CN115595535B - Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate - Google Patents

Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate Download PDF

Info

Publication number
CN115595535B
CN115595535B CN202211602440.5A CN202211602440A CN115595535B CN 115595535 B CN115595535 B CN 115595535B CN 202211602440 A CN202211602440 A CN 202211602440A CN 115595535 B CN115595535 B CN 115595535B
Authority
CN
China
Prior art keywords
ceramic substrate
aluminum nitride
aluminum
coated ceramic
nitride coated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202211602440.5A
Other languages
Chinese (zh)
Other versions
CN115595535A (en
Inventor
王斌
贺贤汉
欧阳鹏
武威
高远
管鹏飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Fulehua Semiconductor Technology Co ltd
Original Assignee
Jiangsu Fulehua Semiconductor Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Fulehua Semiconductor Technology Co ltd filed Critical Jiangsu Fulehua Semiconductor Technology Co ltd
Priority to CN202211602440.5A priority Critical patent/CN115595535B/en
Publication of CN115595535A publication Critical patent/CN115595535A/en
Application granted granted Critical
Publication of CN115595535B publication Critical patent/CN115595535B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3485Sputtering using pulsed power to the target
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5806Thermal treatment
    • C23C14/5813Thermal treatment using lasers
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5873Removal of material
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5873Removal of material
    • C23C14/588Removal of material by mechanical treatment

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Thermal Sciences (AREA)
  • Chemically Coating (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses a method for improving the heat cycle reliability of an aluminum nitride aluminum-coated ceramic substrate, which relates to the field of semiconductor processing and aims at solving the problem that the heat resistance of the aluminum nitride aluminum-coated ceramic substrate is insufficient, and the technical scheme is as follows: a method for improving the heat cycle reliability of an aluminum nitride coated ceramic substrate comprises the following steps: 1) Surface sputtering titanium plating: taking an aluminum nitride coated aluminum ceramic substrate for surface cleaning, and then plating titanium to obtain the aluminum nitride coated aluminum ceramic substrate with a nano-scale titanium layer, wherein the thickness of the titanium layer is 50-100nm; 2) Laser strengthening: taking the aluminum nitride coated ceramic substrate with the nano-level titanium layer in the step 1 for laser strengthening treatment; 3) Surface treatment: and (3) carrying out surface treatment on the aluminum nitride aluminum-coated ceramic substrate treated in the step (2). The method for improving the heat-resistant cycle reliability of the aluminum nitride coated ceramic substrate can effectively improve the heat-resistant cycle performance of the substrate.

