CN109336646A - A kind of manufacturing method for covering copper aluminum nitride ceramic substrate - Google Patents
A kind of manufacturing method for covering copper aluminum nitride ceramic substrate Download PDFInfo
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- CN109336646A CN109336646A CN201811451009.9A CN201811451009A CN109336646A CN 109336646 A CN109336646 A CN 109336646A CN 201811451009 A CN201811451009 A CN 201811451009A CN 109336646 A CN109336646 A CN 109336646A
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
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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
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The present invention relates to a kind of manufacturing methods for covering copper aluminum nitride ceramic substrate, comprising the following steps: (1) preparation of spot corrosion solution；(2) dirty removing processing；(3) ungrease treatment；(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasonic technique；(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is mixed by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate；(6) it is heat-treated；(7) nickel plating；(8) vacuum expands weldering.The present invention solves the problems such as existing copper foil and aluminum nitride ceramic substrate binding force are insufficient, hole ratio is high, peel strength is low, by reducing hole ratio between the two, improves the binding force of the two, the intensity of copper aluminum nitride ceramic substrate is covered in enhancing.
Description
Technical field
The present invention relates to ceramic substrate metallization technology field more particularly to a kind of manufactures for covering copper aluminum nitride ceramic substrate
Method.
Background technique
With the development of generation information technology, along with the reduction of the raising and volume that are integration degree, so that single
Power consumption on the heat dissipation area of position increases, thus the critical issue become in modular manufacture that radiates, and covers copper aluminium nitride ceramics
Substrate, also with the high thermal conductivity characteristic of aluminium nitride ceramics, can meet above-mentioned heat dissipation and want other than the highly conductive characteristic with copper foil
It asks.
Specifically, it covers copper aluminum nitride ceramic substrate and refers to that copper foil is bonded directly at high temperature on aluminium nitride ceramic substrate surface
Special process plate.Made ultra-thin composite substrate has good electrical insulation performance, high thermal conductivity characteristic, excellent solderability
With high adhesive strength, and various figures can be etched as pcb board, there is very big current-carrying capability, be integrated circuit
A kind of widely used substrate in field.
Currently, there are mainly two types of the manufacturing methods of ceramic base copper-clad plate: (1) Direct Bonding copper technology (DBC)；(2) directly
It plates copper technology (DPC).
DBC is by Al2O3Or after the single or double of AlN ceramic is covered with Cu plate, via 1065-1085 DEG C of high temperature
Environment heating makes Cu plate surface because of high-temperature oxydation, expands weldering and Al2O3Substrate generates Cu-Cu2O eutectic phase, makes copper sheet and ceramic base
Plate bonding, forms ceramic base copper-clad plate.DBC requires the control of technological temperature very harsh, it is necessary to extremely stable in temperature
Under 1065-1085 DEG C of temperature range, it can just make layers of copper surface melting eutectic phase, realization is combined closely with ceramic substrate,
Manufacturing cost is high and is not easy to solve Al2O3Existing micro- stomata or the problems such as hole between Cu plate, influences the intensity of product, in turn
So that the performance of product is by extreme influence, meanwhile, reaction temperature is higher, and cause equipment and process conditions more difficult to control, thus
So that the performance of product obtained is affected.
Such as Chinese patent application 200710195406.X(application number: on November 27th, 2007) it discloses a kind of ceramics and covers
The manufacturing method of copper base, this method, which is included under oxidizing atmosphere, heats aluminium nitride ceramics, later in inert gas gas
Aluminium nitride ceramics combination interface in conjunction with the combination interface of copper foil and is subjected to eutectic soldering under atmosphere, wherein this method further includes
After being heated aluminium nitride ceramics under oxidizing atmosphere, in the combination interface of aluminium nitride ceramics and/or the combination interface of copper foil
Upper coating cuprous oxide.This method heating temperature is 1150-1300 DEG C, and heating temperature is larger, is difficult to control, and excessively high heating
Temperature will cause Al2O3The micro- stomata or hole generated between Cu plate, meanwhile, this method will cause Cu by way of coating2O
Particle is not uniform enough in copper foil surface distribution, and arrangement is also not fine and close enough, causes to apply the dispersibility and poor repeatability connect；Secondly, applying
It covers thickness to be difficult to control, the Cu2O layer of coating is too thick or too thin, can all reduce to apply connecing intensity；In addition, the Cu of coating2O will cause
The pollution of environment.
And DPC is a kind of vacuum coating and the combined copper-clad plate manufacturing technology of electroplating technology, principle is first
Using vacuum coating technology in Al2O3Or one layer of copper film is deposited in AlN ceramic, then carry out thickening for copper film with electroplating technology.
The technological temperature of DPC is generally below 400 DEG C, avoids the phenomenon that high temperature is for destruction caused by material or size variation.DPC
Ceramic base copper-clad plate has the advantages that high heat dissipation, high-reliability, high accurancy and precision and manufacturing cost are low etc..DPC ceramic base copper-clad plate
The metallic circuit resolution upper limit is about between 10-50um (using depth-to-width ratio 1:1 as standard), it might even be possible to and it is thinner, and surfacing
Degree is high, therefore is very suitable for that the flip of elevated track precision and high-flatness/eutectic technology is required to use.But use plating
On the one hand technology will cause the pollution of environment, be not on the other hand very by the binding force of the copper film and ceramic substrate that plate
By force, and in electroplating process micro- stomata or hole can be generated.
Based on this, it is necessary to a kind of manufacturing method for covering copper aluminum nitride ceramic substrate is provided, to solve to deposit in the prior art
The problem of.
Summary of the invention
The object of the present invention is to provide a kind of manufacturing methods for covering copper aluminum nitride ceramic substrate, to solve existing copper foil and nitrogen
Change the problems such as aluminium ceramic substrate binding force is insufficient, hole ratio is high, peel strength is low, by reducing hole ratio between the two, mentions
The intensity of copper aluminum nitride ceramic substrate is covered in both high binding force, enhancing.
