CN103819214A - AlN ceramic bonded copper substrate and preparation method thereof - Google Patents
AlN ceramic bonded copper substrate and preparation method thereof Download PDFInfo
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- CN103819214A CN103819214A CN201410010989.4A CN201410010989A CN103819214A CN 103819214 A CN103819214 A CN 103819214A CN 201410010989 A CN201410010989 A CN 201410010989A CN 103819214 A CN103819214 A CN 103819214A
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Abstract
The invention provides an AlN ceramic bonded copper substrate which comprises an AlN ceramic substrate and copper foil bonded and connected onto the AlN ceramic substrate and is characterized in that a spinel structure compound modification layer is formed between the AlN ceramic substrate and the copper foil and comprises one or two of CuAlO2, CuAl2O4, Cu2O and CuO. The invention further provides a preparation method of the AlN ceramic bonded copper substrate. The method comprises the steps of spraying nano Cu2O on the surface of the AlN substrate, sintering in inert gas with a micro oxygen content and air sequentially, and then removing a surface oxide by a pickling manner. The prepared modification layer is tightly combined with matrix ceramic, and also has good affinity characteristic with the Cu foil. A uniform oxidation layer can be formed on the surface of the Cu foil by putting the Cu foil in a prepared solution at a certain temperature for specified time and more facilitates an AlN-DBC (direct bonded copper) technology.
Description
Technical field
The present invention relates to a kind of AlN pottery bonded copper base and preparation method thereof, belong to ceramic metallization field.
Background technology
AlN pottery is widely used in the field such as microelectronics, photoelectron with advantages such as the thermal expansivity of its excellent heat conductivility, preferably specific inductivity and Si coupling, AlN ceramic surface metallization mode is various, as electroless plating, DPC, method for brazing etc., for power electronics, direct copper method (DBC) is comparatively desirable selection, and AlN-DBC can meet the comparatively harsh requirement such as the high thermal conductance of power electronic devices, highly reliable, large electric current.
An aggressiveness that significant characteristic is anti-molten metal of AlN pottery, relies on so liquid phase directly to soak AlN pottery and just becomes comparatively difficulty.Therefore in DBC technique, be, necessary by the modification of AlN ceramic surface.In traditional DBC technique, conventionally AlN pottery high temperature oxidation more than 1200 ℃ need to be made it to Surface Creation one deck Al
2o
3film is realized combination as transition layer and then with Cu within the scope of 1065 ℃-1083 ℃.But big area, continuous copper and Al
2o
3combination difficulty relatively, there is the defect such as bubble, white point at copper and Ceramic bond place more, the existence of these defects obviously reduces the performances such as the stripping strength, bonding strength, heat shock resistance, thermal conductivity of AlN-DBC substrate.
Summary of the invention
The object of the invention is the reliable deposited technical problem connecing that preparation method in order to solve AlN of the prior art pottery bonded copper base is difficult to realize AlN ceramic substrate and Copper Foil.
For reaching goal of the invention, the technical solution used in the present invention is: a kind of AlN pottery bonded copper base, comprise: AlN ceramic substrate, the deposited Copper Foil being connected on AlN ceramic substrate, between described AlN ceramic substrate and Copper Foil, form the compound modified layer of spinel structure, in the compound modified layer of described spinel structure, contain CuAlO
2, CuAl
2o
4, and Cu
2one or both in O, CuO.
In addition, the present invention also provides the preparation method of above-mentioned AlN pottery bonded copper base, comprises the steps:
S1, spraying nanometer Cu
2o forms compound coating on AlN ceramic base plate surface;
S2, this is had to the AlN ceramic substrate of compound coating, successively high temperature sintering in the rare gas element of micro-oxygen level and air, the rear mode with pickling is removed oxide on surface, then dries;
S3, by Copper Foil suitable size chemical oxidation method preoxidation, preoxidation solution medicine comprises Na
2s
2o
8, K
2s
2o
8in one, and one in NaOH, KOH;
The Copper Foil that S4, the AlN ceramic substrate that step S2 is obtained and step S3 obtain applies and connects, and makes AlN pottery bonded copper base.
Preferably, the thickness of described AlN ceramic substrate is 0.38 ~ 1.0mm; The thickness of described Copper Foil is 0.2 ~ 0.3mm.
Preferably, the thickness of described AlN ceramic substrate is 0.63mm; The thickness of described Copper Foil is 0.3mm.
Preferably, in step S1, selecting particle diameter is the nanometer Cu below 100 nm
2o, compound thickness of coating is 0.05 ~ 0.15mm.