Description

Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate
Technical Field
The invention relates to the field of semiconductor preparation, in particular to a method for improving the heat cycle reliability of an aluminum nitride coated ceramic substrate.
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 shaping, so that a bonding interface of aluminum and aluminum nitride ceramics has higher heat-resistant cycle reliability compared with a bonding interface of copper and aluminum nitride ceramics, but as the cycle number increases, the aluminum nitride aluminum-coated substrate prepared by adopting a liquid phase bonding method has large uneven size difference of the aluminum crystal grains on the surface, the crystal grains are easy to deform and slip, hillock shapes are generated on the surface of the substrate in a macroscopic manner, and the roughness is increased rapidly, so that the heat-resistant cycle reliability of the aluminum nitride aluminum-coated ceramic substrate is reduced. Under the practical application environment, hillocks and roughness on the surface of the DBA substrate are increased rapidly, the reliability of a welding layer between a chip and the substrate is affected, and a device is disabled in extreme cases, so that development of a method for improving the heat-resistant cycle reliability of the aluminum nitride aluminum-coated ceramic substrate and reducing the risk of the device is needed.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for improving the heat cycle reliability of an aluminum nitride aluminum-coated ceramic substrate, and the heat cycle resistance of the aluminum nitride aluminum-coated ceramic substrate is improved by titanium plating and then laser strengthening.
The technical aim of the invention is realized by the following technical scheme: a method for improving the heat cycle reliability of an aluminum nitride coated ceramic substrate comprises the following steps:
1) Surface sputtering titanium plating: taking an aluminum nitride coated aluminum ceramic substrate for surface cleaning, and then plating titanium to obtain the aluminum nitride coated aluminum ceramic substrate with a nano-scale titanium layer, wherein the thickness of the titanium layer is 50-100nm;
2) Laser strengthening: taking the aluminum nitride coated ceramic substrate with the nano-level titanium layer in the step 1 for laser strengthening treatment;
3) Surface treatment: and (3) carrying out surface treatment on the aluminum nitride aluminum-coated ceramic substrate treated in the step (2).
The invention is further provided with: in the step 1, the thickness of the aluminum layer on the surface of the aluminum nitride aluminum-coated ceramic substrate is 0.4-0.6 mm.
The invention is further provided with: in 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. preparing 10-20% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step A for pickling for 90-100 s, taking out, cleaning with pure water, and drying at 80-120 ℃ for later use.
The invention is further provided with: in the step (1), the titanizing process is a surface sputtering titanizing process, and the working parameters are as follows: the power is 5KW, the Ar flow is 30Sccm, the temperature of a sputtering substrate is 200-300 ℃, the frequency pulse current is sputtered, the current output mode is sine wave output, the sputtering pressure is 0.3Pa, and the sputtering time is 10min.
The invention is further provided with: step 2, the laser strengthening treatment process parameters are as follows: the laser power is 8-12KW, the scanning speed is 20-25 mm/s, and the spot diameter is 0.25-0.5 mm.
The invention is further provided with: in the step 3, the surface treatment process comprises the following steps: the aluminum nitride coated ceramic substrate is subjected to surface grinding, and then to alkali washing treatment and acid washing treatment.
The invention is further provided with: the surface treatment steps are as follows:
s1, mechanically grinding the substrate after the treatment in the step 2 to remove surface impurities;
s2, preparing a 20% sodium hydroxide aqueous solution, taking the aluminum nitride aluminum-coated ceramic substrate in the step S1, immersing the ceramic substrate in alkali washing for 10-15S, taking out the ceramic substrate and washing the ceramic substrate with pure water;
s3, preparing 40-50% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step S2 into the aqueous solution, pickling for 90-100S, taking out the ceramic substrate, and cleaning the ceramic substrate with pure water to obtain the aluminum nitride coated ceramic substrate.
The invention is further provided with: the amount of the mechanical grinding chip is 5-10 mu m.
The invention is further provided with: in the step 2, remelting and solidifying the aluminum on the surface of the aluminum nitride aluminum-coated ceramic substrate after laser strengthening, wherein the remelting and solidifying depth is 80 mu m; and (3) refining surface grains after remelting and solidification, wherein the average grain size is 32 mu m.
In summary, the invention has the following beneficial effects: the invention provides a method for improving the heat-resistant cycle reliability of an aluminum nitride aluminum-coated ceramic substrate, which comprises the steps of sputtering titanium on the surface of the aluminum nitride aluminum-coated ceramic substrate, strengthening by laser, introducing trace titanium elements into the surface layer of aluminum to form a uniform titanium aluminum solid solution hardening layer, and then carrying out surface treatment on the aluminum solid solution hardening layer.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a sample surface grain structure diagram of the first embodiment;
FIG. 3 is a diagram showing the grain structure of the surface of the sample of comparative example one.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