The present invention is achieved by the following technical solutions:
A kind of manufacturing method for covering copper aluminum nitride ceramic substrate, comprising the following steps:
(1) preparation of spot corrosion solution: spot corrosion solution is mixed by sodium sulphate, sulfuric acid, sustained release agent and additive, wherein sustained release agent
By any or both mixing of ethylene glycol, glycerol, additive is any or both mixing of oxalic acid, EDTA, by selection
Reagent is dissolved in deionized water in proportion, and is stirred under the conditions of 50 DEG C, mixing speed 500-600rpm, and 40-60min is stirred
It filters afterwards and spot corrosion solution is made；
(2) dirty removing processing: aluminum nitride ceramic substrate is immersed except being cleaned in oil solution with ultrasonic cleaning technique, aluminium nitride is removed
The dirt of ceramic base plate surface under sodium sulphate effect, and washes down its surface with deionized water；
(3) ungrease treatment: aluminum nitride ceramic substrate is immersed in degreasant solution, is cleaned with ultrasonic cleaning process, degreasing 5-
It takes out after 10min, is rinsed 4-6 times with deionized water；
(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasound
Technique forms concave point on aluminum nitride ceramic substrate surface under sodium sulphate effect, and taking-up is washed down with deionized water, cold wind drying；
(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is by copper sulphate, sodium peroxydisulfate, boron
Acid and potassium citrate mix, and the aluminum nitride ceramic substrate for being coated with activator is placed in activation furnace and is activated；
(6) it is heat-treated: the aluminum nitride ceramic substrate after spot corrosion being placed in vacuum furnace again, temperature is first risen into 180-220
2-3h is kept the temperature after DEG C, keeps the temperature 1.5-2h after then rising to 250-300 DEG C；
(7) nickel plating: the aluminum nitride ceramic substrate after heat treatment is placed in a vacuum chamber, and by N2By opening in the chamber
Dynamic sputter nickel target forms ion beam and splashes, and the nickle atom splashed out volatilizees to form plasmoid and be adsorbed and be deposited on
On the active faying face of ceramic substrate, nickel plating aluminum nitride ceramic substrate is formed；
(8) vacuum expands weldering: nickel plating aluminum nitride ceramic substrate plate is bonded with the copper foil position to be welded after cleaning with relative fashion,
It is subsequently placed in vacuum to expand in brazier, closes vacuum chamber, open pumped vacuum systems, open heating system, vacuum is expanded into brazier temperature
It is warming up to 650-750 DEG C, before heat preservation starts, applies the pressure of 4-6MPa to the material after fitting, is then 650- in temperature
At 750 DEG C and pressure is keeps the temperature 25-35min under conditions of 4-6MPa, and unloading pressure after heat preservation is cooled to room temperature with furnace temperature, is done
It is dry, it obtains covering copper aluminum nitride ceramic substrate.
Preferably, in the step (1), include sodium sulphate 150-200g in every 1L spot corrosion solution, sulfuric acid 30-50ml, delay
Agent 20-30g, additive 5-10g are released, remaining is water.
Preferably, the oil solution that removes in the step (2) is acid except vinegar liquid, solubility 120-160g/L, ultrasonic power
For 130-160W, sonication treatment time 25-35min.
Preferably, in the step (3), every 1L degreasing agent includes acid degreasing agent 80-120ml, sulfuric acid 150-250ml,
Remaining is water.
Preferably, the ultrasonic frequency in the step (3) is 50-70KHz, and the processing time is 30-50min.
Preferably, the activator in the step (5) by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate in mass ratio
5:3:2:1 is mixed.
Preferably, the specific steps that the step (5) is activated are as follows:
(1) pre-activate: the aluminum nitride ceramic substrate for being coated with activator will be placed in activation furnace, in 2 atmosphere of high-purity N, with 10
DEG C/heating rate of min is warming up to 150 DEG C, temperature 1.5h is kept the temperature, pre-activate aluminum nitride ceramic substrate is obtained；
(2) low-temperature activation in: the pre-activate aluminum nitride ceramic substrate of step (1) is continued to heat up, and is warming up to 250 with 15 DEG C/min
DEG C, 1.0h is kept the temperature, middle low-temperature activation aluminum nitride ceramic substrate is obtained；
(3) high-temperature activation: step (2) aluminum nitride ceramic substrate is continued to heat up, and is warming up to 380 DEG C with 20 DEG C/min, heat preservation temperature
0.5h to get surface active aluminum nitride ceramic substrate.
Preferably, the energy beam in the step (7) is to be carried out at activity using gas ion source to ceramic base plate surface
Reason, and the ion beam energy 10 of ion beam irradiation-2-10-4eV。
Preferably, in the step (7) when starting sputter nickel target, need to by ceramic substrate back bias voltage -380~-
450Volt, and the current density of target is controlled in 0.3-0.5W/cm2, carry out bombardment by ions and be implanted into the time 5- of target
7min。
Preferably, the vacuum degree in the step (7) is not less than 4.0 × 10-3Pa。
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, the present invention solves existing copper foil and aluminum nitride ceramic substrate binding force is insufficient, by reducing voidage between the two,
The binding force of the two is improved, the intensity of copper aluminum nitride ceramic substrate is covered in enhancing；
2, the present invention first carries out dirt, degreasing and spot corrosion to ceramic substrate and handles before being activated to ceramic substrate,
To improve the activity of ceramic substrate Yu copper foil faying face, and then improve and the binding force of copper foil, specifically: by dirt,
Influence of the ceramic base plate surface dust to ceramics and copper foil binding force can be eliminated；And ungrease treatment then makes the surface of ceramic substrate
While becoming smooth, become uniformity, then improve with copper foil binding force, and air gap between ceramic substrate and copper foil can be reduced
Rate, to improve the intensity for covering copper aluminum nitride ceramic substrate；And the spot corrosion processing carried out can be in aluminum nitride ceramic substrate surface shape
At concave point, to increase copper foil and ceramic substrate contact area, the binding force of ceramic substrate and copper foil is improved, while concave point is arranged
The copper foil entered in concave point can be made to be formed and be similar to " fixed column ", and then improve its peel strength；
3, the present invention is by coating activator in ceramic base plate surface, and carries out and carry out in vacuum furnace pre- in activation furnace
Activation, middle low-temperature activation and high-temperature activation, carry out the activation processing for having gradient, so that copper sulphate, sodium peroxydisulfate in activator,
Boric acid and potassium citrate can be sufficiently submerged in ceramic base plate surface, and form high infiltration, high activity in ceramic base plate surface
Active membrane layer, the film layer have preferable affinity and cohesive force, and the removing that the present invention covers copper aluminum nitride ceramic substrate can be improved
Intensity, and achieve the purpose that reduce voidage；
4, heat treatment of the invention, and it is divided to two sections of progress, the activity of ceramic substrate is on the one hand improved, consequent activities faying face is conducive to
Formation, on the other hand, by Fractional Heat-treatment, the stress inside ceramic substrate can be eliminated, reduced since ceramic substrate is answered
Power covers copper aluminum nitride ceramic substrate intensity decline problem caused by changing；
5, the present invention can further improve the binding force of ceramic substrate and copper foil, have by depositing nickel element in active faying face
Body are as follows: on the active faying face that uniform adsorption is deposited on ceramic substrate and nickle atom is become plasmoid, thus
The binding force that nickel element and ceramic substrate faying face have is improved, meanwhile, nickel element and copper foil have preferable affinity, the two
Between can form Cu-Ni graft, to improve the binding force of ceramic substrate and copper foil；
6, the present invention expands weldering welding by using vacuum, can eliminate the generation of phase transformation in welding process, covers copper nitrogen to eliminate
Change the stress of aluminium ceramic substrate inner wall, and reduce the porosity of ceramic copper-clad base plate, improves the intensity of ceramic copper-clad base plate；
7, manufacturing method of the present invention is reproducible, cost is relatively low, good heat dispersion performance, and the present invention meets the big of specialities requirement
Electric current passes through, and product has broad application prospects in encapsulation fields such as integrated circuits.
Detailed description of the invention
Fig. 1 is the flow chart for the manufacturing method that the present invention covers copper aluminum nitride ceramic substrate.
Specific embodiment
Below by specific embodiment, the present invention is further described, it is noted that for the ordinary skill of this field
For personnel, without departing from the principle of the present invention, several variations and modifications can also be made, these also should be regarded as belonging to
Protection scope of the present invention.
Embodiment 1
The manufacturing method for covering copper aluminum nitride ceramic substrate of the present embodiment, comprising the following steps:
(1) preparation of spot corrosion solution: spot corrosion solution is mixed by sodium sulphate, sulfuric acid, sustained release agent and additive, wherein sustained release agent
By any or both mixing of ethylene glycol, glycerol, additive is any or both mixing of oxalic acid, EDTA, by selection
Reagent is dissolved in deionized water in proportion, and is stirred under the conditions of 50 DEG C, mixing speed 500rpm, is filtered after stirring 40min
Spot corrosion solution is made；
(2) dirty removing processing: aluminum nitride ceramic substrate is immersed except being cleaned in oil solution with ultrasonic cleaning technique, aluminium nitride is removed
The dirt of ceramic base plate surface under sodium sulphate effect, and washes down its surface with deionized water；
(3) ungrease treatment: aluminum nitride ceramic substrate is immersed in degreasant solution, is cleaned with ultrasonic cleaning process, degreasing 5min
After take out, with deionized water rinse 4-6 times；
(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasound
Technique forms concave point on aluminum nitride ceramic substrate surface under sodium sulphate effect, and taking-up is washed down with deionized water, cold wind drying；
(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is by copper sulphate, sodium peroxydisulfate, boron
Acid and potassium citrate mix, and the aluminum nitride ceramic substrate for being coated with activator is placed in activation furnace and is activated；
(6) it is heat-treated: the aluminum nitride ceramic substrate after spot corrosion being placed in vacuum furnace again, after temperature is first risen to 180 DEG C
2h is kept the temperature, keeps the temperature 1.5h after then rising to 250 DEG C；
(7) nickel plating: the aluminum nitride ceramic substrate after heat treatment is placed in a vacuum chamber, and by N2By opening in the chamber
Dynamic sputter nickel target forms ion beam and splashes, and the nickle atom splashed out volatilizees to form plasmoid and be adsorbed and be deposited on
On the active faying face of ceramic substrate, nickel plating aluminum nitride ceramic substrate is formed；
(8) vacuum expands weldering: nickel plating aluminum nitride ceramic substrate plate is bonded with the copper foil position to be welded after cleaning with relative fashion,
It is subsequently placed in vacuum to expand in brazier, closes vacuum chamber, open pumped vacuum systems, open heating system, vacuum is expanded into brazier temperature
650 DEG C are warming up to, before heat preservation starts, applies the pressure of 4MPa to the material after fitting, at being then 650 DEG C in temperature and is pressed
Under conditions of power is 4MPa, 25min is kept the temperature, unloading pressure after heat preservation is cooled to room temperature with furnace temperature, and it is dry, it obtains covering copper nitridation
Aluminium ceramic substrate.
Wherein, in the step (1), include sodium sulphate 150g in every 1L spot corrosion solution, sulfuric acid 30ml, sustained release agent 20g, add
Add agent 5g, remaining is water.
Wherein, in the step (2) except oil solution be it is acid remove vinegar liquid, solubility 120g/L, ultrasonic power 130W,
Sonication treatment time is 25min.
Wherein, in the step (3), every 1L degreasing agent includes acid degreasing agent 80ml, sulfuric acid 150ml, remaining is water.
Wherein, the ultrasonic frequency in the step (3) is 50KHz, and the processing time is 30min.
Wherein, the activator in the step (5) is by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate in mass ratio 5:
3:2:1 is mixed.
Wherein, the specific steps that the step (5) is activated are as follows:
(1) pre-activate: the aluminum nitride ceramic substrate for being coated with activator will be placed in activation furnace, in 2 atmosphere of high-purity N, with 10
DEG C/heating rate of min is warming up to 150 DEG C, temperature 1.5h is kept the temperature, pre-activate aluminum nitride ceramic substrate is obtained；
(2) low-temperature activation in: the pre-activate aluminum nitride ceramic substrate of step (1) is continued to heat up, and is warming up to 250 with 15 DEG C/min
DEG C, 1.0h is kept the temperature, middle low-temperature activation aluminum nitride ceramic substrate is obtained；
(3) high-temperature activation: step (2) aluminum nitride ceramic substrate is continued to heat up, and is warming up to 380 DEG C with 20 DEG C/min, heat preservation temperature
0.5h to get surface active aluminum nitride ceramic substrate.
Wherein, the energy beam in the step (7) is to carry out active processing to ceramic base plate surface using gas ion source,
And the ion beam energy 10 of ion beam irradiation-2eV。
Wherein, need to be by ceramic substrate back bias voltage in -380Volt in the step (7) when starting sputter nickel target, and control
The current density of target processed is in 0.3W/cm2, carry out bombardment by ions and be implanted into the time 5min of target.
