plate, it includes ceramic substrate and the electrically conductive copper board of range upon range of setting, and one side of ceramic substrate sets up the electrically conductive copper layer, and its preparation technology includes:
and annealing the polycrystalline copper plate with the thickness of 75 mu m at 1000 ℃ to obtain a single crystal domain copper layer, electroplating the single crystal domain copper layer to thicken, and forming an electroplated copper layer with the thickness of 400 mu m on the surface of the single crystal domain copper layer to obtain the conductive copper plate.
And bonding the conductive copper plate and the ceramic substrate with the thickness of 400 mu m at the temperature of 1050 ℃ so that the single crystal domain copper layer is in contact with the ceramic substrate.
Example 5
The embodiment provides a ceramic copper-clad plate, it includes ceramic substrate and the electrically conductive copper board of range upon range of setting, and one side of ceramic substrate sets up the electrically conductive copper layer, and its preparation technology includes:
carrying out first annealing on a polycrystalline copper plate with the thickness of 20 mu m at 1050 ℃ to obtain a single crystal domain copper layer, electroplating the single crystal domain copper layer to thicken, forming an electroplated copper layer with the thickness of 200 mu m on the surface of the single crystal domain copper layer, and then carrying out second annealing at 700 ℃ to obtain the conductive copper plate with the single crystal domain copper layer and the annealed electroplated copper layer.
And bonding the conductive copper plate and the ceramic substrate with the thickness of 200um at the temperature of 1050 ℃ so that the single crystal domain copper layer is in contact with the ceramic substrate.
Comparative example 1
This comparative example provides a pottery copper-clad plate, and it sets up ceramic substrate and electrically conductive copper board including range upon range of, and one side of ceramic substrate sets up electrically conductive copper layer, and its preparation technology includes:
and bonding the polycrystalline copper plate with the thickness of 250um and the ceramic substrate with the thickness of 200um at the temperature of 1050 ℃.
Test example 1
The single-crystal domain copper layers obtained in examples 1 and 2 and the polycrystalline copper layers obtained in examples 1 and 2 were subjected to property testing, and the results are shown in table 1, and the testing methods are as follows:
(1) detecting the number of crystal boundaries: and observing by a metallographic microscope, and randomly taking the number of the grain boundaries within the range of 250 x 400 mm.
(2) Hardness: GB-T4340.1-2009.
(3) Conductivity: GB-T351-2009.
(4) And (3) detecting the purity and the oxygen content of copper: GB/T5121.1-2008.
TABLE 1 Performance test results of Single-Domain copper layers and polycrystalline copper plates
As can be seen from the results in table 1, the single-crystal domain copper layer of the examples of the present application has higher conductivity and better conductivity than the polycrystalline copper layer.
Test example 2
The single-crystal domain copper layer and the polycrystalline copper layer of example 1 were observed under an electron microscope, and the observed photographs are shown in fig. 5 and 6.
Test example 3
The reliability performance of the ceramic copper clad laminates prepared in the embodiments 1 to 5 and the comparative example 1 is tested, and the test method comprises the following steps: 5 samples are prepared for each sample, the samples are alternately put into a mixed refrigerant of ethanol and dry ice at the temperature of minus 65 ℃ and a high-temperature oil bath at the temperature of 150 ℃, the circulation is set as 1 cycle according to the 5min maintenance, and after 500 cycles of repeated operation, whether the ceramic copper clad laminate of each sample has cracks or warping height or not, and whether the conductive copper plate has peeling or delamination foaming problems from the ceramic substrate or not are confirmed. The test results are reported in table 2.
TABLE 2 reliability Performance test results
As can be seen from the results in table 2, only the ceramic copper clad laminates of examples 4 among the ceramic copper clad laminates of examples 1 to 5 of the present application exhibited cracks and peeling blisters, but the occurrence rates of cracks and peeling blisters were also lower than those of comparative example 1. The ceramic copper-clad plates prepared in the embodiments 1-5 can improve the problems of cracks and warping and peeling of the copper layer. Comparing example 4 with example 1, example 4 has higher probability of crack and peeling blister than example 1 without annealing after forming the electroplated copper layer on the surface of the single crystal domain copper layer, and illustrates that the conductive copper plate including the annealed electroplated copper layer can better improve the problem of crack and warpage peeling of the copper layer.
The foregoing is illustrative of the present application and is not to be construed as limiting thereof, as numerous modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. The ceramic copper-clad plate is characterized by comprising: the conductive copper plate is arranged on at least one side of the ceramic substrate and comprises a single crystal domain copper layer, and the single crystal domain copper layer is arranged close to the surface of the ceramic substrate.
2. The ceramic copper-clad plate according to claim 1, wherein the size of the single crystal domain copper layer is not less than 200 x 200 mm.
3. The ceramic copper-clad plate according to claim 1, wherein the conductive copper plate further comprises an annealed electroplated copper layer.
4. The ceramic copper-clad plate according to claim 3, wherein the thickness of the single-crystal domain copper layer is 25-75 um.
5. The ceramic copper-clad plate according to claim 4, wherein the thickness of the conductive copper plate is 100-600 um.
6. The ceramic copper-clad plate according to any one of claims 1 to 4, wherein the copper lattice orientation of the conductive copper plate is any one of Cu (111), Cu (110), Cu (211) and Cu (100).
7. The ceramic copper-clad plate according to any one of claims 1 to 4, wherein a solder layer is further disposed between the ceramic substrate and the conductive copper plate; optionally, the braze in the braze layer includes at least one of silver, copper, and titanium.
8. The preparation method of the ceramic copper-clad plate according to claim 1 or 2, which comprises the following steps:
and directly bonding the ceramic substrate and the conductive copper plate under the heating condition.
9. The preparation method of the ceramic copper-clad plate according to claim 8, wherein the manufacturing process of the conductive copper plate comprises the following steps:
carrying out first annealing on the polycrystalline copper plate to obtain a single crystal domain copper layer, electroplating and thickening the single crystal domain copper layer to form an electroplated copper layer on the surface of the single crystal domain copper layer, and then carrying out second annealing to obtain the conductive copper plate.
10. A ceramic circuit board is characterized in that the ceramic circuit board is obtained by etching the ceramic copper-clad plate of any one of claims 1 to 6 through a circuit.
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