A method for improving the heat cycle reliability of an aluminum nitride coated ceramic substrate, as shown in the flow chart of figure 1, specifically comprises the following steps:
1) Surface sputtering titanium plating: taking an aluminum nitride coated aluminum ceramic substrate for surface cleaning, and then plating titanium to obtain the aluminum nitride coated aluminum ceramic substrate with a nano-scale titanium layer, wherein the thickness of the titanium layer is 50-100nm;
2) Laser strengthening: taking the aluminum nitride coated ceramic substrate with the nano-level titanium layer in the step 1 for laser strengthening treatment;
3) Surface treatment: and (3) carrying out surface treatment on the aluminum nitride aluminum-coated ceramic substrate treated in the step (2).
Wherein, in the step 1, the thickness of the aluminum layer on the surface of the aluminum nitride aluminum-coated ceramic substrate is 0.4-0.6 mm.
The titanizing process is a surface sputtering titanizing process, and the working parameters are as follows: the power is 5KW, the Ar flow is 30Sccm, the temperature of a sputtering substrate is 200-300 ℃, the frequency pulse current is sputtered, the current output mode is sine wave output, and the sputtering pressure is 0.3Pa for 10min;
in 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. preparing 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;
in the step 2, the laser strengthening treatment process parameters are as follows: the laser power is 8-12KW, the scanning speed is 20-25 mm/s, and the spot diameter is 0.25-0.5 mm;
in the step 2, the aluminum on the surface of the aluminum nitride aluminum-coated ceramic substrate after laser strengthening is remelted and solidified to the depth of the influencing layer of 50-100 mu m; and (3) refining surface grains after remelting and solidification, wherein the average grain size is 20-50 mu m.
In the step 3, the surface treatment process comprises the following steps: grinding the surface of the aluminum nitride coated ceramic substrate, and then performing alkali washing treatment and acid washing treatment;
the specific processing steps are as follows:
s1, mechanically grinding the substrate after the treatment in the step 2 to remove surface impurities, wherein the amount of mechanically ground chips is 5-10 mu m;
s2, preparing a 20% sodium hydroxide aqueous solution, taking the aluminum nitride aluminum-coated ceramic substrate in the step S1, immersing the ceramic substrate in alkali washing for 10-15S, taking out the ceramic substrate and washing the ceramic substrate with pure water;
s3, preparing 40-50% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step S2 into the aqueous solution, pickling for 90-100S, taking out the ceramic substrate, and cleaning the ceramic substrate with pure water to obtain the aluminum nitride coated ceramic substrate.
In the step 3, after the surface treatment is finished, an aluminum nitride aluminum-coated ceramic substrate with a surface fine crystal strengthening layer is obtained;
compared with the prior art, the method for improving the heat-resistant cycle reliability of the aluminum nitride coated ceramic substrate comprises the steps of firstly, carrying out surface sputtering titanium plating treatment and laser strengthening treatment on the surface of the aluminum nitride coated ceramic substrate, introducing a fine crystal strengthening layer on the surface layer of the aluminum nitride coated ceramic substrate, controlling the laser strengthening power and the depth of a strengthening fine crystal area, finally enabling the surface layer of the aluminum nitride coated ceramic substrate to be a fine crystal strengthening area, enabling the inner layer to be a coarse crystal area, inhibiting the sliding and deformation of surface aluminum grains in the fine crystal area, macroscopically representing surface strengthening, eliminating hillock-shaped protrusions under a cold and hot cycle working environment, inhibiting the roughness from increasing sharply, and obviously improving the welding reliability between a chip and the aluminum nitride coated ceramic substrate.
Embodiment one:
(1) Surface sputtering titanium plating: taking an aluminum nitride aluminum-coated ceramic substrate for surface cleaning, and then plating titanium to obtain the aluminum nitride aluminum-coated ceramic substrate with a nano-scale titanium layer, wherein the thickness of the titanium-plated layer is 100nm;
(2) Laser strengthening: taking the aluminum nitride coated ceramic substrate with the nano-level titanium layer in the step (1) for laser strengthening treatment;
(3) Surface treatment: and (3) carrying out surface treatment on the aluminum nitride aluminum-coated ceramic substrate treated in the step (2).
Wherein, the thickness of the aluminum layer on the surface of the aluminum nitride aluminum-coated ceramic substrate is 0.4mm.
The titanizing process is a surface sputtering titanizing process, and the working parameters are as follows: the power is 5KW, the Ar flow is 30Sccm, the temperature of a sputtering substrate is 200-300 ℃, the frequency pulse current is sputtered, the current output mode is sine wave output, and the sputtering pressure is 0.3Pa for 10min;
the surface cleaning steps are as follows:
A. preparing 10-20% sodium hydroxide aqueous solution, immersing the aluminum nitride aluminum-coated ceramic substrate into alkaline washing for 3min, taking out and washing with pure water;
B. preparing a 20% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step A into the solution for pickling for 90s, taking out the substrate, cleaning the substrate with pure water, and drying the substrate with hot air at 80 ℃ for later use;
in the step (2), the laser strengthening treatment process parameters are as follows: laser power 8KW, scanning speed 25mm/s, and spot diameter 0.25mm;
