CN103819215A - Preparation method of aluminium nitride base ceramic copper-clad plate - Google Patents
Preparation method of aluminium nitride base ceramic copper-clad plate Download PDFInfo
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- CN103819215A CN103819215A CN201410105481.2A CN201410105481A CN103819215A CN 103819215 A CN103819215 A CN 103819215A CN 201410105481 A CN201410105481 A CN 201410105481A CN 103819215 A CN103819215 A CN 103819215A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 84
- 229910017083 AlN Inorganic materials 0.000 title claims abstract description 38
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 63
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 58
- 230000003647 oxidation Effects 0.000 claims abstract description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000011889 copper foil Substances 0.000 claims abstract description 51
- 239000000758 substrate Substances 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 27
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 12
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 11
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 21
- 239000001301 oxygen Substances 0.000 claims description 21
- 229910052760 oxygen Inorganic materials 0.000 claims description 21
- 238000010792 warming Methods 0.000 claims description 15
- 238000002203 pretreatment Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- 229940001516 sodium nitrate Drugs 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 8
- 230000005496 eutectics Effects 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000011800 void material Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 238000005245 sintering Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- -1 oxide compound Chemical class 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910018509 Al—N Inorganic materials 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910018516 Al—O Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000002547 anomalous effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 229960004643 cupric oxide Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of copper-clad plate manufacturing, and particularly relates to a preparation method of an aluminium nitride base ceramic copper-clad plate. The preparation method comprises the following steps: pretreating an oxygen-free red copper foil, then putting the pretreated oxygen-free red copper foil in molten sodium nitrate, and carrying out medium temperature chemical oxidation treatment; pretreating an aluminum nitride substrate, and then carrying out high-temperature oxidation treatment; and carrying out magnetron sputtering treatment on the aluminum nitride substrate subjected to high temperature oxidation, prepressing the treated oxygen-free red copper foil into a circular arc shape, stacking the circular arc-shaped oxygen-free red copper foil and the aluminum nitride substrate together, putting in a chained bonding furnace, carrying out high temperature dynamic continuous bonding, and then treating by adopting a sequential temperature difference alternative falling temperature method, thus obtaining the aluminium nitride base ceramic copper-clad plate. The preparation method is simple in production efficiency, stable in quality and low in cost. The prepared aluminium nitride base ceramic copper-clad plate has the characteristics of low void ratio, low coefficient of thermal expansion, low stress, high thermal conductivity, high peel strength and large bonding area.
Description
Technical field
The invention belongs to copper-clad plate manufacturing technology field, be specifically related to a kind of preparation method of aluminum-nitride-based ceramic copper-clad plate.
Background technology
Along with the high-frequency power electronic devices of efficient, energy-conservation, material-saving, economize on electricity, device are to tradition, poor efficiency, power consumption, the power frequency electric power electron device that takes material, the update of device, the current a large amount of IGBT module of power electronics market demand.Due to igbt chip manufacturing process complexity, need be through tens photoetching processes, thereby can not make single large electric current chip, so multi-chip parallel technology just becomes the technical measures of IGBT module to high current capacity development.This just needs a kind of circuit card that can etch various graphic structures as pcb board to realize circuit parallel connection, to solve heat radiation and the Insulation Problems of IGBT module simultaneously, meet large electric current, high-insulativity, high heat conductance, thermal expansivity and approach the technical requirementss such as silicon, therefore ceramic copper-clad plate has become the high frequency device blocks such as IGBT and has manufactured requisite critical material.Though alumina-based ceramic copper-clad plate can meet above-mentioned basic demand, its thermal conductivity is lower more than 6 times than aluminum-nitride-based ceramic copper-clad plate, and thermal expansivity is larger than aluminum-nitride-based ceramic copper-clad plate.And that aluminum-nitride-based ceramic copper-clad plate not only has higher thermal conductivity, thermal expansivity and silicon is very approaching, and electric property and aluminium sesquioxide ceramic copper-clad plate approach, it is more satisfactory ceramic copper-clad panel material in current new generation of high density, great-power electronic encapsulation.
