CN115410925B - Method for improving heat-resistant cycle reliability of aluminum nitride coated aluminum packaging lining plate - Google Patents
Method for improving heat-resistant cycle reliability of aluminum nitride coated aluminum packaging lining plate Download PDFInfo
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Abstract
The invention provides a method for improving the heat-resistant cycle reliability of an aluminum nitride aluminum-coated packaging lining plate, which comprises the steps of sputtering copper plating on the surface of an aluminum nitride aluminum-coated ceramic substrate, performing vacuum diffusion sintering, introducing trace copper elements into the surface layer of aluminum to form a uniform copper-aluminum solid solution hardening layer, performing chemical nickel plating treatment on the surface to form a uniform nickel plating layer on the surface, and reducing the concentration of surface stress of a coating and the cracking condition of the coating by the method.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method for improving the heat-resistant cycle reliability of an aluminum nitride coated packaging lining plate.
Background
With the rapid development of IGBT power electronics, power electronics technology is evolving towards high voltage, high current, high power density, high speed aspects; aluminum nitride coated ceramic substrate (DBA) is used as the packaging substrate of IGBT, has excellent heat-resistant cycle performance, excellent interface bonding reliability, high heat conductivity and high insulating strength, and is favored by third-generation SiC semiconductor devices.
In the heat-resistant cycle performance test process of the device, aluminum has lower yield strength, and crystal grains can absorb partial damage protection ceramics through plastic deformation, so that a bonding interface of aluminum and aluminum nitride ceramics has higher heat-resistant cycle reliability compared with an interface of copper and aluminum nitride ceramics, but as the number of heat-resistant cycles increases, the surface roughness of the bonding interface is increased rapidly, and further, a Ni-plated layer on the surface of a DBA substrate is easily subject to water ripple, burrs and even cracking; in practical application environment, the failure of the reliability of the surface coating may also cause the failure of the device, so that development of a method for improving the reliability of the heat-resistant cycle of the aluminum nitride coated packaging lining plate is needed to be developed, and the reliability problem of the heat-resistant cycle of the device is further reduced or solved.
Disclosure of Invention
The invention aims to provide a method for improving the heat cycle reliability of an aluminum nitride coated packaging lining plate so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for improving the heat-resistant cycle reliability of an aluminum nitride coated packaging lining plate specifically comprises the following steps:
(1) Surface sputtering copper plating: taking an aluminum nitride aluminum-coated ceramic substrate for surface cleaning, and then plating copper to obtain the aluminum nitride aluminum-coated ceramic substrate with a nanoscale copper layer, wherein the thickness of the copper-plated layer is 80-120 nm;
(2) Diffusion annealing: vacuum sintering the nano-scale copper layer aluminum nitride aluminum-coated ceramic substrate in the step (1), preserving heat for 2-3 h at 470-540 ℃, and cooling to 22-25 ℃ along with a furnace;
(3) Surface nickel plating: and (3) taking the aluminum nitride aluminum-coated ceramic substrate treated in the step (2), immersing the ceramic substrate into chemical nickel plating solution for surface nickel plating after secondary zinc immersion, wherein the thickness of the nickel plating layer is 3.5-7 mu m.
Further, in the step (1), the thickness of the aluminum layer on the surface of the aluminum nitride aluminum-coated ceramic substrate is 0.2-0.6 mm.
Further, in the step (1), the copper plating process is a surface sputtering copper plating process, and the working parameters are as follows: the power is 5KW, the Ar flow is 30Sccm, and the sputtering pressure is 0.4Pa for 10min.
Further, in the step (1), the surface cleaning step is as follows:
A. preparing 10-20% sodium hydroxide aqueous solution, immersing the aluminum nitride aluminum-coated ceramic substrate into alkaline washing for 3-5 min, taking out and washing with pure water;
B. and (3) preparing a 10-20% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step (A) into the aqueous solution for pickling for 90-100 s, taking out the ceramic substrate, cleaning the ceramic substrate with pure water, and drying the ceramic substrate at 80-120 ℃ for later use.