remelting and solidifying the aluminum on the surface of the aluminum nitride aluminum-coated ceramic substrate after laser strengthening to ensure that the depth of the influence layer is 80 mu m; and (3) refining surface grains after remelting and solidification, wherein the average grain size is 32 mu m.
The surface treatment process comprises the following steps: grinding the surface of the aluminum nitride coated ceramic substrate, and then performing alkali washing treatment and acid washing treatment;
the specific processing steps are as follows:
A. mechanically grinding the substrate after the treatment in the step (2) to remove surface impurities, wherein the amount of mechanically ground chips is 5 mu m;
B. preparing a 20% sodium hydroxide aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step A into alkali washing for 10s, taking out and washing with pure water.
C. Preparing 40% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step B into acid washing for 90s, taking out and washing with pure water to obtain the aluminum nitride coated ceramic substrate.
And after the surface treatment is finished, obtaining the aluminum nitride aluminum-coated ceramic substrate with the surface fine crystal strengthening layer.
Embodiment two:
(1) Surface sputtering titanium plating: taking an aluminum nitride aluminum-coated ceramic substrate for surface cleaning, and then plating titanium to obtain the aluminum nitride aluminum-coated ceramic substrate with a nano-scale titanium layer, wherein the thickness of the titanium-plated layer is 80nm;
(2) Laser strengthening: taking the aluminum nitride coated ceramic substrate with the nano-level titanium layer in the step (1) for laser strengthening treatment;
(3) Surface treatment: and (3) carrying out surface treatment on the aluminum nitride aluminum-coated ceramic substrate treated in the step (2).
In the step (1), the thickness of the aluminum layer on the surface of the aluminum nitride aluminum-coated ceramic substrate is 0.4mm.
The titanizing process is a surface sputtering titanizing process, and the working parameters are as follows: the power is 5KW, the Ar flow is 30Sccm, the temperature of a sputtering substrate is 200-300 ℃, the frequency pulse current is sputtered, the current output mode is sine wave output, and the sputtering pressure is 0.3Pa for 10min;
the surface cleaning steps are as follows:
A. preparing 10-20% sodium hydroxide aqueous solution, immersing the aluminum nitride aluminum-coated ceramic substrate into alkaline washing for 3min, taking out and washing with pure water;
B. preparing a 20% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step A into the solution for pickling for 90s, taking out the substrate, cleaning the substrate with pure water, and drying the substrate with hot air at 80 ℃ for later use;
in the step (2), the laser strengthening treatment process parameters are as follows: laser power 8KW, scanning speed 25mm/s, and spot diameter 0.25mm;
remelting and solidifying the aluminum on the surface of the aluminum nitride aluminum-coated ceramic substrate after laser strengthening to ensure that the depth of the influence layer is 80 mu m; and (3) refining surface grains after remelting and solidification, wherein the average grain size is 40 mu m.
The surface treatment process comprises the following steps: grinding the surface of the aluminum nitride coated ceramic substrate, and then performing alkali washing treatment and acid washing treatment;
the method comprises the following specific steps:
A. mechanically grinding the substrate after the treatment in the step (2) to remove surface impurities, wherein the amount of mechanically ground chips is 5 mu m;
B. preparing a 20% sodium hydroxide aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step A into alkali washing for 10s, taking out and washing with pure water;
C. preparing 40% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step B into acid washing for 90s, taking out and washing with pure water to obtain the aluminum nitride coated ceramic substrate.
And after the surface treatment is finished, obtaining the aluminum nitride aluminum-coated ceramic substrate with the surface fine crystal strengthening layer.
Comparative example one:
the first comparative example is a non-fine grain reinforced aluminum nitride aluminum coated ceramic substrate, and the thickness of the aluminum layer is 0.4mm.
The substrates of the first embodiment, the second embodiment and the first comparative embodiment are respectively subjected to a grain size and a thermal cycle test at-55/150 ℃ for 200 times, and the surface roughness test is carried out on the substrates, wherein the thermal cycle test conditions are as follows: in a temperature cycle test box (brand: aispeck; model: TSE-122-A), placing a sample at-55deg.C for 30min, placing at 150deg.C for 30min for 1 cycle, and performing repeated thermal cycle test, wherein the intermediate temperature conversion time is less than 60S, and the temperature deviation range is + -2deg.C; the roughness test method comprises the following steps: placing the sample on a marble horizontal table, detecting the surface roughness value by using a contact pin type roughness tester (manufacturer: tokyo precision instrument factory; model specification: mahr M310), taking the Ra value, and detecting the result as follows;
and fig. 2 is a sample surface grain structure diagram of the first embodiment, and fig. 3 is a sample surface grain structure diagram of the first comparative embodiment, which can be obviously compared, the sample prepared by the method has the advantages of significantly reduced surface grains, small roughness change after thermal cycle test, and significantly improved surface reliability.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.