Because aluminium nitride ceramics belongs to the compound that covalent linkage is stronger, very strong covalent linkage and the extremely strong directivity of covalent linkage between Al-N, makes aluminium nitride ceramics have good chemical stability, is difficult to and Copper Foil and oxide compound generation chemical reaction thereof under high temperature.Cu-Cu
2o eutectic melt is at high temperature poor to the wettability of aluminium nitride ceramics, and the aluminium nitride ceramics that therefore covalency key is stronger can not form Direct Bonding with copper, must have one deck oxide compound phase Al
2o
3as transition layer.
The production technique of existing aluminum-nitride-based ceramic copper-clad plate is that anaerobic red copper foil high temperature oxidation is generated to one deck Cu
2o transition layer, generates one deck Al by aluminium nitride substrate high temperature oxidation
2o
3transition layer, anaerobic red copper foil tiling is overlayed and on aluminum nitride ceramic substrate, puts into tube furnace and carry out static state and sinter aluminum-nitride-based ceramic copper-clad plate into, but the ceramic copper-clad plate area of making is less, generally at 40mm × 40mm.Because be static sintering, can only sintering completely a collection ofly could carrying out second batch sintering, and carry out will waiting temperature, nitrogen oxygen atmosphere flow in boiler tube to recover after processing parameter is stablized several minutes to operate before second batch sintering, so production efficiency is very low.Because be static sintering, the tiling of anaerobic red copper foil to be overlayed on aluminum nitride ceramic substrate and puts into rapidly high temperature from room temperature, in short period of time, temperature head alters a great deal, if aluminium nitride substrate area exceedes 40mm × 40mm, be easy at short notice absorb more heat transfer, cause local sintering not firm, occur delamination or cavitation.Because be that tiling stacks sintering, under high temperature, the laminating of anaerobic red copper foil and aluminum nitride ceramic substrate can be very not tight, and in sintering process, also have gas by clip pack in the middle of bi-material, thereby produce a large amount of empty.
Summary of the invention
The object of this invention is to provide a kind of preparation method of aluminum-nitride-based ceramic copper-clad plate, production efficiency is high, steady quality, cost are low, and the aluminum-nitride-based ceramic copper-clad plate of preparation has the advantages that voidage is low, thermal expansivity is low, stress is low, thermal conductivity is high, stripping strength is high, bonding area is large.
The preparation method of aluminum-nitride-based ceramic copper-clad plate of the present invention, step is as follows:
(1) after the pre-treatment of anaerobic red copper foil, then the SODIUMNITRATE of putting into melting carries out warm chemical oxidation treatment, forms the Cu of one deck even compact at the bonding face of anaerobic red copper foil
2o film;
(2) after aluminium nitride substrate pre-treatment, then pass through high temperature oxidation process, respectively form the Al of one deck even compact on the two sides of aluminium nitride substrate
2o
3film;
(3), to the aluminium nitride substrate magnetron sputtering processing after high temperature oxidation, respectively form the Cu of one deck even compact on two sides
2o film;
(4) by by the arc-shaped anaerobic red copper foil after treatment precompressed, guarantee that convex surface is oxidation aspect, concave surface is non-oxide aspect, oxidation aspect and aluminium nitride substrate are stacked to be placed on and in chain type bonding stove, carry out the dynamically continuous bonding of high temperature;
(5) after bonding, adopt the temperature difference in proper order to replace falling temperature method processing, to obtain final product.
The thickness of the anaerobic red copper foil described in step (1) is 0.1～0.4mm, and length is 35～193mm, and width is 35～145mm.
The temperature of the middle temperature chemical oxidation treatment described in step (1) is 350～370 ℃, and the time is 15～20min.
Anaerobic red copper foil pre-treatment described in step (1) be with four brush roll plate brushing machines carry out 5% dilute sulphuric acid pickling, brush board remove natural oxidizing layer, from the beginning washing, high pressure wash from the beginning, the technique such as ultrasonic wave washed with de-ionized water, hot-air seasoning, then on non-oxide, paste the resistance to 400 ℃ of high temperature gummed tapes of one deck, when preventing that nonbonding face is oxidized and causing bonding, melt on surface.Pretreatment process is conventional steps.
The SODIUMNITRATE that SODIUMNITRATE described in step (1) is SILVER REAGENT, state is the SODIUMNITRATE of 350～370 ℃ of meltings, oxidization time is 15～20min.