Wherein, the vacuum degree in the step (7) is not less than 4.0 × 10-3Pa。
Embodiment 2
The manufacturing method for covering copper aluminum nitride ceramic substrate of the present embodiment, comprising the following steps:
(1) preparation of spot corrosion solution: spot corrosion solution is mixed by sodium sulphate, sulfuric acid, sustained release agent and additive, wherein sustained release agent
By any or both mixing of ethylene glycol, glycerol, additive is any or both mixing of oxalic acid, EDTA, by selection
Reagent is dissolved in deionized water in proportion, and is stirred under the conditions of 50 DEG C, mixing speed 600rpm, is filtered after stirring 60min
Spot corrosion solution is made；
(2) dirty removing processing: aluminum nitride ceramic substrate is immersed except being cleaned in oil solution with ultrasonic cleaning technique, aluminium nitride is removed
The dirt of ceramic base plate surface under sodium sulphate effect, and washes down its surface with deionized water；
(3) ungrease treatment: aluminum nitride ceramic substrate is immersed in degreasant solution, is cleaned with ultrasonic cleaning process, degreasing 10min
After take out, with deionized water rinse 4-6 times；
(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasound
Technique forms concave point on aluminum nitride ceramic substrate surface under sodium sulphate effect, and taking-up is washed down with deionized water, cold wind drying；
(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is by copper sulphate, sodium peroxydisulfate, boron
Acid and potassium citrate mix, and the aluminum nitride ceramic substrate for being coated with activator is placed in activation furnace and is activated；
(6) it is heat-treated: the aluminum nitride ceramic substrate after spot corrosion being placed in vacuum furnace again, after temperature is first risen to 220 DEG C
3h is kept the temperature, keeps the temperature 2h after then rising to 300 DEG C；
(7) nickel plating: the aluminum nitride ceramic substrate after heat treatment is placed in a vacuum chamber, and by N2By opening in the chamber
Dynamic sputter nickel target forms ion beam and splashes, and the nickle atom splashed out volatilizees to form plasmoid and be adsorbed and be deposited on
On the active faying face of ceramic substrate, nickel plating aluminum nitride ceramic substrate is formed；
(8) vacuum expands weldering: nickel plating aluminum nitride ceramic substrate plate is bonded with the copper foil position to be welded after cleaning with relative fashion,
It is subsequently placed in vacuum to expand in brazier, closes vacuum chamber, open pumped vacuum systems, open heating system, vacuum is expanded into brazier temperature
750 DEG C are warming up to, before heat preservation starts, applies the pressure of 6MPa to the material after fitting, at being then 750 DEG C in temperature and is pressed
Under conditions of power is 6MPa, 35min is kept the temperature, unloading pressure after heat preservation is cooled to room temperature with furnace temperature, and it is dry, it obtains covering copper nitridation
Aluminium ceramic substrate.
Wherein, in the step (1), include sodium sulphate 200g in every 1L spot corrosion solution, sulfuric acid 50ml, sustained release agent 30g, add
Add agent 10g, remaining is water.
Wherein, in the step (2) except oil solution be it is acid remove vinegar liquid, solubility 160g/L, ultrasonic power 160W,
Sonication treatment time is 35min.
Wherein, in the step (3), every 1L degreasing agent includes acid degreasing agent 120ml, sulfuric acid 250ml, remaining is water.
Wherein, the ultrasonic frequency in the step (3) is 70KHz, and the processing time is 50min.
Wherein, the activator in the step (5) is by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate in mass ratio 5:
3:2:1 is mixed.
Wherein, the specific steps that the step (5) is activated are as follows:
(1) pre-activate: the aluminum nitride ceramic substrate for being coated with activator will be placed in activation furnace, in 2 atmosphere of high-purity N, with 10
DEG C/heating rate of min is warming up to 150 DEG C, temperature 1.5h is kept the temperature, pre-activate aluminum nitride ceramic substrate is obtained；
(2) low-temperature activation in: the pre-activate aluminum nitride ceramic substrate of step (1) is continued to heat up, and is warming up to 250 with 15 DEG C/min
DEG C, 1.0h is kept the temperature, middle low-temperature activation aluminum nitride ceramic substrate is obtained；
(3) high-temperature activation: step (2) aluminum nitride ceramic substrate is continued to heat up, and is warming up to 380 DEG C with 20 DEG C/min, heat preservation temperature
0.5h to get surface active aluminum nitride ceramic substrate.
Wherein, the energy beam in the step (7) is to carry out active processing to ceramic base plate surface using gas ion source,
And the ion beam energy 10 of ion beam irradiation-4eV。
Wherein, need to be by ceramic substrate back bias voltage in -450Volt in the step (7) when starting sputter nickel target, and control
The current density of target processed is in 0.5W/cm2, carry out bombardment by ions and be implanted into the time 7min of target.
Wherein, the vacuum degree in the step (7) is not less than 4.0 × 10-3Pa。
Embodiment 3
The manufacturing method for covering copper aluminum nitride ceramic substrate of the present embodiment, comprising the following steps:
(1) preparation of spot corrosion solution: spot corrosion solution is mixed by sodium sulphate, sulfuric acid, sustained release agent and additive, wherein sustained release agent
By any or both mixing of ethylene glycol, glycerol, additive is any or both mixing of oxalic acid, EDTA, by selection
Reagent is dissolved in deionized water in proportion, and is stirred under the conditions of 50 DEG C, mixing speed 550rpm, is filtered after stirring 50min
Spot corrosion solution is made；
(2) dirty removing processing: aluminum nitride ceramic substrate is immersed except being cleaned in oil solution with ultrasonic cleaning technique, aluminium nitride is removed
The dirt of ceramic base plate surface under sodium sulphate effect, and washes down its surface with deionized water；
(3) ungrease treatment: aluminum nitride ceramic substrate is immersed in degreasant solution, is cleaned with ultrasonic cleaning process, degreasing
It takes out after 7.5min, is rinsed 4-6 times with deionized water；
(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasound
Technique forms concave point on aluminum nitride ceramic substrate surface under sodium sulphate effect, and taking-up is washed down with deionized water, cold wind drying；
(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is by copper sulphate, sodium peroxydisulfate, boron
Acid and potassium citrate mix, and the aluminum nitride ceramic substrate for being coated with activator is placed in activation furnace and is activated；
(6) it is heat-treated: the aluminum nitride ceramic substrate after spot corrosion being placed in vacuum furnace again, after temperature is first risen to 200 DEG C
2.5h is kept the temperature, keeps the temperature 1.8h after then rising to 280 DEG C；
(7) nickel plating: the aluminum nitride ceramic substrate after heat treatment is placed in a vacuum chamber, and by N2By opening in the chamber
Dynamic sputter nickel target forms ion beam and splashes, and the nickle atom splashed out volatilizees to form plasmoid and be adsorbed and be deposited on
On the active faying face of ceramic substrate, nickel plating aluminum nitride ceramic substrate is formed；
(8) vacuum expands weldering: nickel plating aluminum nitride ceramic substrate plate is bonded with the copper foil position to be welded after cleaning with relative fashion,
It is subsequently placed in vacuum to expand in brazier, closes vacuum chamber, open pumped vacuum systems, open heating system, vacuum is expanded into brazier temperature
700 DEG C are warming up to, before heat preservation starts, applies the pressure of 5MPa to the material after fitting, at being then 700 DEG C in temperature and is pressed
Under conditions of power is 5MPa, 30min is kept the temperature, unloading pressure after heat preservation is cooled to room temperature with furnace temperature, and it is dry, it obtains covering copper nitridation
Aluminium ceramic substrate.
Wherein, in the step (1), include sodium sulphate 180g in every 1L spot corrosion solution, sulfuric acid 40ml, sustained release agent 25g, add
Add agent 7.5g, remaining is water.
Wherein, in the step (2) except oil solution be it is acid remove vinegar liquid, solubility 140g/L, ultrasonic power 145W,
Sonication treatment time is 30min.
Wherein, in the step (3), every 1L degreasing agent includes acid degreasing agent 80-120ml, sulfuric acid 200ml, remaining is
Water.
Wherein, the ultrasonic frequency in the step (3) is 60KHz, and the processing time is 40min.
Wherein, the activator in the step (5) is by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate in mass ratio 5:
3:2:1 is mixed.
Wherein, the specific steps that the step (5) is activated are as follows:
(1) pre-activate: the aluminum nitride ceramic substrate for being coated with activator will be placed in activation furnace, in 2 atmosphere of high-purity N, with 10
DEG C/heating rate of min is warming up to 150 DEG C, temperature 1.5h is kept the temperature, pre-activate aluminum nitride ceramic substrate is obtained；
(2) low-temperature activation in: the pre-activate aluminum nitride ceramic substrate of step (1) is continued to heat up, and is warming up to 250 with 15 DEG C/min
DEG C, 1.0h is kept the temperature, middle low-temperature activation aluminum nitride ceramic substrate is obtained；
(3) high-temperature activation: step (2) aluminum nitride ceramic substrate is continued to heat up, and is warming up to 380 DEG C with 20 DEG C/min, heat preservation temperature
0.5h to get surface active aluminum nitride ceramic substrate.
Wherein, the energy beam in the step (7) is to carry out active processing to ceramic base plate surface using gas ion source,
And the ion beam energy 10 of ion beam irradiation-3eV。
Wherein, need to be by ceramic substrate back bias voltage in -415Volt in the step (7) when starting sputter nickel target, and control
The current density of target processed is in 0.34W/cm2, carry out bombardment by ions and be implanted into the time 6min of target.
Wherein, the vacuum degree in the step (7) is not less than 4.0 × 10-3Pa。
Embodiment 4
The manufacturing method for covering copper aluminum nitride ceramic substrate of the present embodiment, comprising the following steps:
(1) preparation of spot corrosion solution: spot corrosion solution is mixed by sodium sulphate, sulfuric acid, sustained release agent and additive, wherein sustained release agent
By any or both mixing of ethylene glycol, glycerol, additive is any or both mixing of oxalic acid, EDTA, by selection
Reagent is dissolved in deionized water in proportion, and is stirred under the conditions of 50 DEG C, mixing speed 530rpm, is filtered after stirring 45min
Spot corrosion solution is made；
(2) dirty removing processing: aluminum nitride ceramic substrate is immersed except being cleaned in oil solution with ultrasonic cleaning technique, aluminium nitride is removed
The dirt of ceramic base plate surface under sodium sulphate effect, and washes down its surface with deionized water；
(3) ungrease treatment: aluminum nitride ceramic substrate is immersed in degreasant solution, is cleaned with ultrasonic cleaning process, degreasing 6min
After take out, with deionized water rinse 4-6 times；
(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasound
Technique forms concave point on aluminum nitride ceramic substrate surface under sodium sulphate effect, and taking-up is washed down with deionized water, cold wind drying；
(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is by copper sulphate, sodium peroxydisulfate, boron
Acid and potassium citrate mix, and the aluminum nitride ceramic substrate for being coated with activator is placed in activation furnace and is activated；
(6) it is heat-treated: the aluminum nitride ceramic substrate after spot corrosion being placed in vacuum furnace again, after temperature is first risen to 190 DEG C
2.2h is kept the temperature, keeps the temperature 1.6h after then rising to 250-300 DEG C；
(7) nickel plating: the aluminum nitride ceramic substrate after heat treatment is placed in a vacuum chamber, and by N2By opening in the chamber
Dynamic sputter nickel target forms ion beam and splashes, and the nickle atom splashed out volatilizees to form plasmoid and be adsorbed and be deposited on
On the active faying face of ceramic substrate, nickel plating aluminum nitride ceramic substrate is formed；
(8) vacuum expands weldering: nickel plating aluminum nitride ceramic substrate plate is bonded with the copper foil position to be welded after cleaning with relative fashion,
It is subsequently placed in vacuum to expand in brazier, closes vacuum chamber, open pumped vacuum systems, open heating system, vacuum is expanded into brazier temperature
Be warming up to 680 DEG C, before heat preservation starts, to after fitting material apply 4.5MPa pressure, then temperature be 680 DEG C at and
Under conditions of pressure is 4.5Pa, 25-35min is kept the temperature, unloading pressure after heat preservation is cooled to room temperature with furnace temperature, and it is dry, it is covered
Copper aluminum nitride ceramic substrate.
Wherein, in the step (1), include sodium sulphate 160g in every 1L spot corrosion solution, sulfuric acid 35ml, sustained release agent 23g, add
Add agent 6g, remaining is water.
Wherein, in the step (2) except oil solution be it is acid remove vinegar liquid, solubility 130g/L, ultrasonic power 135W,
Sonication treatment time is 28min.
Wherein, in the step (3), every 1L degreasing agent includes acid degreasing agent 90ml, sulfuric acid 180ml, remaining is water.
Wherein, the ultrasonic frequency in the step (3) is 55KHz, and the processing time is 35min.
Wherein, the activator in the step (5) is by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate in mass ratio 5:
3:2:1 is mixed.
Wherein, the specific steps that the step (5) is activated are as follows:
(1) pre-activate: the aluminum nitride ceramic substrate for being coated with activator will be placed in activation furnace, in 2 atmosphere of high-purity N, with 10
DEG C/heating rate of min is warming up to 150 DEG C, temperature 1.5h is kept the temperature, pre-activate aluminum nitride ceramic substrate is obtained；
(2) low-temperature activation in: the pre-activate aluminum nitride ceramic substrate of step (1) is continued to heat up, and is warming up to 250 with 15 DEG C/min
DEG C, 1.0h is kept the temperature, middle low-temperature activation aluminum nitride ceramic substrate is obtained；
(3) high-temperature activation: step (2) aluminum nitride ceramic substrate is continued to heat up, and is warming up to 380 DEG C with 20 DEG C/min, heat preservation temperature
0.5h to get surface active aluminum nitride ceramic substrate.
Wherein, the energy beam in the step (7) is to carry out active processing to ceramic base plate surface using gas ion source,
And the ion beam energy 10 of ion beam irradiation-2eV。
Wherein, need to be by ceramic substrate back bias voltage in -400Volt in the step (7) when starting sputter nickel target, and control
The current density of target processed is in 0.3W/cm2, carry out bombardment by ions and be implanted into the time 5 of target.5min.
Wherein, the vacuum degree in the step (7) is not less than 4.0 × 10-3Pa。
Embodiment 5
The manufacturing method for covering copper aluminum nitride ceramic substrate of the present embodiment, comprising the following steps:
(1) preparation of spot corrosion solution: spot corrosion solution is mixed by sodium sulphate, sulfuric acid, sustained release agent and additive, wherein sustained release agent
By any or both mixing of ethylene glycol, glycerol, additive is any or both mixing of oxalic acid, EDTA, by selection
Reagent is dissolved in deionized water in proportion, and is stirred under the conditions of 50 DEG C, mixing speed 580rpm, is filtered after stirring 55min
Spot corrosion solution is made；
(2) dirty removing processing: aluminum nitride ceramic substrate is immersed except being cleaned in oil solution with ultrasonic cleaning technique, aluminium nitride is removed
The dirt of ceramic base plate surface under sodium sulphate effect, and washes down its surface with deionized water；
(3) ungrease treatment: aluminum nitride ceramic substrate is immersed in degreasant solution, is cleaned with ultrasonic cleaning process, degreasing 9min
After take out, with deionized water rinse 4-6 times；
(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasound
Technique forms concave point on aluminum nitride ceramic substrate surface under sodium sulphate effect, and taking-up is washed down with deionized water, cold wind drying；
(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is by copper sulphate, sodium peroxydisulfate, boron
Acid and potassium citrate mix, and the aluminum nitride ceramic substrate for being coated with activator is placed in activation furnace and is activated；
(6) it is heat-treated: the aluminum nitride ceramic substrate after spot corrosion being placed in vacuum furnace again, after temperature is first risen to 210 DEG C
2.8h is kept the temperature, keeps the temperature 1.9h after then rising to 290 DEG C；
(7) nickel plating: the aluminum nitride ceramic substrate after heat treatment is placed in a vacuum chamber, and by N2By opening in the chamber
Dynamic sputter nickel target forms ion beam and splashes, and the nickle atom splashed out volatilizees to form plasmoid and be adsorbed and be deposited on
On the active faying face of ceramic substrate, nickel plating aluminum nitride ceramic substrate is formed；
(8) vacuum expands weldering: nickel plating aluminum nitride ceramic substrate plate is bonded with the copper foil position to be welded after cleaning with relative fashion,
It is subsequently placed in vacuum to expand in brazier, closes vacuum chamber, open pumped vacuum systems, open heating system, vacuum is expanded into brazier temperature
Be warming up to 720 DEG C, before heat preservation starts, to after fitting material apply 5.5MPa pressure, then temperature be 720 DEG C at and
Under conditions of pressure is 5.5MPa, 32min is kept the temperature, unloading pressure after heat preservation is cooled to room temperature with furnace temperature, and it is dry, it obtains covering copper
Aluminum nitride ceramic substrate.
Wherein, in the step (1), include sodium sulphate 190g in every 1L spot corrosion solution, sulfuric acid 45ml, sustained release agent 28g, add
Add agent 9g, remaining is water.
Wherein, in the step (2) except oil solution be it is acid remove vinegar liquid, solubility 150g/L, ultrasonic power 150W,
Sonication treatment time is 32min.
Wherein, in the step (3), every 1L degreasing agent includes acid degreasing agent 110ml, sulfuric acid 220ml, remaining is water.
Wherein, the ultrasonic frequency in the step (3) is 65KHz, and the processing time is 45min.
Wherein, the activator in the step (5) is by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate in mass ratio 5:
3:2:1 is mixed.
Wherein, the specific steps that the step (5) is activated are as follows:
(1) pre-activate: the aluminum nitride ceramic substrate for being coated with activator will be placed in activation furnace, in 2 atmosphere of high-purity N, with 10
DEG C/heating rate of min is warming up to 150 DEG C, temperature 1.5h is kept the temperature, pre-activate aluminum nitride ceramic substrate is obtained；
(2) low-temperature activation in: the pre-activate aluminum nitride ceramic substrate of step (1) is continued to heat up, and is warming up to 250 with 15 DEG C/min
DEG C, 1.0h is kept the temperature, middle low-temperature activation aluminum nitride ceramic substrate is obtained；
(3) high-temperature activation: step (2) aluminum nitride ceramic substrate is continued to heat up, and is warming up to 380 DEG C with 20 DEG C/min, heat preservation temperature
0.5h to get surface active aluminum nitride ceramic substrate.
Wherein, the energy beam in the step (7) is to carry out active processing to ceramic base plate surface using gas ion source,
And the ion beam energy 10 of ion beam irradiation-2-10-4eV。
Wherein, need to be by ceramic substrate back bias voltage in -430Volt in the step (7) when starting sputter nickel target, and control
The current density of target processed is in 0.5W/cm2, carry out bombardment by ions and be implanted into the time 6.5min of target.
Wherein, the vacuum degree in the step (7) is not less than 4.0 × 10-3Pa。
Comparative example 1
In addition to saving step (3) of the invention, other are consistent with embodiment 1.
Comparative example 2
In addition to saving step (6) of the invention, other are consistent with embodiment 1.
Comparative example 3
In addition to saving step (1) of the invention, (4), other are consistent with embodiment 1.
Comparative example 4
In addition to saving step (5) of the invention, other are consistent with embodiment 1.
Test example
Intensity, peel strength, interface are combined by copper aluminum nitride ceramic substrate is covered made from embodiment 1-5 and comparative example 1-4
Layer stomata, thermal cycle test, specific test method are as follows:
Bond strength: kovar alloy is welded on copper aluminum nitride ceramic substrate in covering of obtaining of embodiment 1-5 and comparative example 1-4 respectively
Column, then the stretched vertically on tensile testing machine (Shanghai Shenlian Tester Factory, LDS-50), stretcher strain speed are 1mm/min,
Calculate tension failure when maximum pull and forced area ratio to get arrive collected values of bond strength.
Peel strength: the peeling strength testing machine (YX- of Dongguan City Chang'an AsiaSat precision instrument Co., Ltd production is used
BL-01A type peel strength tester) it is tested, 90 ° of (vertical) directions are carried out to the copper foil in aluminium nitride copper-clad base plate and are torn
Under, test its peel strength.
Times of thermal cycle test: the thermal cycling test machine (KSKB- of KSON Instrument Technology's production is used
415TBS type thermal cycling test machine) it is tested.Sample is put into heat impact tester, with -50 DEG C of heat preservation 30min, 150
DEG C heat preservation 30min is that a circulation is tested, and record aluminium nitride copper-clad base plate occurs that bending, column are horizontal, copper film falls off, and warpage shows
As when cycle-index.
Observing interface layer stomata: by embodiment 1-5 and comparative example 1-4 obtain cover on copper aluminum nitride ceramic substrate copper foil from
It is removed on ceramic substrate, in 1000 times of gold as microscopically observation, observes the stomata on the removing interface of ceramic copper-clad base plate
Quantity.
According to above-mentioned performance test requirement, copper aluminum nitride ceramic substrate is covered into embodiment 1-5 and comparative example 1-4 preparation
Performance parameter is listed in Table 1 below.
Table 1
| Test item | Bond strength (MPa) | Peel strength (N/mm) | Boundary layer stomata | Times of thermal cycle |
| Embodiment 1 | 67.6 | 19.8 | Seldom | 218 |
| Embodiment 2 | 68.2 | 20.4 | Seldom | 228 |
| Embodiment 3 | 69.3 | 20.9 | Seldom | 235 |
| Embodiment 4 | 68.5 | 19.9 | Seldom | 222 |
| Embodiment 5 | 68.8 | 20.2 | Seldom | 230 |
| Comparative example 1 | 64.8 | 19.2 | It is more | 204 |
| Comparative example 2 | 62.3 | 18.7 | It is more | 193 |
| Comparative example 3 | 58.7 | 16.1 | It is more | 178 |
| Comparative example 4 | 55.8 | 15.4 | It is more | 170 |
The bond strength, peel strength, boundary for covering copper aluminum nitride ceramic substrate of the invention it can be seen from the test result of table 1
Surface layer stomata and thermal circulation performance have all obtained significant raising, and from comparative example 1-4:
(1) then make the surface of aluminum nitride ceramic substrate become smooth it is found that passing through ungrease treatment by comparative example 1, become uniform
Unanimously, while then raising with copper foil binding force, and porosity between ceramic substrate and copper foil can be reduced, covers copper nitrogen to improve
Change the intensity of aluminium ceramic substrate；
(2) by comparative example 2 it is found that by the way that ceramic substrate is put into the heat treatment carried out in vacuum furnace, and it is divided to two sections of progress,
On the one hand the activity for improving ceramic substrate, on the other hand, can by Fractional Heat-treatment conducive to the formation of consequent activities faying face
The stress inside ceramic substrate is eliminated, reduces and covers copper aluminum nitride ceramic substrate intensity as caused by ceramic substrate stress variation
Decline problem；
(3) by comparative example 3 it is found that concave point can be formed on aluminum nitride ceramic substrate surface by spot corrosion processing, to increase copper foil
With ceramic substrate contact area, the binding force of ceramic substrate and copper foil is improved, while concave point setting can make to enter in concave point
Copper foil, which is formed, is similar to " fixed column ", and then improves its peel strength；
(4) it by comparative example 3 it is found that the present invention is by coating activator in ceramic base plate surface, and carries out in activation furnace and true
Pre-activate, middle low-temperature activation and high-temperature activation are carried out in empty heating furnace, the activation processing for having gradient are carried out, so that in activator
Copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate can be sufficiently submerged in ceramic base plate surface, and be formed in ceramic base plate surface
Height infiltration, high activity active membrane layer, the film layer have preferable affinity and cohesive force, the present invention can be improved and cover copper aluminium nitride
The peel strength of ceramic substrate, and achieve the purpose that reduce voidage.