Further, in the step (3), the secondary zinc leaching step is as follows: preparing zinc dipping liquid by NaOH and ZnO, wherein the mass fraction of the NaOH is 10%, the mass fraction of the ZnO is 1.6%, and the balance is pure water, immersing the aluminum nitride aluminum-coated ceramic substrate treated in the step (2) for 40-45 s, taking out and cleaning; immersing in 30% aqueous solution of nitric acid, carrying out secondary pickling for 90-100 s, taking out and cleaning; placing the mixture in zinc leaching solution for secondary zinc leaching for 30-35 s, taking out, and cleaning with pure water for standby.
Further, in the step (2), the diffusion annealing temperature rising speed is 1-3 ℃/min, and the Vickers hardness of the annealed aluminum surface is 27-35 HV1.
Further, in the step (3), the surface nickel plating process condition is that the electroless plating is carried out for 20-60 min at 80-85 ℃.
Further, in the step (3), the chemical nickel plating solution is NiSO 4 ·7H 2 O：25g/L，NaH 2 PO 2 ·H 2 O：36g/L，Na 3 C 6 H 5 O 7 ·2H 2 O:12g/l, the rest is pure water; wherein the pH value of the electroless nickel plating solution is 4.5-5.6.
Compared with the prior art, the method comprises the steps of firstly sputtering copper plating treatment and vacuum diffusion sintering treatment on the surface of an aluminum nitride aluminum-coated ceramic substrate, introducing trace copper elements into the surface layer of aluminum to form a uniform copper-aluminum solid solution hardening layer, wherein the surface is silvery white, the Vickers hardness of the surface of aluminum is 27-35 HV1, and then performing surface nickel plating treatment to obtain a final aluminum nitride aluminum-coated packaging lining plate;
the beneficial effects achieved by the invention are as follows: according to the invention, the hardening of the aluminum layer on the surface of the DBA has gradient change characteristics, and the inner layer of the DBA substrate is close to the AlN ceramic aluminum surface and still has the toughness of Al, so that the product has high reliability of a bonding area, and meanwhile, the heat-resistant reliability of the surface coating is obviously improved. The rapid increase of the surface roughness of the substrate in the thermal cycle test process is prevented, the phenomena of plating water ripple, cracking and the like are reduced, and the thermal cycle reliability of the aluminum nitride aluminum-coated substrate is further improved.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is a 3D topography scan of the sample surface of the example 1 package substrate before (left panel) and after (right panel) thermal cycling testing;
FIG. 3 is a 3D topography scan of the surface of a comparative example 1 package liner sample before (left panel) and after (right panel) thermal cycling testing;
FIG. 4 is a plot of the surface roughness after 100 thermal cycles at-55deg.C/150deg.C for example 1;
FIG. 5 is a plot of the surface roughness profile of comparative example 1 after 100 thermal cycles at-55deg.C/150deg.C.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
Example 1
(1) Preparing 10% sodium hydroxide aqueous solution by mass percent, taking an aluminum nitride aluminum-coated ceramic substrate product, completely immersing the product into the sodium hydroxide aqueous solution, taking out the product after alkaline washing for 3min, and cleaning the product with pure water;
(2) Preparing 10 percent of nitric acid aqueous solution, taking the aluminum nitride coated ceramic substrate in the step (1), completely immersing the aluminum nitride coated ceramic substrate in the nitric acid aqueous solution, pickling for 90 seconds, taking out, cleaning with pure water, and drying at 80 ℃ for later use;
(3) Surface sputtering copper plating: taking the aluminum nitride aluminum-coated ceramic substrate cleaned in the step (2), sputtering copper plating on the surface of the aluminum nitride aluminum-coated ceramic substrate, sputtering for 10min under the conditions of 5KW power, 30Sccm Ar flow and 0.4Pa sputtering pressure, wherein the thickness of the copper plating layer is 80nm, and electroplating to obtain the aluminum nitride aluminum-coated ceramic substrate with the nano-scale copper layer on the aluminum surface;
(4) Diffusion annealing: carrying out vacuum sintering on the aluminum nitride coated ceramic substrate in the step (3), carrying out diffusion annealing for 2 hours at 470 ℃, wherein the temperature rising speed of the diffusion annealing is 1 ℃/min, cooling to 22 ℃ along with a furnace after the annealing is finished, and carrying out heat preservation for 2 hours, so as to form a copper-aluminum solid solution hardening layer on the surface of the aluminum nitride coated ceramic substrate, wherein the thickness of the aluminum layer is 0.2mm;
(5) Preparing zinc leaching liquid: the zinc dipping liquid comprises 10 percent of NaOH, 1.6 percent of ZnO and the balance of pure water, the aluminum nitride coated ceramic substrate in the step (4) is fully immersed in the zinc dipping liquid, the zinc dipping time is 40s, the ceramic substrate is taken out and washed, immersed in 30 percent of nitric acid aqueous solution for secondary pickling for 90s, taken out and washed with pure water again, placed in the zinc dipping liquid for secondary zinc dipping for 30s, taken out and washed with pure water for standby;
(6) Surface nickel plating: taking the aluminum nitride coated aluminum ceramic substrate cleaned in the step (5), plating nickel on the surface of the aluminum nitride coated aluminum ceramic substrate by adopting an electroless plating process, wherein the composition of the electroless nickel plating solution is 25g/L of NiSO 4 ·7H 2 NaH of O, 36g/L 2 PO 2 ·H 2 O, 12g/L Na 3 C 6 H 5 O 7 ·2H 2 O, the rest is pure water; controlling the pH value to be 4.5, carrying out chemical plating for 20min at the temperature of 80 ℃ under the nickel plating reaction condition, wherein the thickness of a nickel plating layer is 3.5 mu m, and cleaning the surface by pure water after the nickel plating is finished to obtain the aluminum nitride aluminum-coated packaging lining plate.
Example 2
(1) Preparing a sodium hydroxide aqueous solution with the mass percentage of 13%, taking an aluminum nitride aluminum-coated ceramic substrate product, completely immersing the aluminum nitride aluminum-coated ceramic substrate product into the sodium hydroxide aqueous solution, taking out the aluminum nitride aluminum-coated ceramic substrate product after alkaline washing for 4min, and washing the aluminum nitride aluminum-coated ceramic substrate product with pure water;
(2) Preparing a 13 percent nitric acid aqueous solution, taking the aluminum nitride coated ceramic substrate in the step (1), completely immersing the aluminum nitride coated ceramic substrate in the nitric acid aqueous solution, pickling for 93 seconds, taking out, cleaning with pure water, and drying at 90 ℃ for later use;
(3) Surface sputtering copper plating: taking the aluminum nitride aluminum-coated ceramic substrate cleaned in the step (2), sputtering copper plating on the surface of the aluminum nitride aluminum-coated ceramic substrate, sputtering for 10min under the conditions of 5KW power, 30Sccm Ar flow and 0.4Pa sputtering pressure, wherein the thickness of the copper plating layer is 95nm, and electroplating to obtain the aluminum nitride aluminum-coated ceramic substrate with the nano-scale copper layer on the aluminum surface;
(4) Diffusion annealing: carrying out vacuum sintering on the aluminum nitride aluminum-coated ceramic substrate in the step (3), carrying out diffusion annealing at 490 ℃ for 2.5 hours, wherein the temperature rising speed of the diffusion annealing is 2 ℃/min, cooling to 23 ℃ along with a furnace after the annealing is finished, and carrying out heat preservation for 2.5 hours, so as to form a copper-aluminum solid solution hardening layer on the surface of the aluminum nitride aluminum-coated ceramic substrate, wherein the thickness of the aluminum layer is 0.3mm;
(5) Preparing zinc leaching liquid: the zinc dipping liquid comprises 10 percent of NaOH, 1.6 percent of ZnO and the balance of pure water, the aluminum nitride coated ceramic substrate in the step (4) is fully immersed in the zinc dipping liquid, the zinc dipping time is 42s, the ceramic substrate is taken out and washed, immersed in 30 percent of nitric acid aqueous solution for secondary acid washing for 93s, taken out and washed again with pure water, placed in the zinc dipping liquid for secondary zinc dipping for 32s, taken out and washed with pure water for standby;
(6) Surface nickel plating: taking the aluminum nitride coated aluminum ceramic substrate cleaned in the step (5), plating nickel on the surface of the aluminum nitride coated aluminum ceramic substrate by adopting an electroless plating process, wherein the composition of the electroless nickel plating solution is 25g/L of NiSO 4 ·7H 2 NaH of O, 36g/L 2 PO 2 ·H 2 O, 12g/L Na 3 C 6 H 5 O 7 ·2H 2 O, the rest is pure water; controlling the pH value to be 4.8, carrying out chemical plating for 35min at the temperature of 82 ℃ under the nickel plating reaction condition, wherein the thickness of a nickel plating layer is 5 mu m, and cleaning the surface by pure water after the nickel plating is finished to obtain the aluminum nitride aluminum-coated packaging lining plate.
Example 3
(1) Preparing a sodium hydroxide aqueous solution with the mass percentage of 18%, taking an aluminum nitride aluminum-coated ceramic substrate product, completely immersing the aluminum nitride aluminum-coated ceramic substrate product into the sodium hydroxide aqueous solution, taking out the aluminum nitride aluminum-coated ceramic substrate product after alkaline washing for 4min, and washing the aluminum nitride aluminum-coated ceramic substrate product with pure water;
(2) Preparing 18 percent of nitric acid aqueous solution, taking the aluminum nitride coated ceramic substrate in the step (1), completely immersing the aluminum nitride coated ceramic substrate in the nitric acid solution, pickling for 97 seconds, taking out, cleaning with pure water, and drying at 100 ℃ for later use;
(3) Surface sputtering copper plating: taking the aluminum nitride aluminum-coated ceramic substrate cleaned in the step (2), sputtering copper plating on the surface of the aluminum nitride aluminum-coated ceramic substrate, sputtering for 10min under the conditions of 5KW power, 30Sccm Ar flow and 0.4Pa sputtering pressure, wherein the thickness of the copper plating layer is 105nm, and electroplating to obtain the aluminum nitride aluminum-coated ceramic substrate with the nano-scale copper layer on the aluminum surface;
(4) Diffusion annealing: carrying out vacuum sintering on the aluminum nitride aluminum-coated ceramic substrate in the step (3), carrying out diffusion annealing at 510 ℃ for 2.5 hours, wherein the temperature rising speed of the diffusion annealing is 2 ℃/min, cooling to 24 ℃ along with a furnace after the annealing is finished, and carrying out heat preservation for 2.5 hours, so as to form a copper-aluminum solid solution hardening layer on the surface of the aluminum nitride aluminum-coated ceramic substrate, wherein the thickness of the aluminum layer is 0.4mm;
(5) Preparing zinc leaching liquid: the zinc dipping liquid comprises 10 percent of NaOH, 1.6 percent of ZnO and the balance of pure water, the aluminum nitride coated ceramic substrate in the step (4) is fully immersed in the zinc dipping liquid, the zinc dipping time is 44s, the ceramic substrate is taken out and washed, immersed in 30 percent of nitric acid aqueous solution for secondary acid washing for 97s, taken out and washed again with pure water, placed in the zinc dipping liquid for secondary zinc dipping for 34s, taken out and washed with pure water for standby;
(6) Surface nickel plating: taking the aluminum nitride coated aluminum ceramic substrate cleaned in the step (5), plating nickel on the surface of the aluminum nitride coated aluminum ceramic substrate by adopting an electroless plating process, wherein the composition of the electroless nickel plating solution is 25g/L of NiSO 4 ·7H 2 NaH of O, 36g/L 2 PO 2 ·H 2 O, 12g/L Na 3 C 6 H 5 O 7 ·2H 2 O, the rest is pure water; controlling pH value to 5.2, electroless plating at 85 ℃ for 45min, nickel plating thickness to 6 μm, and cleaning the surface with pure water after nickel plating to obtain the aluminum nitride aluminum-coated packaging lining plate.
Example 4
(1) Preparing a sodium hydroxide aqueous solution with the mass percentage of 20%, taking an aluminum nitride aluminum-coated ceramic substrate product, completely immersing the aluminum nitride aluminum-coated ceramic substrate product into the sodium hydroxide aqueous solution, taking out the aluminum nitride aluminum-coated ceramic substrate product after alkaline washing for 5min, and washing the aluminum nitride aluminum-coated ceramic substrate product with pure water;
(2) Preparing 20 percent of nitric acid aqueous solution, taking the aluminum nitride coated ceramic substrate in the step (1), completely immersing the aluminum nitride coated ceramic substrate in the nitric acid solution, pickling for 100 seconds, taking out, cleaning with pure water, and drying at 120 ℃ for later use;
(3) Surface sputtering copper plating: taking the aluminum nitride aluminum-coated ceramic substrate cleaned in the step (2), sputtering copper plating on the surface of the aluminum nitride aluminum-coated ceramic substrate, sputtering for 10min under the conditions of 5KW power, 30Sccm Ar flow and 0.4Pa sputtering pressure, wherein the thickness of the copper plating layer is 120nm, and electroplating to obtain the aluminum nitride aluminum-coated ceramic substrate with the nano-scale copper layer on the aluminum surface;
(4) Diffusion annealing: carrying out vacuum sintering on the aluminum nitride coated ceramic substrate in the step (3), carrying out diffusion annealing for 3 hours at 540 ℃, wherein the temperature rising speed of the diffusion annealing is 3 ℃/min, cooling to 25 ℃ along with a furnace after the annealing is finished, and carrying out heat preservation for 3 hours, so as to form a copper-aluminum solid solution hardening layer on the surface of the aluminum nitride coated ceramic substrate, wherein the thickness of the aluminum layer is 0.6mm;
(5) Preparing zinc leaching liquid: the zinc dipping liquid comprises 10 percent of NaOH, 1.6 percent of ZnO and the balance of pure water, the aluminum nitride coated ceramic substrate in the step (4) is completely immersed in the zinc dipping liquid, the zinc dipping time is 45s, the ceramic substrate is taken out and washed, immersed in 30 percent of nitric acid aqueous solution for secondary pickling for 100s, taken out and washed again with pure water, placed in the zinc dipping liquid for secondary zinc dipping for 35s, taken out and washed with pure water for standby;
(6) Surface nickel plating: taking the aluminum nitride coated aluminum ceramic substrate cleaned in the step (5), plating nickel on the surface of the aluminum nitride coated aluminum ceramic substrate by adopting an electroless plating process, wherein the composition of the electroless nickel plating solution is 25g/L of NiSO 4 ·7H 2 NaH of O, 36g/L 2 PO 2 ·H 2 O, 12g/L Na 3 C 6 H 5 O 7 ·2H 2 O, the rest is pure water; controlling the pH value to be 5.6, carrying out chemical plating for 60min at the temperature of 85 ℃ under the nickel plating reaction condition, wherein the thickness of a nickel plating layer is 7 mu m, and cleaning the surface by pure water after the nickel plating is finished to obtain the aluminum nitride aluminum-coated packaging lining plate.
Comparative example 1
Comparative example 1 in which example 1 was used as a control group, the parameters were changed to nickel plating only on the surface of the aluminum nitride-coated ceramic substrate.
(1) Preparing 10% sodium hydroxide aqueous solution by mass percent, taking an aluminum nitride aluminum-coated ceramic substrate product, completely immersing the product into the sodium hydroxide aqueous solution, taking out the product after alkaline washing for 3min, and cleaning the product with pure water;
(2) Preparing 10 percent of nitric acid aqueous solution, taking the aluminum nitride coated ceramic substrate in the step (1), completely immersing the aluminum nitride coated ceramic substrate in the nitric acid solution, pickling for 90 seconds, taking out, cleaning with pure water, and drying at 80 ℃;
(3) Preparing zinc leaching liquid: the zinc dipping liquid comprises 10 percent of NaOH, 1.6 percent of ZnO and the balance of pure water, the aluminum nitride coated ceramic substrate in the step (2) is fully immersed into the zinc dipping liquid, the zinc dipping time is 40s, the ceramic substrate is taken out and washed, immersed into 30 percent of nitric acid aqueous solution for secondary pickling for 90s, taken out and washed with pure water again, placed in the zinc dipping liquid for secondary zinc dipping for 30s, taken out and washed with pure water for standby;
(4) Surface nickel plating: taking the aluminum nitride aluminum-coated ceramic substrate cleaned in the step (3), plating nickel on the surface of the aluminum nitride aluminum-coated ceramic substrate by adopting an electroless plating process, wherein the composition of the electroless nickel plating solution is 25g/L of NiSO 4 ·7H 2 NaH of O, 36g/L 2 PO 2 ·H 2 O, 12g/L Na 3 C 6 H 5 O 7 ·2H 2 O, the rest is pure water; controlling the pH value to be 4.5, carrying out chemical plating for 20min at the temperature of 80 ℃ under the nickel plating reaction condition, wherein the thickness of a nickel plating layer is 3.5 mu m, and cleaning the surface by pure water after the nickel plating is finished to obtain the aluminum nitride aluminum-coated packaging lining plate.
Comparative example 2
Comparative example 2 comparative example 1 was used as a control group, and the parameters were changed to change the thickness of the nickel plating layer on the surface of the aluminum nitride-coated ceramic substrate.
(1) Preparing 10% sodium hydroxide aqueous solution by mass percent, taking an aluminum nitride aluminum-coated ceramic substrate product, completely immersing the product into the sodium hydroxide aqueous solution, taking out the product after alkaline washing for 3min, and cleaning the product with pure water;
(2) Preparing 10 percent of nitric acid aqueous solution, taking the aluminum nitride coated ceramic substrate in the step (1), completely immersing the aluminum nitride coated ceramic substrate in the nitric acid solution, pickling for 90 seconds, taking out, cleaning with pure water, and drying at 80 ℃;
(3) Preparing zinc leaching liquid: the zinc dipping liquid comprises 10 percent of NaOH, 1.6 percent of ZnO and the balance of pure water, the aluminum nitride coated ceramic substrate in the step (2) is fully immersed into the zinc dipping liquid, the zinc dipping time is 40s, the ceramic substrate is taken out and washed, immersed into 30 percent of nitric acid aqueous solution for secondary pickling for 90s, taken out and washed with pure water again, placed in the zinc dipping liquid for secondary zinc dipping for 30s, taken out and washed with pure water for standby;
(4) Surface nickel plating: taking the aluminum nitride aluminum-coated ceramic substrate cleaned in the step (3), plating nickel on the surface of the aluminum nitride aluminum-coated ceramic substrate by adopting an electroless plating process, wherein the composition of the electroless nickel plating solution is 25g/L of NiSO 4 ·7H 2 NaH of O, 36g/L 2 PO 2 ·H 2 O, 12g/L Na 3 C 6 H 5 O 7 ·2H 2 O, the rest is pure water; controlling the pH value to be 4.5, carrying out chemical plating for 30min at the temperature of 80 ℃ under the nickel plating reaction condition, wherein the thickness of a nickel plating layer is 4.7 mu m, and cleaning the surface by pure water after the nickel plating is finished to obtain the aluminum nitride aluminum-coated packaging lining plate.
Experiment
(1) Taking the aluminum nitride coated aluminum ceramic substrates in the step (4) of the examples 1-3, the aluminum nitride coated aluminum packaging lining plates in the comparative examples 1-2, measuring the surface hardness of the coating by using a Vickers hardness tester and calculating an average value;
(2) Taking the aluminum nitride coated aluminum packaging liners in examples 1-3 and comparative examples 1-2, measuring the surface roughness by using a surface roughness meter and calculating an average value, then carrying out a thermal cycle test at-55-150 ℃ on the aluminum nitride coated aluminum packaging liners in examples 1-3 and comparative examples 1-2, and measuring the surface roughness again and calculating the average value after the test is completed.
The test results of experiments (1) to (2) are shown in the following table 1:
table 1: surface performance test of aluminum-coated ceramic substrate
| Surface hardness (HV 2) | Roughness average before thermal cycling | Roughness average after thermal cycling | |
| Example 1 | 27.2 | 0.35 | 0.42 |
| Example 2 | 29.5 | 0.34 | 0.43 |
| Example 3 | 28.3 | 0.35 | 0.41 |
| Example 4 | 29.6 | 0.34 | 0.40 |
| Comparative example 1 | 20.2 | 0.33 | 0.76 |
| Comparative example 2 | 21.4 | 0.32 | 0.74 |
As a result, the surface roughness Ra of examples 1 to 4 increased by about 20% after heat cycle, and the surface roughness Ra of comparative examples 1 to 2 increased by about 130% after heat cycle; as shown by 3D appearance characterization of a profilometer after 100 times of thermal cycling, the surface roughness of the samples of comparative examples 1-2 is large, and the surface of the samples of examples 1-4 is smooth without obvious roughness; the plating layers were visually inspected for no cracking.
In conclusion, copper plating and vacuum diffusion sintering are performed on the surface of the aluminum nitride aluminum-coated ceramic substrate, trace copper elements are introduced into the surface layer of aluminum to form a surface hardening layer, and then nickel plating treatment is performed on the surface hardening layer, so that the risks of roughness surge, coating cracking and device failure caused by high temperature during device operation under extreme conditions are reduced, and the heat cycle reliability of the aluminum nitride aluminum-coated packaging lining plate is further improved.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for improving the heat-resistant cycle reliability of an aluminum nitride coated aluminum packaging lining plate is characterized in that: the specific operation steps are as follows:
(1) Surface sputtering copper plating: taking an aluminum nitride aluminum-coated ceramic substrate for surface cleaning, and then plating copper to obtain the aluminum nitride aluminum-coated ceramic substrate with a nanoscale copper layer, wherein the thickness of the copper-plated layer is 80-120 nm; the copper plating process is a surface sputtering copper plating process, and the working parameters are as follows: the power is 5KW, the Ar flow is 30Sccm, and the sputtering pressure is 0.4Pa for 10min;
(2) Diffusion annealing: vacuum sintering the nano-scale copper layer aluminum nitride aluminum-coated ceramic substrate in the step (1), preserving heat for 2-3 h at 470-540 ℃, and cooling to 22-25 ℃ along with a furnace; the temperature rising speed of diffusion annealing is 1-3 ℃/min; the Vickers hardness of the surface of the annealed aluminum layer is 27-35 HV1;
(3) Surface nickel plating: taking the aluminum nitride aluminum-coated ceramic substrate treated in the step (2), immersing the ceramic substrate into chemical nickel plating solution for surface nickel plating after secondary zinc immersion, wherein the thickness of a nickel plating layer is 3.5-7 mu m; the surface nickel plating process is carried out for 20-60 min at 80-85 ℃.
2. The method for improving the heat cycle reliability of the aluminum nitride coated aluminum packaging liner plate according to claim 1, which is characterized in that: in the step (1), the thickness of the aluminum layer on the surface of the aluminum nitride aluminum-coated ceramic substrate is 0.2-0.6 mm.
3. The method for improving the heat cycle reliability of the aluminum nitride coated aluminum packaging liner plate according to claim 1, which is characterized in that: in the step (1), the surface cleaning step is as follows:
A. preparing 10-20% sodium hydroxide aqueous solution, immersing the aluminum nitride aluminum-coated ceramic substrate into alkaline washing for 3-5 min, taking out and washing with pure water;
B. and (3) preparing a 10-20% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step (A) into the aqueous solution for pickling for 90-100 s, taking out the ceramic substrate, cleaning the ceramic substrate with pure water, and drying the ceramic substrate at 80-120 ℃ for later use.
4. The method for improving the heat cycle reliability of the aluminum nitride coated aluminum packaging liner plate according to claim 1, which is characterized in that: in the step (3), the secondary zinc leaching step is as follows: preparing zinc dipping liquid by NaOH and ZnO, wherein the mass fraction of the NaOH is 10%, the mass fraction of the ZnO is 1.6%, and the balance is pure water, immersing the aluminum nitride aluminum-coated ceramic substrate treated in the step (2) for 40-45 s, and taking out the pure water for cleaning; immersing in 30% aqueous solution of nitric acid, pickling for 90-100 s, taking out pure water, and cleaning; placing the mixture in zinc leaching solution for secondary zinc leaching for 30-35 s, taking out, and cleaning with pure water for standby.
5. The method for improving the heat cycle reliability of the aluminum nitride coated aluminum packaging liner plate according to claim 1, which is characterized in that: in the step (3), the chemical nickel plating solution comprises 25g/L of NiSO 4 ·7H 2 NaH of O, 36g/L 2 PO 2 ·H 2 O, 12g/L Na 3 C 6 H 5 O 7 ·2H 2 O, the rest is pure water; wherein the pH value of the electroless nickel plating solution is 4.5-5.6.
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| PCT/CN2022/126137 WO2024060342A1 (en) | 2022-09-22 | 2022-10-19 | Method for improving thermal cycle reliability of aluminum nitride direct-bonded aluminum packaging substrate |
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| CN115595535B (en) * | 2022-12-14 | 2024-02-09 | 江苏富乐华半导体科技股份有限公司 | Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate |
| CN116429817A (en) * | 2023-05-05 | 2023-07-14 | 江苏富乐华半导体科技股份有限公司 | Thermal cycle testing device and method for aluminum nitride coated ceramic lining plate |
| CN117161323B (en) * | 2023-09-07 | 2024-01-30 | 江苏富乐华半导体科技股份有限公司 | Forming die for lining plate production and forming method thereof |
| CN117756555B (en) * | 2023-12-22 | 2024-09-03 | 江苏富乐华半导体科技股份有限公司 | A method for preparing a high-reliability aluminum nitride-coated aluminum substrate |
| CN118098989B (en) * | 2024-02-29 | 2024-12-17 | 江苏富乐华功率半导体研究院有限公司 | Preparation method of aluminum-coated aluminum nitride ceramic substrate double-sided heat dissipation power module |
| CN118206398B (en) * | 2024-03-20 | 2024-09-27 | 江苏富乐华功率半导体研究院有限公司 | A method for preparing aluminum nitride-coated aluminum ceramic substrate with surface enhancement |
| CN118835200B (en) * | 2024-06-27 | 2025-03-28 | 江苏富乐华功率半导体研究院有限公司 | A method for preparing a low thermal expansion coefficient aluminum-clad ceramic lining |
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| KR100528638B1 (en) * | 2003-07-30 | 2005-11-15 | 한국생산기술연구원 | Plating Process of Nickel on Magnesium Alloy |
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