Based on the character of SODIUMNITRATE, SODIUMNITRATE can not melting lower than 306 ℃, produces oxygen and easily generates the cupric oxide CuO of black higher than 380 ℃ of decomposition, reacts following 2Cu+O
2→ 2CuO.So determine and generate Cu according to above temperature profile comprehensive test
2350～370 ℃, the reasonable temperature interval of O film, forms Cu
2the chemical process of O film is 2Cu+NaNO
3→ Cu
2o+NaNO
2.
Because aluminium nitride ceramics belongs to the compound that covalent linkage is stronger, very strong covalent linkage and the extremely strong directivity of covalent linkage between Al-N, makes aluminium nitride ceramics have good chemical stability, is difficult to and Copper Foil and oxide compound generation chemical reaction thereof under high temperature.Cu-Cu
2o eutectic melt is at high temperature poor to the wettability of aluminium nitride ceramics, and the aluminium nitride ceramics that therefore covalency key is stronger can not form Direct Bonding with copper, must have one deck oxide compound phase Al
2o
3as transition layer.
The AlN that aluminium nitride substrate described in step (2) is content >=97%, thickness is 0.38～1.0mm, and length is 40～200mm, and width is 40～150mm.
The temperature of the high temperature oxidation process described in step (2) is 1095～1105 ℃, and the time is 200～230min, and oxygen flow is 20～30ml/min, high purity oxygen gas purity >=99.99%.
High temperature oxidation process described in step (2) is that aluminium nitride substrate carries out in high temperature oxidation furnace, and high temperature oxidation burner hearth material is content 99%Al
2o
3, size of burner hearth is φ 350mm × 1500mm.
By to aluminium nitride substrate high temperature oxidation process, can be at the Al of aluminum nitride ceramic substrate Surface Creation one deck densification
2o
3layer, reaction formula is 4AlN+3O
2→ 2Al
2o
3+ 2N
2.
Aluminium nitride substrate pre-treatment described in step (2) is the cleaning of ultrasonic wave acetone, ultrasonic wave washed with de-ionized water, oven dry.Pretreatment process is conventional steps.
Magnetron sputtering processing described in step (3) is that aluminum nitride ceramic substrate is put into JGP-350C type magnetron sputtering equipment (Shenyang scientific instrument limited-liability company of the Chinese Academy of Sciences), sputter target used is high-purity Cu target (purity > 99.99%), diameter is 60mm, thickness 3mm.Distance between target and substrate is 70mm, adopts Ar(purity > 99.999%) be working gas, O
2(purity > 99.999%) is reactant gases.Power is 76W, and air pressure is 1.0Pa, Ar flow 76ml/min～78ml/min, O
2flow 7.6ml/min～7.8ml/min, oxygen partial pressure ratio is 6.6 × 10
-2, depositing time 13min～15min.By magnetron sputtering processing, at the Al of aluminum nitride ceramic substrate Surface Creation
2o
3the Cu of sputter one deck even compact on layer
2o film, can be to Al
2o
3film forms protection and reinforces, and prevents under high temperature nitrogen atmosphere very thin Al
2o
3again there is to react as follows 2Al with nitrogen in film
2o
3+ 2N
2→ 4AlN+3O
2thereby, transition layer Al
2o
3film destroy, produces stripping strength situation not up to standard after causing bonding.
Magnetron sputtering method is in high vacuum, to pour appropriate argon gas, between negative electrode (Style Columu Talget or planar target) and anode (plated film locular wall), apply volts DS, in coating chamber, produce magnet controlled anomalous glow discharge, argon gas is ionized, argon ion is accelerated and bombarding cathode target surface by negative electrode, target material surface atom sputtering is out deposited on and on substrate surface, forms film, by changing the target sputtering time different with control of unlike material, can obtain the coatings of unlike material and different thickness, the bonding force that magnetron sputtering method has coatings and base material is strong, coatings densification, the advantage such as evenly.
Chain type bonding stove described in step (4) is the continuous transmission nitrogen of chain-belt type oxygen atmosphere high temperature eutectic bonding stove.
Bonding temperature described in step (4) is 1070～1078 ℃, and bonding time is 3～7min, and nitrogen oxygen atmosphere flow is 20～40L/min, and oxygen content is 20～100ppm, oxygen purity >=99.99%, nitrogen gas purity >=99.99%.
