CN114874030B - Preparation method for improving insulation reliability of copper-clad ceramic substrate - Google Patents

Preparation method for improving insulation reliability of copper-clad ceramic substrate Download PDF

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CN114874030B
CN114874030B CN202210327811.7A CN202210327811A CN114874030B CN 114874030 B CN114874030 B CN 114874030B CN 202210327811 A CN202210327811 A CN 202210327811A CN 114874030 B CN114874030 B CN 114874030B
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ceramic substrate
copper
preparation
aluminum
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CN114874030A (en
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欧阳鹏
贺贤汉
王斌
高远
蹇满
张进
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Jiangsu Fulehua Power Semiconductor Research Institute Co ltd
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    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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    • C04B41/5155—Aluminium
    • 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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    • C23F1/00—Etching metallic material by chemical means
    • C23F1/02—Local etching
    • 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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    • C23F1/18—Acidic compositions for etching copper or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • 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
    • H05K1/05—Insulated conductive substrates, e.g. insulated metal substrate
    • H05K1/053—Insulated conductive substrates, e.g. insulated metal substrate the metal substrate being covered by an inorganic insulating layer
    • 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
    • H05K3/0011—Working of insulating substrates or insulating layers
    • 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

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Abstract

The invention discloses a preparation method for improving the insulation reliability of a copper-clad ceramic substrate, which comprises the following steps: the method comprises the following steps: forming an aluminum metallization layer on the surface of the ceramic substrate; step two: carrying out pattern etching and anodic oxidation on the aluminum metallization layer; step three: and brazing and sintering the active metal, attaching a copper foil, and etching the pattern to obtain the copper-clad ceramic substrate. In order to avoid the situations of local high voltage and unstable local discharge amount on the surface of the copper-clad ceramic substrate, the insulating aluminum anodic oxidation layer with high-strength bonding is introduced into the copper-ceramic junction surface, so that the insulating reliability of the product is improved, the graphic characteristics of the insulating anodic oxidation layer can be customized according to the product characteristics, and the insulating reliability of the product under the local high-voltage condition is further improved.

Description

Preparation method for improving insulation reliability of copper-clad ceramic substrate
Technical Field
The invention relates to the technical field of semiconductors, in particular to a preparation method for improving the insulation reliability of a copper-clad ceramic substrate.
Background
An IGBT power electronic device is a core component in the field of industrial control and automation, has the action similar to human hearts, and can adjust voltage, current, frequency, phase and the like in a circuit according to signal instructions in an industrial device so as to achieve the aim of precise regulation and control. The copper-clad ceramic substrate is used as a packaging substrate of the IGBT device and has the functions of current carrying, insulation, support, heat dissipation and the like. Compared with other power devices, the IGBT has outstanding product competitiveness in terms of high voltage, large current, and high speed, and the copper-clad ceramic substrate is also required to have higher insulation reliability.
The partial discharge performance is an important index for representing the insulation reliability of the copper-clad ceramic substrate. The complicated power conversion of power electronic device during operation can lead to the copper-clad ceramic substrate surface to appear local high pressure and the unstable condition of local discharge capacity, and under extreme condition, the continuous discharge will cause the copper-clad ceramic substrate to insulate to lose efficacy to cause the device to lose efficacy. How to improve and optimize the insulation reliability problem of the copper-clad ceramic substrate caused under the condition of high voltage or local high voltage is a difficult problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method for improving the insulation reliability of a copper-clad ceramic substrate, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a patent name.
A preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing an aluminum metallization layer on the surface of the ceramic substrate by sequentially performing screen printing and high-temperature infiltration sintering on the pure aluminum slurry for later use;
s2: presetting a graph A, taking the ceramic substrate in the step S1, etching the graph of the aluminum metallization layer to form the graph A, and carrying out anodic oxidation on the graph A on the surface of the aluminum metallization layer to form an anodic oxidation layer;
s3: and (3) coating active metal brazing filler metal on the two side surfaces of the ceramic substrate prepared in the step (S2), attaching copper foils to the two sides of the ceramic substrate, performing vacuum sintering, performing contraposition exposure, etching circuit patterns on the surfaces of the copper foils, and cutting to obtain the copper-clad ceramic substrate.
In a further optimized scheme, the method for anodizing the aluminum metallization layer comprises the following steps: placing a ceramic substrate with an aluminum metallization layer on the surface as an anode and a graphite plate as a cathode in a sulfuric acid aqueous solution at a current density of 2.5-4.5A/dm 2 And carrying out oxidation reaction.
In a further optimized scheme, the concentration of the sulfuric acid aqueous solution is 90-130g/L, the oxidation reaction temperature is 0-3 ℃, and the oxidation reaction time is 60-150min.
In the step S1, the preparation method of the pure aluminum slurry comprises the steps of mixing pure aluminum powder and an organic carrier, stirring and reacting for 10-15min, and grinding and running in to obtain the pure aluminum slurry, wherein the mass ratio of the pure aluminum powder to the organic carrier is (3-4): 1.
According to a further optimized scheme, the pure aluminum powder is spherical aluminum powder with the particle size of 1-10 microns; the materials required for the organic vehicle include, by weight: 5-10% of stearic acid, 6-12% of ethyl cellulose, 3-6% of diisononyl phthalate, 5-10% of lauryl alcohol ester and the balance of isopropanol.
In the step S1, the high-temperature wettability sintering temperature is 850-1200 ℃, and the sintering time is 10-120min.
In the step S3, the vacuum sintering temperature is 850-950 ℃, the temperature is kept for 60min, and the pressure is 0.2-0.6N/cm 2 And (5) cooling along with the furnace.
In a further optimized scheme, in the step S1, the thickness of the aluminum metalized layer is 20-100 μm; in step S3, the thickness of the copper foil is 0.2-0.8mm.
According to a further optimized scheme, the thickness of the ceramic substrate is 0.25-1.0mm; the ceramic substrate is one or more of an aluminum nitride ceramic substrate, an aluminum oxide ceramic substrate and a silicon nitride ceramic substrate.
The method comprises the steps of preparing pure aluminum slurry, printing and coating the pure aluminum slurry on the surface of the ceramic, sintering at high temperature in a wetting manner, uniformly adhering the pure aluminum slurry to the surface of the ceramic to form a high-strength bonded aluminum metal layer, carrying out aluminum pattern etching and anodic oxidation processes on the aluminum metal layer to convert the aluminum layer into an anodic oxidation layer with insulation characteristics and characteristic patterns, and preparing the anodic oxidation layer with certain thickness and pattern characteristics, wherein the aluminum anodic oxidation layer has certain insulation performance and forms a firm insulation boss structure on a ceramic matrix. And then, after the ceramic with the anodic oxide layer is subjected to an AMB sintering process, a copper-clad ceramic substrate mother board can be prepared, and the preparation of the copper-clad ceramic substrate is completed through the procedures of alignment exposure, pattern etching and cutting.
Compared with the existing ceramic substrate, the copper-clad ceramic substrate has a structure which is different from the conventional ceramic substrate in that the conventional ceramic substrate is Cu-ceramic-Cu, and the copper-clad ceramic substrate has a structure of Cu-Al anodic oxide layer-ceramic-Al anodic oxide layer, and the high-strength bonded insulating aluminum anodic oxide layer is introduced on the basis of the conventional copper-clad ceramic substrate, so that the high-voltage insulation reliability of the product is improved.
In order to avoid discharge instability under the condition of local high voltage, the preparation of the aluminum metallization layer is firstly carried out on the surface of Tao Jiban, and pattern etching and anodic oxidation are carried out on the local high-voltage part of the aluminum metallization layer, so that local high voltage concentration can be improved, local discharge instability is reduced, and insulation reliability is improved. Compared with the prior art, the invention has the following beneficial effects: according to the invention, the insulating aluminum anodic oxidation layer with high-strength bonding is introduced into the copper-ceramic junction surface, so that the insulating reliability of the product is improved, the graphic characteristics of the insulating anodic oxidation layer can be customized according to the product characteristics, and the insulating reliability of the product under the local high-voltage condition is further improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of a process for producing a copper-clad ceramic substrate according to the present invention;
FIG. 2 is partial discharge performance of example 1 of the present invention;
FIG. 3 is partial discharge performance of comparative example 1 of the present invention;
FIG. 4 is an aluminum metallization layer formed on the surface of a ceramic substrate in step S2 of example 1 of the present invention;
FIG. 5 is a graph A formed by etching a surface graph of an aluminum metallization layer in step S3 in example 1 of the present invention;
FIG. 6 is an anodized layer prepared in step S4 of example 1 of the present invention;
FIG. 7 is a schematic view showing that in step S5 of example 1 of the present invention, active metal solders are coated on both sides of the ceramic substrate;
FIG. 8 is a schematic view showing the steps of S5 for bonding copper foils to both sides of a ceramic substrate in accordance with example 1 of the present invention;
FIG. 9 is a circuit pattern etched on the surface of the copper foil in step S5 in example 1 of the present invention.
In the figure: 1-a ceramic substrate; 2-aluminum metallization layer; 3-graph A; 4-an anodic oxidation layer; 5-active metal solder; 6-copper foil; 7-circuit diagram.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1: a preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing pure aluminum slurry:
mixing 100g of spherical pure aluminum powder with the content of more than 99.9 percent with 27.1g of organic carrier, stirring and reacting for 10min, and fully grinding and mixing the slurry for 3 times by a three-roll grinder to form pure aluminum slurry;
s2: sintering of the ceramic aluminum metal layer:
selecting an aluminum nitride ceramic substrate 1 with the thickness of 1.0mm and the roughness Ra of 1.0 mu m, passing pure aluminum slurry through a 180-mesh screen, performing screen printing on one surface of the aluminum nitride ceramic substrate 1, drying by hot air nitrogen, continuously printing the pure aluminum slurry on the other surface of the ceramic substrate 1, horizontally placing the aluminum nitride ceramic substrate in a vacuum furnace after drying by the hot air nitrogen, vacuumizing to 0.0032Pa, heating to 950 ℃ for heat preservation for 120min, cooling to room temperature along with the furnace, and forming an aluminum metallization layer 2 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s3: etching of the aluminum metallization layer:
presetting a graph A3, taking the aluminum nitride ceramic substrate 1 prepared in the step S2, pasting a film on the surface of the aluminum nitride ceramic substrate 1, exposing, developing, and etching the aluminum metallization layer 2 graph to form the graph A3 for later use;
s4: anodizing of the aluminum metallization layer:
preparing 90g/L aqueous solution of sulfuric acid, heating to 0 deg.C, controlling the voltage at 15V and current density at 3.2A/dm by using the aluminum nitride ceramic substrate 1 as anode and graphite plate as cathode in step S3 2 Oxidizing for 120min to form an anodic oxide layer 4 on the surface of the aluminum nitride ceramic substrate for later use;
s5: brazing and sintering of active metal:
taking the aluminum nitride ceramic substrate 1 in the step S4, performing active metal printing and coating on an anodic oxidation layer 4 on the surface of the aluminum nitride ceramic substrate 1 by utilizing Ag-Cu-Ti active metal brazing filler metal 5, selecting a 180-mesh printing screen, coating the printing screen on the surface of the anodic oxidation layer, attaching 0.3mm copper foils 6 on two surfaces of the aluminum nitride ceramic substrate 1, performing vacuum sintering, keeping the sintering temperature at 860 ℃, keeping the temperature for 60min, and pressurizing for 0.2N/cm 2 Cooling to room temperature along with the furnace, pasting a film on the aluminum nitride ceramic substrate 1, carrying out contraposition exposure and development, etching a circuit pattern 7 on the surface of the copper foil 6, and carrying out a cutting process to obtain the copper-clad ceramic substrate.
In the embodiment, 100g of Ag-Cu-Ti alloy powder is mixed with 25.0g of organic carrier, after stirring for 10min, the slurry is fully ground and mixed for 5 times by a three-roll grinder to form Ag-Cu-Ti active metal slurry, and the alloy powder comprises 68.8% of Ag, 28.7% of Cu and 2.5% of Ti according to mass percentage; the grain diameter of the Ag-Cu-Ti alloy powder is 1-10 mu m.
The organic vehicle comprises 5.0% stearic acid, 6.0% ethylcellulose, 3.8% diisononyl phthalate, 6.8% dodecanol ester film former, and the balance isopropanol.
The thickness of the aluminium metallisation layer was 20 μm.
Example 2: a preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing pure aluminum slurry:
mixing 100g of spherical pure aluminum powder with the content of more than 99.9 percent with 33g of organic carrier, stirring and reacting for 10min, and fully grinding and mixing the slurry for 3 times by a three-roll grinder to form pure aluminum slurry;
s2: sintering of the ceramic aluminum metal layer:
selecting an aluminum nitride ceramic substrate 1 with the thickness of 1.0mm and the roughness Ra of 0.4 mu m, passing pure aluminum slurry through a 180-mesh screen, performing screen printing on one surface of the aluminum nitride ceramic substrate 1, drying by hot air nitrogen, continuously printing the pure aluminum slurry on the other surface of the ceramic substrate 1, horizontally placing the aluminum nitride ceramic substrate in a vacuum furnace after drying by the hot air nitrogen, vacuumizing to 0.0032Pa, heating to 850 ℃ for heat preservation for 10min, cooling to room temperature along with the furnace, and forming an aluminum metallization layer 2 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s3: etching of the aluminum metallization layer:
presetting a pattern A3, taking the aluminum nitride ceramic substrate 1 prepared in the step S2, pasting a film on the surface of the aluminum nitride ceramic substrate 1, exposing, developing, and etching the aluminum metallization layer 2 pattern to form the pattern A3 for later use;
s4: anodizing of the aluminum metallization layer:
after preparing an aqueous solution having a sulfuric acid concentration of 90g/L, the temperature was raised to 0 ℃ and the aluminum nitride ceramic substrate 1 obtained in step S3 was used as an anode and a graphite plate as a cathode, and the voltage and current density were controlled to 15V and 2.5A/dm, respectively 2 Oxidizing for 60min to form an anodic oxide layer 4 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s5: brazing and sintering of active metal:
taking the aluminum nitride ceramic substrate 1 in the step S4, utilizing Ag-Cu-Ti active metal solder 5 to carry out active metal printing and coating on an anodic oxidation layer 4 on the surface of the aluminum nitride ceramic substrate 1, selecting a 180-mesh printing screen, coating the printing screen on the surface 4 of the anodic oxidation layer, attaching 0.3mm copper foils 6 on two sides of the aluminum nitride ceramic substrate 1, carrying out vacuum sintering, wherein the sintering temperature is 850 ℃, keeping the temperature for 60min, and pressurizing for 0.2N/cm 2 And cooling to room temperature along with the furnace, then pasting a film on the aluminum nitride ceramic substrate 1, carrying out contraposition exposure and development, etching a circuit pattern 7 on the surface of the copper foil 6, and carrying out a cutting process to obtain the copper-clad ceramic substrate.