Claims (6)

1. A method for improving the heat cycle reliability of an aluminum nitride coated ceramic substrate, comprising the steps of:
1) Surface sputtering titanium plating: taking an aluminum nitride coated aluminum ceramic substrate for surface cleaning, and then plating titanium to obtain the aluminum nitride coated aluminum ceramic substrate with a nano-scale titanium layer, wherein the thickness of the titanium layer is 50-100nm;
2) Laser strengthening: carrying out laser strengthening treatment on the aluminum nitride coated ceramic substrate with the nano-level titanium layer in the step 1, and carrying out aluminum remelting solidification on the surface of the aluminum nitride coated ceramic substrate after laser strengthening, wherein the remelting solidification depth is 80 mu m; refining surface grains after remelting and solidification, wherein the average grain size is 32 mu m;
3) Surface treatment: carrying out surface treatment on the aluminum nitride aluminum-coated ceramic substrate treated in the step 2;
in the step 1), the titanizing process is a surface sputtering titanizing process, and the working parameters are as follows: the power is 5KW, the Ar flow is 30Sccm, the temperature of a sputtering substrate is 200-300 ℃, the frequency pulse current is sputtered, the current output mode is sine wave output, the sputtering pressure is 0.3Pa, and the sputtering time is 10min;
in the step 2), the laser strengthening treatment process parameters are as follows: the laser power is 8-12KW, the scanning speed is 20-25 mm/s, and the spot diameter is 0.25-0.5 mm.
2. The method for improving the heat cycle reliability of the aluminum nitride coated ceramic substrate according to claim 1, wherein the method comprises the following steps: in the step 1, the thickness of the aluminum layer on the surface of the aluminum nitride aluminum-coated ceramic substrate is 0.4-0.6 mm.
3. The method for improving the heat cycle reliability of the aluminum nitride coated ceramic substrate according to claim 1, wherein the method comprises the following steps: in 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. preparing 10-20% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step A for pickling for 90-100 s, taking out, cleaning with pure water, and drying at 80-120 ℃ for later use.
4. The method for improving the heat cycle reliability of the aluminum nitride coated ceramic substrate according to claim 1, wherein the method comprises the following steps: in the step 3, the surface treatment process comprises the following steps: the aluminum nitride coated ceramic substrate is subjected to surface grinding, and then to alkali washing treatment and acid washing treatment.
5. The method for improving the heat cycle reliability of an aluminum nitride coated ceramic substrate according to claim 4, wherein the surface treatment step comprises:
s1, mechanically grinding the substrate after the treatment in the step 2 to remove surface impurities;
s2, preparing a 20% sodium hydroxide aqueous solution, taking the aluminum nitride aluminum-coated ceramic substrate in the step S1, immersing the ceramic substrate in alkali washing for 10-15S, taking out the ceramic substrate and washing the ceramic substrate with pure water;
s3, preparing 40-50% nitric acid aqueous solution, immersing the aluminum nitride coated ceramic substrate in the step S2 into the aqueous solution, pickling for 90-100S, taking out the ceramic substrate, and cleaning the ceramic substrate with pure water to obtain the aluminum nitride coated ceramic substrate.
6. The method for improving the heat cycle reliability of the aluminum nitride coated ceramic substrate according to claim 5, wherein the method comprises the following steps: the amount of the mechanical grinding chip is 5-10 mu m.
CN202211602440.5A 2022-12-14 2022-12-14 Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate Active CN115595535B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211602440.5A CN115595535B (en) 2022-12-14 2022-12-14 Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211602440.5A CN115595535B (en) 2022-12-14 2022-12-14 Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate

Publications (2)

Publication Number Publication Date
CN115595535A CN115595535A (en) 2023-01-13
CN115595535B true CN115595535B (en) 2024-02-09

Family

ID=84853859

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211602440.5A Active CN115595535B (en) 2022-12-14 2022-12-14 Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate

Country Status (1)

Country Link
CN (1) CN115595535B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115394658A (en) * 2022-10-27 2022-11-25 江苏富乐华功率半导体研究院有限公司 Surface treatment process of DPC ceramic substrate
CN115410925A (en) * 2022-09-22 2022-11-29 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 aluminum-coated packaging lining plate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115410925A (en) * 2022-09-22 2022-11-29 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 aluminum-coated packaging lining plate
CN115394658A (en) * 2022-10-27 2022-11-25 江苏富乐华功率半导体研究院有限公司 Surface treatment process of DPC ceramic substrate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
铝合金表面激光熔覆tial合金涂层的性能研究;杨智成;《广西大学学位论文》;第9、10、13、14、27、28页 *

Also Published As

Publication number Publication date
CN115595535A (en) 2023-01-13

Similar Documents

Publication Publication Date Title
CN115595535B (en) Method for improving heat cycle reliability of aluminum nitride coated ceramic substrate
CN106475679B (en) A kind of discontinuous pressure process diffusion connecting process of unrepeatered transmission of copper and aluminium alloy
CN101279401B (en) Pressure welding method of large-area target material
CN102248278A (en) Magnesium alloy and aluminum alloy interlayer diffusion welding method
CN101537533A (en) Welding structure and method of target and backing plate
CN103949472B (en) A kind of copper-molybdenum copper-copper three layer composite plate and manufacture method thereof
CN111320487A (en) Silicon nitride ceramic surface modification auxiliary direct diffusion connection method
CN101862922B (en) Binary alloy sealing solder wire
CN115626835A (en) Manufacturing method of ceramic-based copper-clad plate and product thereof
CN110335798B (en) Diamond energy transmission window and preparation method thereof
CN112355427A (en) Method for welding magnesium oxide target and back plate
CN111254398A (en) Platinum sputtering target with high oriented grain and preparation method thereof
CN113501725B (en) Preparation method of aluminum-coated ceramic insulating lining plate
CN110634757B (en) Welding process for wafer back copper coating
CN112225567A (en) Method for preparing molybdenum silicide coating by slurry sintering
CN113774339B (en) Aluminum-silicon target material and preparation method thereof
CN114645253B (en) Semiconductor tantalum target and forging method thereof
CN112894111B (en) Diffusion welding method of high-scandium-content aluminum-scandium alloy target material and prepared welding assembly
CN109400206A (en) A kind of method of ceramic surface metallization
CN113817997A (en) High-purity alloy aluminum target material and preparation method thereof
CN103496215A (en) Embedded type combined heat sink as well as preparation method thereof
CN103692151A (en) Manufacturing method for titanium focusing ring
CN101733591A (en) Method for manufacturing bright aluminum alloy welding wire
CN114951880B (en) Method for welding three-layer ceramic target
CN113667945B (en) Preparation method of oxygen-free copper backboard with water channel

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant