CN117756555A - Preparation method of high-reliability aluminum nitride aluminum-coated substrate - Google Patents
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- CN117756555A CN117756555A CN202311775182.5A CN202311775182A CN117756555A CN 117756555 A CN117756555 A CN 117756555A CN 202311775182 A CN202311775182 A CN 202311775182A CN 117756555 A CN117756555 A CN 117756555A
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 103
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 88
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000000758 substrate Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 58
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005266 casting Methods 0.000 claims abstract description 11
- 238000005121 nitriding Methods 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000000227 grinding Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 abstract description 2
- 230000017525 heat dissipation Effects 0.000 abstract description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000002344 surface layer Substances 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 description 12
- 238000005219 brazing Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000007788 liquid Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
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Abstract
The invention relates to the field of semiconductors, in particular to a preparation method of a high-reliability aluminum nitride aluminum-coated substrate. The method carries out alkali treatment and accelerated aging treatment on the aluminum nitride ceramic to hydrolyze and convert the aluminum hydroxide on the surface layer of the aluminum nitride ceramic into a uniform aluminum oxide film layer. And then nitriding and sintering are carried out, and an aluminum oxynitride layer is formed on the surface of the aluminum nitride ceramic. And then placing the treated aluminum nitride ceramic in a forming die, and casting and sintering to obtain the high-reliability aluminum nitride coated substrate. The high-reliability aluminum nitride aluminum-coated substrate prepared by the method has the advantages of strong reliability, low thermal resistance, good heat resistance, ceramic strength enhancement and capability of meeting the packaging heat dissipation requirement.
Description
Technical Field
The invention relates to the field of semiconductors, in particular to a preparation method of a high-reliability aluminum nitride aluminum-coated substrate.
Background
In recent years, IGBT high-power device modules are coming into the view of people, and ceramic substrates are an indispensable ring, and their performance becomes one of important performances of IGBT modules. The direct bond copper substrates (Direct Bonding Copper, DBC) and the active metal brazing substrates (Active Metal Brazing, AMB) are currently the most common two ceramic substrates on the market, and have the characteristics of high thermal conductivity, high mechanical strength, low expansion coefficient and the like, but as the working temperature is changed, copper forms a large amount of residual stress at the ceramic substrate, so that cracks are generated at the interface of the ceramic substrate. Compared with copper, the high plasticity and lower yield strength of aluminum can effectively buffer the thermal stress caused by the temperature transformation of the substrate, so that the reliability of the interface is enhanced to a certain extent, the Direct bonding aluminum substrate (Direct BondingAluminum, DBA) is unique in the high reliability direction, but under the extreme working temperature condition, the thermal fatigue can also occur at the interface of the aluminum nitride aluminum-coated substrate after multiple cold and hot transformations, and the stress is accumulated to form cracks at the ceramic interface.
In order to overcome the defects of the prior art, the invention provides a preparation method of a high-reliability aluminum nitride aluminum-coated substrate.
Disclosure of Invention
The invention aims to provide a preparation method of a high-reliability aluminum nitride aluminum-coated substrate, which aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a high-reliability aluminum nitride coated aluminum substrate comprises the following steps:
step one: placing aluminum nitride ceramics in a sodium hydroxide solution, taking out the aluminum nitride ceramics after ultrasonic cleaning, aging the aluminum nitride ceramics for 96-120 hours at the temperature of 120-140 ℃ under the humidity of 98-100%, washing with pure water after the reaction is finished, and drying to obtain pretreated aluminum nitride ceramics;
step two: nitriding and sintering the pretreated aluminum nitride ceramic in a nitrogen environment, cooling along with a furnace after sintering is finished, and forming an aluminum oxynitride layer on the surface;
step three: and (3) placing the aluminum nitride ceramic treated in the second step in a forming die, placing a high-purity aluminum block at the upper end of a pouring gate of the die, pouring and sintering at 660-950 ℃ for 60-120min after clamping, cooling with a furnace after sintering, forming a metal aluminum layer on the surface, and demoulding, cutting, grinding and repairing the plate to obtain the high-reliability aluminum nitride coated aluminum substrate.
More preferably, in step one, the concentration of the sodium hydroxide solution is 1-3g/L.
More preferably, in the first step, the ultrasonic cleaning parameters: the temperature is 40-60 ℃ and the time is 30-60s.
More optimally, in the second step, nitriding sintering process parameters: the temperature is 1500-1800 ℃, the time is 60-120min, and the gas pressure is 1-5MPa.
More preferably, in the second step, the thickness of the aluminum oxynitride layer is 0.5-3.0 μm.
More preferably, in the third step, the vacuum degree is 0.001-0.01Pa during casting and sintering.
The invention has the beneficial effects that:
the invention provides a preparation method of a high-reliability aluminum nitride coated substrate, which is mainly prepared by an aluminum oxynitride layer on the surface of aluminum nitride ceramic, wherein the surface of the aluminum nitride ceramic is subjected to alkaline treatment by adopting sodium hydroxide solution, aging treatment is accelerated, so that the surface aluminum hydroxide is hydrolyzed and converted into a uniform aluminum oxide film layer, and then a layer of aluminum oxynitride film is formed on the surface of the aluminum nitride ceramic by nitriding and sintering. The aluminum oxynitride layer generated on the surface of the aluminum nitride ceramic has high strength, high reliability in combination with the aluminum nitride ceramic, and can be used for optimally controlling the thickness of the aluminum oxynitride layer, so that the ceramic strength can be further enhanced under the heat dissipation condition meeting the packaging requirement, and the aluminum liquid is adopted for high-temperature direct infiltration molding, so that a direct ceramic aluminum-coated interface can be directly formed, the thermal resistance is lower, and the reliability is higher.
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 flow chart of a method for manufacturing a high-reliability aluminum nitride coated substrate according to the present invention;
FIG. 2 is a schematic diagram of an interface structure layer of a high reliability aluminum nitride aluminum-clad substrate according to embodiment 1 of the present invention;
FIG. 3 is a cross-sectional SEM image of a highly reliable aluminum nitride coated substrate according to example 5;
in fig. 2: 1-metallic aluminum layer, 2-aluminum oxynitride layer, 3-aluminum nitride ceramic.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely in connection with the embodiments of the present invention, and it is apparent that the described embodiments 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.
The raw material sources are as follows:
aluminum nitride ceramics, available from Hai God technology Co., ltd., are 138X 190X 0.635mm in size.
Example 1: step one: placing aluminum nitride ceramic 3 with the size of 138 multiplied by 190 multiplied by 0.635mm in sodium hydroxide solution with the concentration of 3g/L, immersing and washing for 60s under the conditions that the reaction temperature is 55 ℃ and the ultrasonic frequency is 20KHz, taking out, placing in an accelerated aging box, keeping the humidity at 100 percent, maintaining at 130 ℃ for 96 hours, washing with pure water at 25 ℃ after the reaction is finished, and drying to obtain pretreated aluminum nitride ceramic;
step two: in a nitrogen environment, heating the pretreated aluminum nitride ceramic to 1800 ℃ at a heating rate of 10 ℃/min, nitriding and sintering for 120min under the conditions that the temperature is 1800 ℃ and the gas pressure is 3.5MPa, cooling along with a furnace after sintering is finished, and forming an aluminum oxynitride layer 2 with the thickness of 3 mu m on the surface;
step three: placing the aluminum nitride ceramic treated in the second step into a forming die, and placing a high-purity aluminum block with the mass of 62.5g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; and (3) placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 750 ℃ for 120min, wherein the sintering vacuum degree is 0.0026Pa, cooling along with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out a product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment by sequentially using 800# and 1200# grinding liquid to obtain the high-reliability aluminum nitride coated aluminum substrate.
Example 2: step one: placing aluminum nitride ceramic 3 with the size of 138 multiplied by 190 multiplied by 0.635mm in sodium hydroxide solution with the concentration of 4g/L, immersing and washing for 60s under the conditions that the reaction temperature is 52 ℃ and the ultrasonic frequency is 20KHz, taking out, placing in an accelerated aging box, keeping the humidity at 99.3 percent, maintaining at 125 ℃ for 97 hours, washing with pure water at 25 ℃ after the reaction is finished, and drying to obtain pretreated aluminum nitride ceramic;
step two: in a nitrogen environment, heating the pretreated aluminum nitride ceramic to 1800 ℃ at a heating rate of 10 ℃/min, nitriding and sintering for 120min under the conditions that the temperature is 1800 ℃ and the gas pressure is 2.8MPa, cooling along with a furnace after sintering is finished, and forming an aluminum oxynitride layer 2 with the thickness of 2.8 mu m on the surface;
step three: placing the aluminum nitride ceramic treated in the second step into a forming die, and placing a high-purity aluminum block with the mass of 68.3g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; and (3) placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 750 ℃ for 120min, wherein the sintering vacuum degree is 0.0035Pa, cooling along with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out a product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment by sequentially using 800# and 1200# grinding liquid to obtain the high-reliability aluminum nitride coated aluminum substrate.
Example 3: step one: placing aluminum nitride ceramic 3 with the size of 138 multiplied by 190 multiplied by 0.635mm in sodium hydroxide solution with the concentration of 2.9g/L, immersing and washing for 60s under the conditions that the reaction temperature is 56 ℃ and the ultrasonic frequency is 20KHz, taking out, placing in an accelerated aging box, keeping the humidity at 100 percent, maintaining at 130 ℃ for 93 hours, washing with pure water at 25 ℃ after the reaction is finished, and drying to obtain pretreated aluminum nitride ceramic;
step two: heating the pretreated aluminum nitride ceramic to 1780 ℃ at a heating rate of 10 ℃/min in a nitrogen environment, nitriding and sintering for 120min at 1780 ℃ under the condition of a gas pressure of 4.1MPa, cooling along with a furnace after sintering is finished, and forming an aluminum oxynitride layer 2 with a thickness of 3.2 mu m on the surface;
step three: placing the aluminum nitride ceramic treated in the second step into a forming die, and placing a high-purity aluminum block with the mass of 65.7g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; and (3) placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 750 ℃ for 120min, wherein the sintering vacuum degree is 0.0053Pa, cooling along with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out a product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment by sequentially using 800# and 1200# grinding liquid to obtain the high-reliability aluminum nitride coated aluminum substrate.
Example 4: step one: placing aluminum nitride ceramic 3 with the size of 138 multiplied by 190 multiplied by 0.635mm in sodium hydroxide solution with the concentration of 3g/L, immersing and washing for 60s under the conditions that the reaction temperature is 58 ℃ and the ultrasonic frequency is 20KHz, taking out, placing in an accelerated aging box, keeping the humidity at 98.3 percent for 90 hours at 120 ℃, washing with pure water at 25 ℃ after the reaction is finished, and drying to obtain pretreated aluminum nitride ceramic;
step two: heating the pretreated aluminum nitride ceramic to 1750 ℃ at a heating rate of 10 ℃/min in a nitrogen environment, nitriding and sintering for 120min at a temperature of 1750 ℃ and a gas pressure of 4.8MPa, cooling with a furnace after sintering is finished, and forming an aluminum oxynitride layer 2 with a thickness of 3 mu m on the surface;
step three: placing the aluminum nitride ceramic treated in the second step into a forming die, and placing a high-purity aluminum block with the mass of 60.2g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 745 ℃ for 120min, wherein the sintering vacuum degree is 0.0033Pa, cooling along with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out a product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment by using 800# and 1200# grinding liquid in sequence to obtain the high-reliability aluminum nitride coated aluminum substrate.
Example 5: step one: placing aluminum nitride ceramic 3 with the size of 138 multiplied by 190 multiplied by 0.635mm in sodium hydroxide solution with the concentration of 3g/L, immersing and washing for 60s under the conditions that the reaction temperature is 52 ℃ and the ultrasonic frequency is 20KHz, taking out, placing in an accelerated aging box, keeping the humidity at 98.9 percent and the temperature at 120 ℃ for 90 hours, washing with pure water at 25 ℃ after the reaction is finished, and drying to obtain pretreated aluminum nitride ceramic;
step two: in a nitrogen environment, heating the pretreated aluminum nitride ceramic to 1700 ℃ at a heating rate of 10 ℃/min, nitriding and sintering for 120min under the conditions that the temperature is 1700 ℃ and the gas pressure is 2.6MPa, cooling along with a furnace after sintering is finished, and forming an aluminum oxynitride layer 2 with the thickness of 1.3 mu m on the surface;
step three: placing the aluminum nitride ceramic treated in the second step into a forming die, and placing a high-purity aluminum block with the mass of 66.1g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; and (3) placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 780 ℃ for 120min, wherein the sintering vacuum degree is 0.0065Pa, cooling along with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out a product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment sequentially by using 800# and 1200# grinding liquid to obtain the high-reliability aluminum nitride coated aluminum substrate, wherein a Scanning Electron Microscope (SEM) image of the section aluminum oxynitride layer is shown in the following figure 3.
Comparative example 1: the preparation of the aluminum nitride coated substrate is carried out by selecting an aluminum nitride ceramic wafer which is not subjected to surface treatment, and the specific steps are as follows: placing untreated aluminum nitride ceramic 3 into a forming die, and placing a high-purity aluminum block with the mass of 58.2g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; and (3) placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 750 ℃ for 120min, wherein the sintering vacuum degree is 0.0026Pa, cooling along with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out a product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment by using 800# and 1200# grinding liquid in sequence to obtain the aluminum nitride coated aluminum substrate.
Comparative example 2: the preparation of the aluminum nitride coated substrate is carried out by selecting an aluminum nitride ceramic wafer which is not subjected to surface treatment, and the specific steps are as follows: placing untreated aluminum nitride ceramic 3 into a forming die, and placing a high-purity aluminum block with the mass of 65.3g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; and (3) placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 750 ℃ for 120min, wherein the sintering vacuum degree is 0.0068Pa, cooling along with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out a product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment by using 800# and 1200# grinding liquid in sequence to obtain the aluminum nitride coated aluminum substrate.
Comparative example 3: the preparation of the aluminum nitride coated substrate is carried out by selecting an aluminum nitride ceramic wafer which is not subjected to surface treatment, and the specific steps are as follows: placing untreated aluminum nitride ceramic 3 into a forming die, and placing a high-purity aluminum block with the mass of 59.1g, which is subjected to surface treatment and is subjected to oxide layer removal, at the upper end of a pouring gate of the die; and (3) placing the aluminum nitride coated aluminum sample subjected to clamping in a vacuum brazing furnace, casting and sintering at 750 ℃ for 120min, cooling with the furnace after sintering, forming a metal aluminum layer 1 on the surface, taking out the product, demolding, cutting and grinding an aluminum overflow area at the edge of the aluminum nitride coated aluminum lining plate after demolding, and then carrying out plate repairing treatment by using 800# and 1200# grinding liquid in sequence to obtain the high-reliability aluminum nitride coated aluminum substrate.
Detection test:
flexural Strength test: the aluminum nitride aluminum-coated substrate prepared by the method is used as a sample to be measured, and a sample with the size of 24.0mm x 42.0mm is obtained after laser cutting. Placing a sample in a universal testing machine, performing bending strength test by adopting a three-point bending method, positioning the sample between two lower rollers and an upper roller, wherein the upper roller is positioned in the midspan, and the relative movement of the upper roller and the lower roller enables the sample to generate bending fracture to measure corresponding values; the test values are shown in the following table.
Cold and hot cycle test: taking the aluminum nitride aluminum-coated substrate prepared by the method as a sample, carrying out ultrasonic nondestructive testing on the interface void ratio of the sample, selecting a qualified sample area with the void ratio, carrying out cold and hot circulation testing, wherein the allowable deviation range of the temperature is +/-2 ℃ in a testing area of-55 ℃ to 150 ℃, carrying out ultrasonic interface testing on the sample after every 100 times of high and low temperature circulation, and the testing results are shown in the following table.
| Flexural Strength/MPa | Cold and hot cycle test | |
| Example 1 | 536 | More than or equal to 3500 times |
| Example 2 | 512 | More than or equal to 3500 times |
| Example 3 | 554 | More than or equal to 3500 times |
| Example 4 | 514 | More than or equal to 3500 times |
| Example 5 | 502 | More than or equal to 3500 times |
| Comparative example 1 | 460 | Less than or equal to 2000 times |
| Comparative example 2 | 479 | Less than or equal to 2000 times |
| Comparative example 3 | 454 | Less than or equal to 2000 times |
Conclusion: the experiment shows that the aluminum nitride ceramic can obviously improve the bonding reliability of aluminum nitride and an aluminum layer in the aluminum oxynitride layer prepared by surface treatment sintering, the cold and hot cycle times are more than or equal to 3500 times, the untreated sample is less than or equal to 2000 times, and the interface reliability of the aluminum nitride coated aluminum substrate is obviously 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 (7)
1. A preparation method of a high-reliability aluminum nitride coated aluminum substrate is characterized by comprising the following steps of: the method comprises the following steps:
step one: placing the aluminum nitride ceramic (3) in a sodium hydroxide solution, taking out the aluminum nitride ceramic after ultrasonic cleaning, placing the aluminum nitride ceramic under 98-100% humidity, aging for 96-120h at 120-140 ℃, washing with pure water after the reaction is finished, and drying to obtain pretreated aluminum nitride ceramic;
step two: nitriding and sintering the pretreated aluminum nitride ceramic in a nitrogen environment, cooling along with a furnace after sintering is finished, and forming an aluminum oxynitride layer (2) on the surface;
step three: and (3) placing the aluminum nitride ceramic treated in the second step in a forming die, placing a high-purity aluminum block at the upper end of a pouring gate of the die, pouring and sintering at 660-950 ℃ for 60-120min after clamping, cooling with a furnace after sintering, forming a metal aluminum layer (1) on the surface, and demoulding, cutting, grinding and repairing the plate to obtain the high-reliability aluminum nitride coated substrate.
2. The method for manufacturing a highly reliable aluminum nitride coated substrate according to claim 1, wherein: in the first step, the concentration of the sodium hydroxide solution is 1-3g/L.
3. The method for manufacturing a highly reliable aluminum nitride coated substrate according to claim 1, wherein: in the first step, ultrasonic cleaning parameters: the temperature is 40-60 ℃ and the time is 30-60s.
4. The method for manufacturing a highly reliable aluminum nitride coated substrate according to claim 1, wherein: in the second step, nitriding sintering process parameters: the temperature is 1500-1800 ℃, the time is 60-120min, and the gas pressure is 1-5MPa.
5. The method for manufacturing a highly reliable aluminum nitride coated substrate according to claim 1, wherein: in the second step, the thickness of the aluminum oxynitride layer (2) is 0.5-3.0 mu m.
6. The method for manufacturing a highly reliable aluminum nitride coated substrate according to claim 1, wherein: in the third step, the vacuum degree is 0.001-0.01Pa when casting and sintering.
7. A highly reliable aluminum nitride coated substrate, characterized in that it is prepared by the preparation method according to any one of claims 1 to 6.
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