In summary, the present invention solves existing copper foil and aluminum nitride ceramic substrate binding force deficiency, hole ratio is high, removing is strong
The problems such as low is spent, by reducing hole ratio between the two, improves the binding force of the two, copper aluminum nitride ceramic substrate is covered in enhancing
Intensity.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of manufacturing method for covering copper aluminum nitride ceramic substrate, which comprises the following steps:
(1) preparation of spot corrosion solution: spot corrosion solution is mixed by sodium sulphate, sulfuric acid, sustained release agent and additive, wherein sustained release agent
By any or both mixing of ethylene glycol, glycerol, additive is any or both mixing of oxalic acid, EDTA, by selection
Reagent is dissolved in deionized water in proportion, and is stirred under the conditions of 50 DEG C, mixing speed 500-600rpm, and 40-60min is stirred
It filters afterwards and spot corrosion solution is made；
(2) dirty removing processing: aluminum nitride ceramic substrate is immersed except being cleaned in oil solution with ultrasonic cleaning technique, aluminium nitride is removed
The dirt of ceramic base plate surface under sodium sulphate effect, and washes down its surface with deionized water；
(3) ungrease treatment: aluminum nitride ceramic substrate is immersed in degreasant solution, is cleaned with ultrasonic cleaning process, degreasing 5-
It takes out after 10min, is rinsed 4-6 times with deionized water；
(4) aluminum nitride ceramic substrate surface pitting is handled: aluminum nitride ceramic substrate being immersed in spot corrosion solution, and is aided with ultrasound
Technique forms concave point on aluminum nitride ceramic substrate surface under sodium sulphate effect, and taking-up is washed down with deionized water, cold wind drying；
(5) it is activated: activator is coated on aluminum nitride ceramic substrate surface, the activator is by copper sulphate, sodium peroxydisulfate, boron
Acid and potassium citrate mix, and the aluminum nitride ceramic substrate for being coated with activator is placed in activation furnace and is activated；
(6) it is heat-treated: the aluminum nitride ceramic substrate after spot corrosion being placed in vacuum furnace again, temperature is first risen into 180-220
2-3h is kept the temperature after DEG C, keeps the temperature 1.5-2h after then rising to 250-300 DEG C；
(7) nickel plating: the aluminum nitride ceramic substrate after heat treatment is placed in a vacuum chamber, and by N2By starting in the chamber
Sputter nickel target forms ion beam and splashes, and the nickle atom splashed out volatilizees to form plasmoid and be adsorbed and be deposited on pottery
On the active faying face of porcelain substrate, nickel plating aluminum nitride ceramic substrate is formed；
(8) vacuum expands weldering: nickel plating aluminum nitride ceramic substrate plate is bonded with the copper foil position to be welded after cleaning with relative fashion,
It is subsequently placed in vacuum to expand in brazier, closes vacuum chamber, open pumped vacuum systems, open heating system, vacuum is expanded into brazier temperature
It is warming up to 650-750 DEG C, before heat preservation starts, applies the pressure of 4-6MPa to the material after fitting, is then 650- in temperature
At 750 DEG C and pressure is keeps the temperature 25-35min under conditions of 4-6MPa, and unloading pressure after heat preservation is cooled to room temperature with furnace temperature, is done
It is dry, it obtains covering copper aluminum nitride ceramic substrate.
2. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (1)
In, in every 1L spot corrosion solution include sodium sulphate 150-200g, sulfuric acid 30-50ml, sustained release agent 20-30g, additive 5-10g, remaining
For water.
3. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (2)
In except oil solution be it is acid remove vinegar liquid, solubility 120-160g/L, ultrasonic power 130-160W, sonication treatment time is
25-35min。
4. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (3)
In, every 1L degreasing agent includes acid degreasing agent 80-120ml, sulfuric acid 150-250ml, remaining is water.
5. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (3)
In ultrasonic frequency be 50-70KHz, the processing time be 30-50min.
6. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (5)
In activator mixed by copper sulphate, sodium peroxydisulfate, boric acid and potassium citrate 5:3:2:1 in mass ratio.
7. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (5)
The specific steps of activation processing are as follows:
(1) pre-activate: the aluminum nitride ceramic substrate for being coated with activator will be placed in activation furnace, in 2 atmosphere of high-purity N, with 10
DEG C/heating rate of min is warming up to 150 DEG C, temperature 1.5h is kept the temperature, pre-activate aluminum nitride ceramic substrate is obtained；
(2) low-temperature activation in: the pre-activate aluminum nitride ceramic substrate of step (1) is continued to heat up, and is warming up to 250 with 15 DEG C/min
DEG C, 1.0h is kept the temperature, middle low-temperature activation aluminum nitride ceramic substrate is obtained；
(3) high-temperature activation: step (2) aluminum nitride ceramic substrate is continued to heat up, and is warming up to 380 DEG C with 20 DEG C/min, heat preservation temperature
0.5h to get surface active aluminum nitride ceramic substrate.
8. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (7)
In energy beam be that active processing, and the ion beam energy of ion beam irradiation are carried out to ceramic base plate surface using gas ion source
10-2-10-4eV。
9. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (7)
, need to be by ceramic substrate back bias voltage in -380~-450Volt when middle starting sputter nickel target, and the current density for controlling target exists
0.3-0.5W/cm2, carry out bombardment by ions and be implanted into the time 5-7min of target.
10. the manufacturing method according to claim 1 for covering copper aluminum nitride ceramic substrate, which is characterized in that the step (7)
In vacuum degree be not less than 4.0 × 10-3Pa。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111081674A (en) * | 2020-01-02 | 2020-04-28 | 上海航天电子通讯设备研究所 | High-silicon aluminum alloy adapter plate and preparation method thereof |
| CN112624788A (en) * | 2020-12-17 | 2021-04-09 | 东南大学 | Method for quickly coating copper on surface of aluminum nitride ceramic |
| CN114907135A (en) * | 2022-05-16 | 2022-08-16 | 江苏富乐华半导体科技股份有限公司 | Preparation method of aluminum nitride copper-clad ceramic substrate |
| CN115322011A (en) * | 2022-07-25 | 2022-11-11 | 深圳市吉迩科技有限公司 | Hydrophobic and oleophylic porous ceramic preparation method, hydrophobic and oleophylic porous ceramic and application thereof |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111081674A (en) * | 2020-01-02 | 2020-04-28 | 上海航天电子通讯设备研究所 | High-silicon aluminum alloy adapter plate and preparation method thereof |
| CN111081674B (en) * | 2020-01-02 | 2022-02-18 | 上海航天电子通讯设备研究所 | High-silicon aluminum alloy adapter plate and preparation method thereof |
| CN112624788A (en) * | 2020-12-17 | 2021-04-09 | 东南大学 | Method for quickly coating copper on surface of aluminum nitride ceramic |
| CN114907135A (en) * | 2022-05-16 | 2022-08-16 | 江苏富乐华半导体科技股份有限公司 | Preparation method of aluminum nitride copper-clad ceramic substrate |
| CN115322011A (en) * | 2022-07-25 | 2022-11-11 | 深圳市吉迩科技有限公司 | Hydrophobic and oleophylic porous ceramic preparation method, hydrophobic and oleophylic porous ceramic and application thereof |
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Application publication date: 20190215 |