Preferably, in step S1, compound thickness of coating is 0.1mm.
Preferably; priority described in step S2 is high temperature sintering in the rare gas element of micro-oxygen level and air; refer to and first under the rare gas element Ar of micro-oxygen level guard mode, be sintered to T1 temperature; the insulation t1 time; in air, the temperature rise rate with 1 ~ 1.5 ℃/min is warmed up to T2 temperature from T1 temperature again; the insulation t2 time; wherein T1 is 900 ~ 1000 ℃; the t1 time is 10 ~ 60Min; T2 is 1080 ~ 1100 ℃; the t2 time is 10 ~ 60Min, in the HCl solution that is then 5% in mass concentration, places 10 ~ 60Min.
Preferably, described T1 is 1000 ℃, and the t1 time is 40Min, and temperature rise rate is 1 ℃/min, and T2 is 1090 ℃, and the t2 time is 40Min, and pickling time is 40min.
Preferably, described step S4 carries out in atmosphere furnace, and protective atmosphere is that purity is greater than or equal to 99.99% N
2, temperature is 1070 ~ 1080 ℃, the time is 5 ~ 20 Min.
Preferably, in described step S4, temperature is 1075 ℃, and the time is 15Min.
Implement beneficial effect of the present invention:
1, adopt the method for spraying can control the thickness of the compound coating of AlN ceramic base plate surface.
2, pass through high temperature sintering, compound coating is in self densified sintering product, compound coating and AlN ceramic substrate are closely linked, the compound modified layer of spinel structure of the even compact forming, AlN ceramic substrate and Copper Foil can be separated completely, avoid Cu-O eutectic liquid phase to be penetrated into inner AlN layer and reacted generation bubble with AlN, thereby improved yield rate;
3, the introducing of the compound modified layer of AlN ceramic base plate surface spinel structure, improve to a great extent the wetness degree of the relative AlN ceramic base plate surface of Cu-O eutectic liquid, reduce wetting angle, make Cu-O eutectic liquid can fully soak mutually the surface of AlN ceramic substrate, Copper Foil is realized with engaging more easily of AlN ceramic substrate; Meanwhile, compound modified layer has also improved because Copper Foil and the thermal stresses of AlN ceramic substrate are not mated the excessive defect of AlN ceramic copper-clad base plate internal stress causing.
Embodiment
embodiment 1
The preparation method of this AlN pottery bonded copper base, comprises the steps:
S1, spraying: the method for use spraying for the surface of 0.63mmAlN ceramic substrate sprays plated film, makes the surface of AlN ceramic substrate form a nanometer Cu at the thickness cleaning
2o coating, the thickness of coating finally needing is controlled at 0.1mm;
S2, sintering: will be after spraying; the AlN ceramic substrate that surface is formed with compound coating is first placed under the rare gas element Ar guard mode of micro-oxygen level and is sintered to 1000 ℃ of temperature; insulation 40Min; then in air, the temperature rise rate of 1 ℃/min is warmed up to 1090 ℃ of temperature from 1000 ℃ of temperature, insulation 40Min.In the HCl solution that is 5% in mass concentration again, place 40Min, remove oxide on surface.In sintering process, the surface oxidation of AlN ceramic substrate forms Al
2o
3when thin layer, also can there is correlated response in compound coating, and various chemical equation are specific as follows:
AlN+O
2→Al
2O
3+?N
2↑
Al
2O
3+?Cu
2O→Cu?AlO
2
AlN+Cu
2O+O
2→Cu?AlO
2+?N
2↑
As from the foregoing, compound coating in self densified sintering product, also can with AlN pottery (or the Al of AlN ceramic surface
2o
3layer) be closely adhered to together.
The oxidation of S3, Copper Foil: it is that the solution of 5% Na2S2O8,10% NaOH soaks 5Min copper foil surface and generates Cu at 25 ℃ that the Copper Foil of cutting suitable dimension is put into mass concentration
2o; The thickness of described Copper Foil is 0.3mm.Concrete chemical equation is as follows:
Na
2S
2O
8+2Cu+2?NaOH→Cu
2O↓+2?Na
2SO
4+H
2O。
S4, Copper Foil and the deposited of AlN ceramic substrate connect: will apply and connect with put into tube-type atmosphere furnace after the Copper Foil of preoxidation is superimposed through the AlN ceramic substrate of high temperature sintering, protective atmosphere be N
2(purity>=99.99%), deposited jointing temp is 1075 ℃, and the surface of Copper Foil forms Cu-O eutectic liquid phase, and soaking time is 15Min, and then then cool to room temperature removes the preoxidation layer on non-binding of Copper Foil, makes AlN pottery bonded copper base.