In the atmosphere bonding process that at high temperature oxygen level is certain, the Cu that copper foil surface chemical oxidation generates
2the Cu of O film and aluminium nitride ceramics surface magnetic control sputtering
2there is Cu-Cu during higher than eutectoid point in temperature in O film
2o eutectic liquid phase, Cu wherein
2o phase and Al
2o
3film has good affinity, and interfacial energy is reduced, and eutectic liquid is on good terms and is soaked well Copper Foil and pottery.Cu in liquid phase simultaneously
2o and Al
2o
3there is chemical reaction and generate CuAlO
2, reaction formula is Al
2o
3+ Cu
2o → CuAlO
2, cooling rear by Cu-Al-O chemical bond, Copper Foil and aluminium nitride ceramics are firmly bonded together.
The temperature difference in proper order described in step (5) replaces falling temperature method, and step is as follows:
(1) the 7min time is cooled to 800 ℃ from bonding temperature;
(2) the 3min time is warming up to 900 ℃ from 800 ℃;
(3) the 7min time is cooled to 600 ℃ from 900 ℃;
(4) the 3min time is warming up to 700 ℃ from 600 ℃;
(5) the 7min time is cooled to 300 ℃ from 700 ℃;
(6) the 3min time is warming up to 400 ℃ from 300 ℃;
(7) the 7min time is cooled to 200 ℃ from 400 ℃;
(8) 3min time naturally cooling from 200 ℃ are cooled to 50 ℃.
After bonding, adopt the temperature difference in proper order to replace falling temperature method to reach elimination matrix material because of the inconsistent stress of thermal expansivity and warpage issues.
The aluminum-nitride-based ceramic copper-clad board parameter that uses technique of the present invention to make, in table 1.
The aluminum-nitride-based ceramic copper-clad board parameter of table 1
The present invention compared with prior art, has following beneficial effect:
(1) Cu obtaining by middle temperature (350 ℃～370 ℃) chemical oxidation treatment
2the Cu that O film obtains than high temperature oxidation
2o film even compact, Cu
2o film thickness is 2 μ m～6 μ m, and maximum benefit is that middle temperature chemical oxidation treatment makes Copper Foil that high temperature annealing reaction not occur, and Copper Foil still presents hard state shape, and this Copper Foil that is circular arc is linear and aluminium nitride substrate and fits tightly that to get rid of bubble highly beneficial.And the Copper Foil of high temperature oxidation is soft state shape, make the Copper Foil of circular arc be difficult to be at high temperature linear and aluminium nitride substrate and fit tightly, cause bonding face to produce large cavity.
(2) aluminium nitride substrate after high temperature oxidation is carried out to magnetron sputtering processing, respectively form the Cu of one deck even compact on two sides
2o film, can be to Al
2o
3film forms protection and reinforces, and prevents under high temperature nitrogen atmosphere very thin Al
2o
3again there is to react as follows 2Al with nitrogen in film
2o
3+ 2N
2→ 4AlN+3O
2thereby, transition layer Al
2o
3film destroy, produces stripping strength situation not up to standard.
(3) existing aluminum-nitride-based ceramic copper-clad plate is because be static sintering, the tiling of anaerobic red copper foil to be overlayed on aluminum nitride ceramic substrate and puts into rapidly high temperature from room temperature, in short period of time, temperature head alters a great deal, if aluminium nitride substrate area exceedes 40mm × 40mm, be easy to absorb at short notice heat more, cause local sintering not firm, occur delamination or cavitation.Bonding of the present invention is dynamically continuous bonding, bonding stove is the continuous transmission nitrogen of chain-belt type oxygen atmosphere high temperature eutectic bonding stove, this bonding mode be a little anaerobic red copper foil tiling overlay on aluminum nitride ceramic substrate from room temperature slowly continuously heat absorption enter high temperature bonding, being unlikely temperature head in the short period of time alters a great deal, be not easy to absorb at short notice more heat transfer, being very easy to so aluminum-nitride-based ceramic copper-clad plate bonding area exceedes 40mm × 40mm, is 200mm × 150mm by the aluminum-nitride-based ceramic copper-clad plate maximum area of explained hereafter of the present invention.
(4) the aluminum-nitride-based ceramic copper-clad plate after bonding adopts " temperature difference replaces falling temperature method in proper order " to eliminate matrix material because of the inconsistent stress of thermal expansivity and warpage issues, warpage≤0.002mm/mm to reach.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
(1) chemical oxidation treatment of Copper Foil
1. anaerobic red copper foil size 193mm × 145mm × 0.2mm, pre-treatment;
2. Copper Foil is put into the SODIUMNITRATE of 350 ℃ of meltings, oxidization time is 20min, forms the Cu of compact and firm at copper foil surface
2o film.
(2) high temperature oxidation of aluminum nitride ceramic substrate
Aluminum nitride ceramic substrate is of a size of 200mm × 150mm × 0.38mm, pre-treatment; Aluminum nitride ceramic substrate is inserted to Al
2o
3in the ceramic grillage of material, push in three station high temperature oxidation boiler tubes and carry out oxide treatment, parameter is as follows: 1095 ℃ of high temperature oxidation temperature, oxygen flow 30ml/min, soaking time 230min.
(3) magnetron sputtering of aluminum nitride ceramic substrate
Radio frequency power 76W, operating pressure is 1.0Pa, Ar flow 78ml/min, O
2flow 7.8ml/min, oxygen partial pressure ratio is 6.5 × 10
-2, depositing time 15min.
(4) the high temperature bonding of aluminum-nitride-based ceramic copper-clad plate
The Copper Foil of chemical oxidation is pressed into circular arc type in advance along length 193mm direction, guarantees action 20mm, guarantee that convex surface is oxidation aspect, concave surface is non-oxide aspect; Copper Foil oxidation aspect and aluminium nitride substrate are stacked to be placed on and in chain type bonding stove, carry out dynamically bonding continuously of high temperature; 1070 ℃ of bonding region temperature, bonding time 7min, nitrogen oxygen atmosphere flow is 40L/min, oxygen content is 100ppm.
(5) aluminum-nitride-based ceramic copper-clad plate adopts " temperature difference replaces falling temperature method in proper order "
1. the 7min time is cooled to 800 ℃ from 1070 ℃ of bonding temperatures;
2. the 3min time is warming up to 900 ℃ from 800 ℃;
3. the 7min time is cooled to 600 ℃ from 900 ℃;
4. the 3min time is warming up to 700 ℃ from 600 ℃;
5. the 7min time is cooled to 300 ℃ from 700 ℃;
6. the 3min time is warming up to 400 ℃ from 300 ℃;
7. the 7min time is cooled to 200 ℃ from 400 ℃;
8. 3min time naturally cooling from 200 ℃ are cooled to 50 ℃.
Embodiment 2
(1) chemical oxidation treatment of Copper Foil
1. anaerobic red copper foil size 193mm × 145mm × 0.3mm, pre-treatment;
2. Copper Foil is put into the SODIUMNITRATE of 360 ℃ of meltings, oxidization time is 18min, forms the Cu of compact and firm at copper foil surface
2o film.
(2) high temperature oxidation of aluminum nitride ceramic substrate
Aluminum nitride ceramic substrate is of a size of 200mm × 150mm × 0.63mm, pre-treatment; Aluminum nitride ceramic substrate is inserted to Al
2o
3in the ceramic grillage of material, push in three station high temperature oxidation boiler tubes and carry out oxide treatment, parameter is as follows: 1100 ℃ of high temperature oxidation temperature, oxygen flow 25ml/min, soaking time 215min.
(3) magnetron sputtering of aluminum nitride ceramic substrate
Radio frequency power 76W, operating pressure is 1.0Pa, Ar flow 77ml/min, O
2flow 7.7ml/min, oxygen partial pressure ratio is 6.5 × 10
-2, depositing time 14min.
(4) the high temperature bonding of aluminum-nitride-based ceramic copper-clad plate
The Copper Foil of chemical oxidation is pressed into circular arc type in advance along length 193mm direction, guarantees action 20mm, guarantee that convex surface is oxidation aspect, concave surface is non-oxide aspect; Copper Foil oxidation aspect and aluminium nitride substrate are stacked to be placed on and in chain type bonding stove, carry out dynamically bonding continuously of high temperature; 1075 ℃ of bonding region temperature, bonding time 5min, nitrogen oxygen atmosphere flow is 30L/min, oxygen content is 60ppm.
(5) aluminum-nitride-based ceramic copper-clad plate adopts " temperature difference replaces falling temperature method in proper order "
1. the 7min time is cooled to 800 ℃ from 1075 ℃ of bonding temperatures;
2. the 3min time is warming up to 900 ℃ from 800 ℃;
3. the 7min time is cooled to 600 ℃ from 900 ℃;
4. the 3min time is warming up to 700 ℃ from 600 ℃;
5. the 7min time is cooled to 300 ℃ from 700 ℃;
6. the 3min time is warming up to 400 ℃ from 300 ℃;
7. the 7min time is cooled to 200 ℃ from 400 ℃;
8. 3min time naturally cooling from 200 ℃ are cooled to 50 ℃.
Embodiment 3
(1) chemical oxidation treatment of Copper Foil
1. anaerobic red copper foil size 193mm × 145mm × 0.35mm, pre-treatment;
2. Copper Foil is put into the SODIUMNITRATE of 370 ℃ of meltings, oxidization time is 15min, forms the Cu of compact and firm at copper foil surface
2o film.
(2) high temperature oxidation of aluminum nitride ceramic substrate
Aluminum nitride ceramic substrate is of a size of 200mm × 150mm × 1.0mm, pre-treatment; Aluminum nitride ceramic substrate is inserted to Al
2o
3in the ceramic grillage of material, push in three station high temperature oxidation boiler tubes and carry out oxide treatment, parameter is as follows: 1105 ℃ of high temperature oxidation temperature, oxygen flow 20ml/min, soaking time 200min.
(3) magnetron sputtering of aluminum nitride ceramic substrate
Radio frequency power 76W, Ar flow 76ml/min, O
2flow 7.6ml/min, oxygen partial pressure ratio is 6.5 × 10
-2, depositing time 13min.
(4) the high temperature bonding of aluminum-nitride-based ceramic copper-clad plate
The Copper Foil of chemical oxidation is pressed into circular arc type in advance along length 193mm direction, guarantees action 20mm, guarantee that convex surface is oxidation aspect, concave surface is non-oxide aspect; Copper Foil oxidation aspect and aluminium nitride substrate are stacked to be placed on and in chain type bonding stove, carry out dynamically bonding continuously of high temperature; 1078 ℃ of bonding region temperature, bonding time 3min, nitrogen oxygen atmosphere flow is 20L/min, oxygen content is 20ppm.
(5) aluminum-nitride-based ceramic copper-clad plate adopts " temperature difference replaces falling temperature method in proper order "
1. the 7min time is cooled to 800 ℃ from 1078 ℃ of bonding temperatures;
2. the 3min time is warming up to 900 ℃ from 800 ℃;
3. the 7min time is cooled to 600 ℃ from 900 ℃;
4. the 3min time is warming up to 700 ℃ from 600 ℃;
5. the 7min time is cooled to 300 ℃ from 700 ℃;
6. the 3min time is warming up to 400 ℃ from 300 ℃;
7. the 7min time is cooled to 200 ℃ from 400 ℃;
8. 3min time naturally cooling from 200 ℃ are cooled to 50 ℃.
Comparative example 1
This comparative example is used for illustrating aluminum-nitride-based ceramic copper-clad plate of the prior art.
Adopt common process to prepare aluminum-nitride-based ceramic copper-clad plate, concrete grammar is:
(1) high temperature oxidation of Copper Foil
Copper Foil is put into three station Al
2o
3in the ceramic boiler tube of material, carry out oxide treatment, parameter is as follows: 750 ℃ of temperature, under the nitrogen atmosphere that is 450ppm at oxygen content, carry out high temperature oxidation, and gas flow is 300ml/min, soaking time 10min, copper foil surface obtains Cu
2o film.
(2) high temperature oxidation of aluminum nitride ceramic substrate
Aluminum nitride ceramic substrate is of a size of 200mm × 150mm × 0.63mm, and aluminum nitride ceramic substrate is inserted to Al
2o
3in the ceramic grillage of material, push in three station high temperature oxidation boiler tubes and carry out oxide treatment, parameter is as follows: 1098 ℃ of high temperature oxidation temperature, oxygen flow 25ml/min, soaking time 230min.
(3) the high temperature bonding of aluminum-nitride-based ceramic copper-clad plate
The tiling of the Copper Foil of high temperature oxidation and aluminum nitride ceramic substrate is stacked together to be placed in bonding stove and carries out static state high-temperature bonding, 1075 ℃ of bonding region temperature, bonding time 5min, nitrogen oxygen atmosphere flow is 30L/min, oxygen content is 60ppm.
The aluminum-nitride-based ceramic copper-clad plate that the aluminum-nitride-based ceramic copper-clad plate that above-described embodiment 1～3 is made and comparative example 1 are made carries out voidage, stripping strength, thermal conductivity, dielectric strength properties test.
The test result obtaining, in table 2.
Table 2 test result
| Quality index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 |
| Voidage (%) | 0.97 | 0.92 | 0.95 | 3.16 |
| Stripping strength (N/mm) | 8.6 | 8.9 | 8.3 | 4.3 |
| Thermal conductivity (W/mK) | 183 | 181 | 182 | 169 |
| Dielectric strength (kV/mm) | 15.2 | 15.5 | 15.1 | 15.2 |
Can find out from the test result of table 2, the prior art of comparing, thermal conductivity, the stripping strength of aluminum-nitride-based ceramic copper-clad plate of the present invention are improved, and voidage has obtained decline.
Claims (8)
1. a preparation method for aluminum-nitride-based ceramic copper-clad plate, is characterized in that step is as follows:
(1) after the pre-treatment of anaerobic red copper foil, then the SODIUMNITRATE of putting into melting carries out warm chemical oxidation treatment, forms the Cu of one deck even compact at the bonding face of anaerobic red copper foil
2o film;
(2) after aluminium nitride substrate pre-treatment, then pass through high temperature oxidation process, respectively form the Al of one deck even compact on the two sides of aluminium nitride substrate
2o
3film;
(3), to the aluminium nitride substrate magnetron sputtering processing after high temperature oxidation, respectively form the Cu of one deck even compact on two sides
2o film;
(4), by by the arc-shaped anaerobic red copper foil after treatment precompressed, be stacked to be placed on aluminium nitride substrate and in chain type bonding stove, carry out dynamically bonding continuously of high temperature;
(5) after bonding, adopt the temperature difference in proper order to replace falling temperature method processing, to obtain final product.
2. the preparation method of aluminum-nitride-based ceramic copper-clad plate according to claim 1, the thickness that it is characterized in that the anaerobic red copper foil described in step (1) is 0.1～0.4mm, and length is 35～193mm, and width is 35～145mm.
3. the preparation method of aluminum-nitride-based ceramic copper-clad plate according to claim 1, the temperature that it is characterized in that the middle temperature chemical oxidation treatment described in step (1) is 350～370 ℃, the time is 15～20min.
4. the preparation method of aluminum-nitride-based ceramic copper-clad plate according to claim 1, is characterized in that the AlN that the aluminium nitride substrate described in step (2) is content >=97%, and thickness is 0.38～1.0mm, and length is 40～200mm, and width is 40～150mm.
5. the preparation method of aluminum-nitride-based ceramic copper-clad plate according to claim 1, the temperature that it is characterized in that the high temperature oxidation process described in step (2) is 1095～1105 ℃, the time is 200～230min.
6. the preparation method of aluminum-nitride-based ceramic copper-clad plate according to claim 1, is characterized in that the chain type bonding stove described in step (4) is the continuous transmission nitrogen of chain-belt type oxygen atmosphere high temperature eutectic bonding stove.
7. the preparation method of aluminum-nitride-based ceramic copper-clad plate according to claim 1, is characterized in that the bonding temperature described in step (4) is 1070～1078 ℃, and bonding time is 3～7min.
8. the preparation method of aluminum-nitride-based ceramic copper-clad plate according to claim 1, is characterized in that the temperature difference in proper order described in step (5) replaces falling temperature method, and step is as follows:
(1) the 7min time is cooled to 800 ℃ from bonding temperature;
(2) the 3min time is warming up to 900 ℃ from 800 ℃;
(3) the 7min time is cooled to 600 ℃ from 900 ℃;
(4) the 3min time is warming up to 700 ℃ from 600 ℃;
(5) the 7min time is cooled to 300 ℃ from 700 ℃;
(6) the 3min time is warming up to 400 ℃ from 300 ℃;
(7) the 7min time is cooled to 200 ℃ from 400 ℃;
(8) 3min time naturally cooling from 200 ℃ are cooled to 50 ℃.
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