In the embodiment, 100g of Ag-Cu-Ti alloy powder is mixed with 25.0g of organic carrier, after stirring for 10min, the slurry is fully ground and mixed for 5 times by a three-roll grinder to form Ag-Cu-Ti active metal slurry, and the alloy powder comprises 68.8% of Ag, 28.7% of Cu and 2.5% of Ti according to mass percentage; the grain diameter of the Ag-Cu-Ti alloy powder is 1-10 mu m.
The organic vehicle included 5.0% stearic acid, 6.0% ethylcellulose, 3.8% diisononyl phthalate, 6.8% dodecanol ester film former, and the balance isopropanol.
The thickness of the aluminium metallisation layer was 30 μm.
Example 3: a preparation method for improving insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing pure aluminum slurry:
mixing 100g of spherical pure aluminum powder with the content of more than 99.9 percent with 25g of organic carrier, stirring and reacting for 11min, and fully grinding and mixing the slurry for 3 times by a three-roll grinder to form pure aluminum slurry;
s2: sintering of the ceramic aluminum metal layer:
selecting an aluminum nitride ceramic substrate 1 with the thickness of 1.0mm and the roughness Ra of 0.5 mu m, passing pure aluminum slurry through a 180-mesh screen, performing screen printing on one surface of the aluminum nitride ceramic substrate 1, drying by hot air nitrogen, continuously printing the pure aluminum slurry on the other surface of the ceramic substrate 1, horizontally placing the aluminum nitride ceramic substrate in a vacuum furnace after drying by the hot air nitrogen, vacuumizing to 0.0032Pa, heating to 860 ℃ for heat preservation for 20min, cooling to room temperature along with the furnace, and forming an aluminum metallization layer 2 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s3: etching of the aluminum metallization layer:
presetting a pattern A3, taking the aluminum nitride ceramic substrate 1 prepared in the step S2, pasting a film on the surface of the aluminum nitride ceramic substrate 1, exposing, developing, and etching the aluminum metallization layer 2 pattern to form the pattern A3 for later use;
s4: anodic oxidation of aluminum metallization layer:
after preparing an aqueous solution having a sulfuric acid concentration of 100g/L, the temperature was raised to 1 ℃ and the aluminum nitride ceramic substrate 1 obtained in step S3 was used as an anode and a graphite plate as a cathode, and the voltage and current density were controlled to 15V and 3.0A/dm, respectively 2 Oxidizing for 70min to form an anodic oxide layer 4 on the surface of the aluminum nitride ceramic substrate 1Using;
s5: brazing and sintering of active metal:
taking the aluminum nitride ceramic substrate 1 in the step S4, performing active metal printing and coating on an anodic oxide layer on the surface of the aluminum nitride ceramic substrate by utilizing Ag-Cu-Ti active metal brazing filler metal 5, selecting a 180-mesh printing screen, coating the printing screen on the surface 4 of the anodic oxide layer, attaching 0.3mm copper foils 6 on two surfaces of the aluminum nitride ceramic substrate 1, performing vacuum sintering, keeping the sintering temperature at 860 ℃, keeping the temperature for 60min, and pressurizing for 0.3N/cm 2 And cooling the aluminum nitride ceramic substrate 1 to room temperature along with the furnace, laminating a film on the aluminum nitride ceramic substrate 1, carrying out contraposition exposure and development, etching a circuit pattern 7 on the surface of the copper foil 6, and carrying out a cutting process to obtain the copper-clad ceramic substrate.
In the embodiment, 100g of Ag-Cu-Ti alloy powder is mixed with 25.0g of organic carrier, after stirring for 10min, the slurry is fully ground and mixed for 5 times by a three-roll grinder to form Ag-Cu-Ti active metal slurry, and the alloy powder comprises 68.8% of Ag, 28.7% of Cu and 2.5% of Ti according to mass percentage; the grain diameter of the Ag-Cu-Ti alloy powder is 1-10 mu m.
The organic vehicle comprises 5.0% stearic acid, 6.0% ethylcellulose, 3.8% diisononyl phthalate, 6.8% dodecanol ester film former, and the balance isopropanol.
The thickness of the aluminium metallisation layer was 40 μm.
Example 4: a preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing pure aluminum slurry:
mixing 100g of spherical pure aluminum powder with the content of more than 99.9 percent with 30g of organic carrier, stirring and reacting for 12min, and fully grinding and mixing the slurry for 3 times by a three-roll grinder to form pure aluminum slurry;
s2: sintering of the ceramic aluminum metal layer:
selecting an aluminum nitride ceramic substrate 1 with the thickness of 1.0mm and the roughness Ra of 0.7 mu m, passing pure aluminum slurry through a 180-mesh screen, performing screen printing on one surface of the aluminum nitride ceramic substrate 1, drying by hot air nitrogen, continuously printing the pure aluminum slurry on the other surface of the ceramic substrate 1, horizontally placing in a vacuum furnace after drying by the hot air nitrogen, vacuumizing to 0.0032Pa, heating to 870 ℃, preserving heat for 50min, cooling to room temperature along with the furnace, and forming an aluminum metallization layer 2 on the surface of the aluminum nitride ceramic substrate for later use;
s3: etching of the aluminum metallization layer:
presetting a pattern A3, taking the aluminum nitride ceramic substrate 1 prepared in the step S2, pasting a film on the surface of the aluminum nitride ceramic substrate 1, exposing, developing, and etching the aluminum metallization layer 2 pattern to form the pattern A3 for later use;
s4: anodizing of the aluminum metallization layer:
preparing an aqueous solution with a sulfuric acid concentration of 110g/L, heating to 2 ℃, and controlling the voltage to be 15V and the current density to be 3.5A/dm by taking the aluminum nitride ceramic substrate 1 in the step S3 as an anode and a graphite plate as a cathode 2 Oxidizing for 80min to form an anodic oxide layer 4 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s5: active metal brazing and sintering:
taking the aluminum nitride ceramic substrate 1 in the step S4, performing active metal printing and coating on the anodic oxidation layer 4 on the surface of the aluminum nitride ceramic substrate 1 by utilizing Ag-Cu-Ti active metal brazing filler metal 5, selecting a 180-mesh printing screen, coating the printing screen on the surface of the anodic oxidation layer 4, attaching 0.3mm copper foils 6 on two surfaces of the aluminum nitride ceramic substrate 1, performing vacuum sintering, keeping the sintering temperature of 8800 ℃, keeping the temperature for 60min, and pressurizing for 0.3N/cm 2 Cooling to room temperature along with the furnace, pasting a film on the aluminum nitride ceramic substrate 1, carrying out contraposition exposure and development, etching a circuit pattern 7 on the surface of the copper foil 6, and carrying out a cutting process to obtain the copper-clad ceramic substrate.
In the embodiment, 100g of Ag-Cu-Ti alloy powder is mixed with 25.0g of organic carrier, after stirring for 10min, the slurry is fully ground and mixed for 5 times by a three-roll grinder to form Ag-Cu-Ti active metal slurry, and the alloy powder comprises 68.8% of Ag, 28.7% of Cu and 2.5% of Ti according to mass percentage; the grain diameter of the Ag-Cu-Ti alloy powder is 1-10 mu m.
The organic vehicle comprises 5.0% stearic acid, 6.0% ethylcellulose, 3.8% diisononyl phthalate, 6.8% dodecanol ester film former, and the balance isopropanol.
The thickness of the aluminium metallisation layer is 50 μm.
Example 5: a preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing pure aluminum slurry:
mixing 100g of spherical pure aluminum powder with the content of more than 99.9 percent and 28g of organic carrier, stirring and reacting for 13min, and fully grinding and mixing the slurry for 4 times by a three-roll grinder to form pure aluminum slurry;
s2: sintering of the ceramic aluminum metal layer:
selecting an aluminum nitride ceramic substrate 1 with the thickness of 1.0mm and the roughness Ra of 0.8 mu m, passing pure aluminum slurry through a 180-mesh screen, performing screen printing on one surface of the aluminum nitride ceramic substrate 1, drying by hot air nitrogen, continuously printing the pure aluminum slurry on the other surface of the ceramic substrate 1, horizontally placing the aluminum nitride ceramic substrate in a vacuum furnace after drying by the hot air nitrogen, vacuumizing to 0.0032Pa, heating to 890 ℃, preserving heat for 60min, cooling to room temperature along with the furnace, and forming an aluminum metallization layer 2 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s3: etching of the aluminum metallization layer:
presetting a pattern A3, taking the aluminum nitride ceramic substrate 1 prepared in the step S2, pasting a film on the surface of the aluminum nitride ceramic substrate 1, exposing, developing, and etching the aluminum metallization layer 2 pattern to form the pattern A3 for later use;
s4: anodizing of the aluminum metallization layer:
after preparing an aqueous solution having a sulfuric acid concentration of 120g/L, the temperature was raised to 1 ℃ and the aluminum nitride ceramic substrate 1 obtained in step S3 was used as an anode and a graphite plate as a cathode, and the voltage and current density were controlled to 15V and 3.6A/dm, respectively 2 Oxidizing for 80min to form an anodic oxide layer 4 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s5: active metal brazing and sintering:
taking the aluminum nitride ceramic substrate 1 in the step S4, performing active metal printing and coating on the anodic oxidation layer 4 on the surface of the aluminum nitride ceramic substrate 1 by utilizing Ag-Cu-Ti active metal brazing filler metal 5, selecting a 180-mesh printing screen, coating the screen on the surface of the anodic oxidation layer 4, and then coating the screen on two sides of the aluminum nitride ceramic substrate 1After being attached with a 0.3mm copper foil 6, vacuum sintering is carried out, the sintering temperature is 890 ℃, the temperature is kept for 60min, and the pressure is 0.3N/cm 2 And cooling to room temperature along with the furnace, then pasting a film on the aluminum nitride ceramic substrate 1, carrying out contraposition exposure and development, etching a circuit pattern 7 on the surface of the copper foil 6, and carrying out a cutting process, thus obtaining the copper-clad ceramic substrate.
In the embodiment, 100g of Ag-Cu-Ti alloy powder is mixed with 25.0g of organic carrier, after stirring for 10min, the slurry is fully ground and mixed for 5 times by a three-roll grinder to form Ag-Cu-Ti active metal slurry, and the alloy powder comprises 68.8% of Ag, 28.7% of Cu and 2.5% of Ti according to mass percentage; the grain diameter of the Ag-Cu-Ti alloy powder is 1-10 mu m.
The organic vehicle comprises 5.0% stearic acid, 6.0% ethylcellulose, 3.8% diisononyl phthalate, 6.8% dodecanol ester film former, and the balance isopropanol.
The thickness of the aluminium metallisation layer was 60 μm.
Example 6: a preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing pure aluminum slurry:
mixing 100g of spherical pure aluminum powder with the content of more than 99.9 percent with 26g of organic carrier, stirring and reacting for 4min, and fully grinding and mixing the slurry for 4 times by a three-roll grinder to form pure aluminum slurry;
s2: sintering of the ceramic aluminum metal layer:
selecting an aluminum nitride ceramic substrate 1 with the thickness of 1.0mm and the roughness Ra of 0.9 mu m, passing pure aluminum slurry through a 180-mesh screen, performing screen printing on one surface of the aluminum nitride ceramic substrate 1, drying by hot air nitrogen, continuously printing the pure aluminum slurry on the other surface of the ceramic substrate 1, horizontally placing the aluminum nitride ceramic substrate in a vacuum furnace after drying by the hot air nitrogen, vacuumizing to 0.0032Pa, heating to 900 ℃, preserving heat for 90min, cooling to room temperature along with the furnace, and forming an aluminum metallization layer 2 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s3: etching of the aluminum metallization layer:
presetting a graph A3, taking the aluminum nitride ceramic substrate 1 prepared in the step S2, pasting a film on the surface of the aluminum nitride ceramic substrate 1, exposing, developing, and etching the aluminum metallization layer graph to form the graph A3 for later use;
s4: anodizing of the aluminum metallization layer:
preparing aqueous solution with sulfuric acid concentration of 110g/L, heating to 3 ℃, taking the aluminum nitride ceramic substrate in the step S3 as an anode and a graphite plate as a cathode, controlling the voltage to be 15V and the current density to be 2.5A/dm 2 Oxidizing for 100min to form an anodic oxide layer on the surface of the aluminum nitride ceramic substrate for later use;
s5: brazing and sintering of active metal:
taking the aluminum nitride ceramic substrate 1 in the step S4, utilizing Ag-Cu-Ti active metal solder 5 to carry out active metal printing and coating on an anodic oxidation layer 4 on the surface of the aluminum nitride ceramic substrate 1, selecting a 180-mesh printing screen, coating the printing screen on the surface of the anodic oxidation layer 4, attaching 0.3mm copper foils 6 on two surfaces of the aluminum nitride ceramic substrate 1, carrying out vacuum sintering, wherein the sintering temperature is 920 ℃, keeping the temperature for 60min, and pressurizing for 0.5N/cm 2 And cooling to room temperature along with the furnace, then pasting a film on the aluminum nitride ceramic substrate 1, carrying out contraposition exposure and development, etching a circuit pattern 7 on the surface of the copper foil 6, and carrying out a cutting process to obtain the copper-clad ceramic substrate.
In the embodiment, 100g of Ag-Cu-Ti alloy powder and 25.0g of organic carrier are mixed, stirred for 10min, and then the slurry is fully ground and mixed for 5 times by a three-roll grinder to form Ag-Cu-Ti active metal slurry, wherein the alloy powder comprises 68.8% of Ag, 28.7% of Cu and 2.5% of Ti according to mass percentage; the grain diameter of the Ag-Cu-Ti alloy powder is 1-10 mu m.
The organic vehicle comprises 5.0% stearic acid, 6.0% ethylcellulose, 3.8% diisononyl phthalate, 6.8% dodecanol ester film former, and the balance isopropanol.
The thickness of the aluminium metallisation layer was 80 μm.
Example 7: a preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
s1: preparing pure aluminum slurry:
mixing 100g of spherical pure aluminum powder with the content of more than 99.9 percent and 33g of organic carrier, stirring and reacting for 15min, and then fully grinding and mixing the slurry for 5 times by a three-roll grinder to form pure aluminum slurry;
s2: sintering of the ceramic aluminum metal layer:
selecting an aluminum nitride ceramic substrate 1 with the thickness of 1.0mm and the roughness Ra of 1.6 mu m, passing pure aluminum slurry through a 180-mesh screen, performing screen printing on one surface of the aluminum nitride ceramic substrate 1, drying by hot air nitrogen, continuously printing the pure aluminum slurry on the other surface of the ceramic substrate 1, horizontally placing in a vacuum furnace after drying by the hot air nitrogen, vacuumizing to 0.0032Pa, heating to 1200 ℃, preserving heat for 120min, cooling to room temperature along with the furnace, and forming an aluminum metalized layer 2 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s3: etching of the aluminum metallization layer:
presetting a pattern A3, taking the aluminum nitride ceramic substrate 1 prepared in the step S2, pasting a film on the surface of the aluminum nitride ceramic substrate 1, exposing, developing, and etching the aluminum metallization layer 2 pattern to form the pattern A3 for later use;
s4: anodizing of the aluminum metallization layer:
preparing 130g/L aqueous solution of sulfuric acid, heating to 3 deg.C, controlling voltage at 15V and current density at 4.5A/dm with the aluminum nitride ceramic substrate 1 as anode and graphite plate as cathode in step S3 2 Oxidizing for 120min to form an anodic oxide layer 4 on the surface of the aluminum nitride ceramic substrate 1 for later use;
s5: active metal brazing and sintering:
taking the aluminum nitride ceramic substrate 1 in the step S4, utilizing Ag-Cu-Ti active metal solder 5 to carry out active metal printing and coating on an anodic oxidation layer 4 on the surface of the aluminum nitride ceramic substrate 1, selecting a 180-mesh printing screen, coating the printing screen on the surface of the anodic oxidation layer 4, attaching 0.3mm copper foils 6 on two surfaces of the aluminum nitride ceramic substrate 1, carrying out vacuum sintering, wherein the sintering temperature is 950 ℃, keeping the temperature for 60min, and pressurizing for 0.6N/cm 2 And cooling to room temperature along with the furnace, then pasting a film on the aluminum nitride ceramic substrate 1, carrying out contraposition exposure and development, etching a circuit pattern 7 on the surface of the copper foil 6, and carrying out a cutting process to obtain the copper-clad ceramic substrate.
In the embodiment, 100g of Ag-Cu-Ti alloy powder is mixed with 25.0g of organic carrier, after stirring for 10min, the slurry is fully ground and mixed for 5 times by a three-roll grinder to form Ag-Cu-Ti active metal slurry, and the alloy powder comprises 68.8% of Ag, 28.7% of Cu and 2.5% of Ti according to mass percentage; the grain diameter of the Ag-Cu-Ti alloy powder is 1-10 mu m.
The organic vehicle comprises 5.0% stearic acid, 6.0% ethylcellulose, 3.8% diisononyl phthalate, 6.8% dodecanol ester film former, and the balance isopropanol.
The thickness of the aluminium metallisation layer is 100 μm.
Comparative example
Comparative example 1: a preparation method for improving the insulation reliability of a copper-clad ceramic substrate comprises the following steps:
the copper-clad ceramic substrate is prepared by adopting a general active metal brazing method, namely, the aluminum nitride ceramic with the same specification as the aluminum nitride ceramic in the embodiment 1 is adopted, the aluminum nitride ceramic is subjected to Ag-Cu-Ti slurry pattern printing, the copper foil with the thickness of 0.3mm is attached to the two sides of the aluminum nitride ceramic, the vacuum sintering is carried out, the sintering temperature is 860 ℃, the heat preservation is carried out for 60min, and the pressurization is carried out for 0.2N/cm 2 And cooling to room temperature along with the furnace, and then adopting common processes of film pasting, contraposition exposure, development, etching, cutting and the like to finish the preparation of the copper-clad ceramic substrate.