In the AlN pottery bonded copper base finally obtaining, stripping strength >=6N/mm; Bubble rate≤10%.
embodiment 2
The preparation method of this AlN pottery bonded copper base, comprises the steps:
S1, spraying: the method for use spraying for the surface of 0.38mmAlN ceramic substrate sprays plated film, makes the surface of AlN ceramic substrate form a nanometer Cu at the thickness cleaning
2o coating, the thickness of coating finally needing is controlled at 0.05mm;
S2, sintering: will be after spraying; the AlN ceramic substrate that surface is formed with compound coating is first placed under the rare gas element Ar guard mode of micro-oxygen level and is sintered to 900 ℃ of temperature; insulation 10Min; then in air, the temperature rise rate of 1.5 ℃/min is warmed up to 1100 ℃ of temperature from 900 ℃ of temperature, insulation 10Min.In the HCl solution that is 5% in mass concentration again, place 10Min, remove oxide on surface;
The oxidation of S3, Copper Foil: it is 5% Na that the Copper Foil of cutting suitable dimension is put into mass concentration
2s
2o
8, 10% KOH solution at 25 ℃, soak 5Min copper foil surface and generate Cu
2o; The thickness of described Copper Foil is 0.2mm.
S4, Copper Foil and the deposited of AlN ceramic substrate connect: will apply and connect with put into tube-type atmosphere furnace after the Copper Foil of preoxidation is superimposed through the AlN ceramic substrate of high temperature sintering, protective atmosphere be N
2(purity>=99.99%), deposited jointing temp is 1070 ℃, and the surface of Copper Foil forms Cu-O eutectic liquid phase, and soaking time is 20Min, and then then cool to room temperature removes the preoxidation layer on non-binding of Copper Foil, makes AlN pottery bonded copper base.
The AlN pottery bonded copper base stripping strength >=5N/mm finally obtaining; Bubble rate≤10%.
?
embodiment 3
The preparation method of this AlN pottery bonded copper base, comprises the steps:
S1, spraying: the method for use spraying for the surface of 1.0mmAlN ceramic substrate sprays plated film, makes the surface of AlN ceramic substrate form a nanometer Cu at the thickness cleaning
2o coating, the thickness of coating finally needing is controlled at 0.15mm;
S2, sintering: will be after spraying; the AlN ceramic substrate that surface is formed with compound coating is first placed under the rare gas element Ar guard mode of micro-oxygen level and is sintered to 1000 ℃ of temperature; insulation 60Min; then in air, the temperature rise rate of 1.2 ℃/min is warmed up to 1080 ℃ of temperature from 1000 ℃ of temperature, insulation 60Min.In the HCl solution that is 2.5% in mass concentration again, place 60Min, remove oxide on surface.
The oxidation of S3, Copper Foil: it is 5% K that the Copper Foil of cutting suitable dimension is put into mass concentration
2s
2o
8, 10% NaOH solution at 25 ℃, soak 5Min copper foil surface and generate Cu
2o; The thickness of described Copper Foil is 0.25mm.
S4, Copper Foil and the deposited of AlN ceramic substrate connect: will apply and connect with put into tube-type atmosphere furnace after the Copper Foil of preoxidation is superimposed through the AlN ceramic substrate of high temperature sintering, protective atmosphere be N
2(purity>=99.99%), deposited jointing temp is 1080 ℃, and the surface of Copper Foil forms Cu-O eutectic liquid phase, and soaking time is 5Min, and then then cool to room temperature removes the preoxidation layer on non-binding of Copper Foil, makes AlN pottery bonded copper base.
The AlN pottery bonded copper base >=5N/mm finally obtaining; Bubble rate≤13%.
?
embodiment 4
The preparation method of this AlN pottery bonded copper base, comprises the steps:
S1, spraying: the method for use spraying for the surface of 1.0mmAlN ceramic substrate sprays plated film, makes the surface of AlN ceramic substrate form a nanometer Cu at the thickness cleaning
2o coating, the thickness of coating finally needing is controlled at 0.1mm;
S2, sintering: will be after spraying; the AlN ceramic substrate that surface is formed with compound coating is first placed under the rare gas element Ar guard mode of micro-oxygen level and is sintered to 950 ℃ of temperature; insulation 30Min; then in air, the temperature rise rate of 1.3 ℃/min is warmed up to 1090 ℃ of temperature from 950 ℃ of temperature, insulation 30Min.In the HCl solution that is 5% in mass concentration again, place 50Min, remove oxide on surface.
The oxidation of S3, Copper Foil: it is 5% K that the Copper Foil of cutting suitable dimension is put into mass concentration
2s
2o
8, 10% KOH solution at 25 ℃, soak 5Min copper foil surface and generate Cu
2o; The thickness of described Copper Foil is 0.25mm.
S4, Copper Foil and the deposited of AlN ceramic substrate connect: will apply and connect with put into tube-type atmosphere furnace after the Copper Foil of preoxidation is superimposed through the AlN ceramic substrate of high temperature sintering, protective atmosphere be N
2(purity>=99.99%), deposited jointing temp is 1075 ℃, and the surface of Copper Foil forms Cu-O eutectic liquid phase, and soaking time is 13Min, and then then cool to room temperature removes the preoxidation layer on non-binding of Copper Foil, makes AlN pottery bonded copper base.
The AlN pottery bonded copper base >=6N/mm finally obtaining; Bubble rate≤10%.
Claims (10)
1. an AlN pottery bonded copper base, comprise: AlN ceramic substrate, the deposited Copper Foil being connected on AlN ceramic substrate, it is characterized in that: between described AlN ceramic substrate and Copper Foil, form the compound modified layer of spinel structure, in the compound modified layer of described spinel structure, contain CuAlO
2, CuAl
2o
4, and Cu
2one or both in O, CuO.
2. the preparation method of the pottery of the AlN described in claim 1 or 2 bonded copper base, is characterized in that:
S1, spraying nanometer Cu
2o forms compound coating on AlN ceramic base plate surface;
S2, this is had to the AlN ceramic substrate of compound coating, successively high temperature sintering in the rare gas element of micro-oxygen level and air, the rear mode with pickling is removed oxide on surface, then dries;
S3, by Copper Foil suitable size chemical oxidation method preoxidation, preoxidation solution medicine comprises Na
2s
2o
8, K
2s
2o
8in one, and one in NaOH, KOH;
The Copper Foil that S4, the AlN ceramic substrate that step S2 is obtained and step S3 obtain applies and connects, and makes AlN pottery bonded copper base.
3. the preparation method of AlN pottery bonded copper base according to claim 2, is characterized in that: the thickness of described AlN ceramic substrate is 0.38 ~ 1.0mm; The thickness of described Copper Foil is 0.2 ~ 0.3mm.
4. the preparation method of AlN pottery bonded copper base according to claim 3, is characterized in that: the thickness of described AlN ceramic substrate is 0.63mm; The thickness of described Copper Foil is 0.3mm.
5. the preparation method of AlN pottery bonded copper base according to claim 3, is characterized in that: in step S1, selecting particle diameter is the nanometer Cu below 100 nm
2o, compound thickness of coating is 0.05 ~ 0.15mm.
6. the preparation method of AlN pottery bonded copper base according to claim 5, is characterized in that: in step S1, compound thickness of coating is 0.1mm.
7. the preparation method of AlN pottery bonded copper base according to claim 5, it is characterized in that: the priority described in step S2 is high temperature sintering in the rare gas element of micro-oxygen level and air, refer to and first under the rare gas element Ar of micro-oxygen level guard mode, be sintered to T1 temperature, the insulation t1 time, in air, the temperature rise rate with 1 ~ 1.5 ℃/min is warmed up to T2 temperature from T1 temperature again, the insulation t2 time, wherein T1 is 900 ~ 1000 ℃, the t1 time is 10 ~ 60Min, T2 is 1080 ~ 1100 ℃, the t2 time is 10 ~ 60Min, then in the HCl solution that is 5% in mass concentration, place 10 ~ 60Min.
8. the preparation method of AlN pottery bonded copper base according to claim 7, is characterized in that: described T1 is 1000 ℃, and the t1 time is 40Min, and temperature rise rate is 1 ℃/min, and T2 is 1090 ℃, and the t2 time is 40Min, and pickling time is 40min.
9. the preparation method of AlN pottery bonded copper base according to claim 7, is characterized in that: described step S4 carries out in atmosphere furnace, and protective atmosphere is that purity is greater than or equal to 99.99% N
2, temperature is 1070 ~ 1080 ℃, the time is 5 ~ 20 Min.
10. the preparation method of AlN pottery bonded copper base according to claim 9, is characterized in that: in described step S4, temperature is 1075 ℃, and the time is 15 Min.
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| CN103819214B (en) | 2015-04-01 |
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