Experimental data
The samples of the examples and the comparative example 1 were subjected to the front and back partial discharge performance test under the condition of a high voltage of 8.3KV and a duration of 1 min.
TABLE 1 EXAMPLES 1-7, COMPARATIVE EXAMPLE 1 examination results of each item
Figure BDA0003574137850000111
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Figure BDA0003574137850000121
And (4) conclusion: the comparison shows that the drift characteristic of the partial discharge capacity of the sample in the embodiment 1 is obviously reduced compared with that of the sample in the comparative example 1, so that the risk caused by unstable partial discharge capacity due to power conversion or local high voltage and other factors when the device works is greatly reduced, and the insulation reliability of the product is improved.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A preparation method for improving the insulation reliability of a copper-clad ceramic substrate is characterized by comprising the following steps: the method comprises the following steps:
s1: preparing an aluminum metallization layer (2) on the surface of the ceramic substrate (1) by sequentially performing screen printing and high-temperature wettability sintering on pure aluminum slurry for later use;
s2: presetting a pattern A (3), taking the ceramic substrate (1) in the step S1, etching the pattern of the aluminum metallization layer (2) to form the pattern A (3), and carrying out anodic oxidation on the pattern A (3) on the surface of the aluminum metallization layer to form an anodic oxidation layer (4);
s3: taking the substrate prepared in the step S2, coating active metal brazing filler metal (5) on the surfaces of two sides of the ceramic substrate (1), attaching copper foils (6) on two sides of the ceramic substrate (1), performing vacuum sintering, performing contraposition exposure, and etching and cutting circuit patterns (7) on the surfaces of the copper foils (6) to obtain the copper-clad ceramic substrate;
the method for anodizing the aluminum metallization layer (2) comprises the following steps: placing a ceramic substrate with an aluminum metalized layer on the surface as an anode and a graphite plate as a cathode in a sulfuric acid aqueous solution at a current density of 2.5-4.5A/dm 2 And carrying out an oxidation reaction.
2. The preparation method for improving the insulation reliability of the copper-clad ceramic substrate according to claim 1, wherein the preparation method comprises the following steps: the concentration of the sulfuric acid aqueous solution is 90-130g/L, the oxidation reaction temperature is 0-3 ℃, and the oxidation reaction time is 60-150min.
3. The preparation method for improving the insulation reliability of the copper-clad ceramic substrate according to claim 1, wherein the preparation method comprises the following steps: in the step S1, the preparation method of the pure aluminum slurry comprises the steps of mixing pure aluminum powder and an organic carrier, stirring and reacting for 10-15min, and grinding to obtain the pure aluminum slurry, wherein the mass ratio of the pure aluminum powder to the organic carrier is (3-4): 1.
4. The preparation method for improving the insulation reliability of the copper-clad ceramic substrate according to claim 3, wherein the preparation method comprises the following steps: the pure aluminum powder is spherical aluminum powder with the particle size of 1-10 mu m; the organic carrier comprises the following materials in parts by weight: 5-10% of stearic acid, 6-12% of ethyl cellulose, 3-6% of diisononyl phthalate, 5-10% of dodecanol ester and the balance of isopropanol.
5. The preparation method for improving the insulation reliability of the copper-clad ceramic substrate according to claim 1, wherein the preparation method comprises the following steps: in the step S1, the high-temperature wettability sintering temperature is 850-1200 ℃, and the sintering time is 10-120min.
6. The preparation method for improving the insulation reliability of the copper-clad ceramic substrate according to claim 1, wherein the preparation method comprises the following steps: in step S3, the vacuum sintering temperature is 850-950 ℃, the temperature is kept for 60min, and the pressure is 0.2-0.6N/cm 2 And (5) cooling along with the furnace.
7. The preparation method for improving the insulation reliability of the copper-clad ceramic substrate according to claim 1, wherein the preparation method comprises the following steps: in the step S1, the thickness of the aluminum metallization layer (2) is 20-100 μm; in the step S3, the thickness of the copper foil (6) is 0.2-0.8mm.
8. The preparation method for improving the insulation reliability of the copper-clad ceramic substrate according to claim 1, wherein the preparation method comprises the following steps: the thickness of the ceramic substrate (1) is 0.25-1.0mm; the ceramic substrate (1) is one or more of an aluminum nitride ceramic substrate, an aluminum oxide ceramic substrate and a silicon nitride ceramic substrate.
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