CN102560488B - DBC (Direct Bonded Copper) substrate surface treatment process based on nano-silver soldering paste connecting chip - Google Patents
DBC (Direct Bonded Copper) substrate surface treatment process based on nano-silver soldering paste connecting chip Download PDFInfo
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- CN102560488B CN102560488B CN201210023335.6A CN201210023335A CN102560488B CN 102560488 B CN102560488 B CN 102560488B CN 201210023335 A CN201210023335 A CN 201210023335A CN 102560488 B CN102560488 B CN 102560488B
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Abstract
The invention discloses a DBC (Direct Bonded Copper) substrate surface treatment process based on a nano-silver soldering paste connecting chip. The process solves the technology that not only the copper on the DBC substrate surface is prevented from bleeding out of a silver plating surface, but also the combination strength between the nano-silver soldering paste connecting chip and the DBC substrate is ensured. The DBC substrate surface treatment process comprises the following steps of: firstly carrying out cleaning pretreatment on the surface of a DBC substrate; then carrying out electronickelling treatment on the pretreated DBC substrate; and finally, after thorough cleaning, carrying out silverplating treatment on the surface of the electronickelled DBC substrate by using a magnetron sputtering method. The DBC substrate surface treatment process based on the nano-silver soldering paste connecting chip has the following beneficial effects: when the electronickelled DBC substrate subjected to magnetron sputtering silver is sintered at high temperature by using a nano-silver soldering paste, the metal copper on the surface of the DBC substrate does not oxidize, i.e. the metal copper does not permeate the surface of a silvering layer; after being sintered, the nano-silver soldering paste has good bonding strength with the electronickelled DBC substrate subjected to magnetron sputtering silver; and the DBC substrate surface treatment process is green and environment-friendly and has no adverse effect on the environment.
Description
Technical field
The present invention relates to a kind of process of surface treatment of direct copper substrate, specifically, relate to a kind of pottery-copper bonding substrate (DBC substrate) process of surface treatment that connects chip based on nano mattisolda.
Background technology
In high-power insulated gate bipolar transistor (IGBT) module, DBC substrate provides the functions such as a connection, thermodiffusion, mechanical support for chip.The traditional technology that device connects is by conductive resin or scolder, and the terminal of chip is connected with DBC substrate, and the other end connects with fine aluminum wire.But there is short, the shortcoming such as fusing point is low, poor radiation in work-ing life in conventional conductive glue or scolder, thereby causes the working temperature of high-power chip and DBC substrate tie point can not exceed 150 ℃, and high-power IGBT module is restricted in actual applications.
The nano mattisolda of new type low temperature sintering, major ingredient is argent, many merits conduction, thermal conductivity and the solderabilities etc. as high, good in fusing point of silver, make this novel encapsulated material can realize connection high-power, high-temperature electronic device.
When high-power IGBT module is used nano mattisolda as the connecting material of chip and DBC substrate, need first at DBC substrate plating surface one deck silver, and require silvering enough fine and close, prevent that the copper of DBC is diffused into the surface of silvering, could realize high-intensity connection.The traditional silver plating process that can realize this function adopts prussiate, and still, prussiate is very large to the harm of environment; And adopt non-cyanide silver electroplating when formula, and silvered film is fine and close not, and the metallic copper of DBC substrate surface can ooze out silvered film surface, affect the bonding strength of nano mattisolda connection chip and DBC substrate.Therefore, need to take certain process of surface treatment, both can prevent that DBC substrate surface copper from oozing out silvered film surface, can guarantee again to use nano mattisolda to connect the bonding strength between chip and DBC substrate, and can not exert an adverse impact to environment.
Summary of the invention
What the present invention will solve is the existing the problems referred to above of prior art, a kind of pottery-copper bonding substrate process of surface treatment that connects chip based on nano mattisolda is provided, can guarantee that DBC substrate uses nano mattisolda when high temperature sintering, the metallic copper of DBC substrate surface can not diffuse to silvering surface; Nano mattisolda is after sintering, and the bonding strength of nano mattisolda and DBC substrate is good; In addition, also can not produce detrimentally affect to environment.
In order to solve the problems of the technologies described above, the present invention is achieved by following technical scheme:
Pottery-copper bonding substrate the process of surface treatment that connects chip based on nano mattisolda, the method is carried out according to following steps:
A. pottery-copper bonding substrate surface is cleaned to pre-treatment;
B. to pretreated pottery-copper bonding substrate, adopt electrochemical method to carry out electronickelling processing, described nickel plating solution is comprised of following formula: single nickel salt 250～350g/L, nickelous chloride 40～50g/L, boric acid 35～45g/L keep 15～25mA/cm at 50～60 ℃ of temperature
2cathode current density 5～10min, negative electrode and annode area, than being 1:1, stir nickel plating solution in electroplating process;
C. to the pottery-copper bonding substrate surface after electronickelling, adopt magnetron sputtering method to do silver-plated processing:
(1) to pottery-copper bonding substrate after electronickelling, use flowing water to clean;
(2) with dehydrated alcohol, carry out ultrasonic cleaning pottery-copper bonding substrate;
(3) dry up;
(4) pottery-copper bonding substrate after drying up is put into ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment, and ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment are vacuumized;
(5) use ion gun to carry out Ion Cleaning to the surface that dries up standby pottery-copper bonding substrate, line is 4～6ml, and sparking voltage is 40～60V, heater current is 7～8A, acceleration voltage is 80～120V, and line voltage is 400～600V, scavenging period 3～5min;
(6) pottery-copper bonding substrate surface after Ion Cleaning is carried out to magnetron sputtering silver, argon flow amount is 25～35ml, during build-up of luminance, air pressure is 1～3Pa, during magnetron sputtering silver, pressure maintains 0.2～0.4Pa, d.c. sputtering electric current is (0.1～0.2) A, d.c. sputtering voltage is (0.1～0.3) KV, sputtering time 15～20min.
Wherein, the cleaning pre-treatment of described step a, carry out in accordance with the following steps:
(1) to pottery-copper bonding substrate, use 10% sodium hydroxide solution to clean 20～40s;
(2) flowing water cleans up;
(3) use dilute nitric acid solution to carry out Passivation Treatment to pottery-copper bonding substrate;
(4) pottery-copper bonding substrate surface exposes after copper crystal grain, and flowing water cleans up;
(5) to pottery-copper bonding substrate, use dilute hydrochloric acid solution to clean 20～40s;
(6) flowing water cleans up;
(7) by washed with de-ionized water;
(8) with filter paper, suck the deionized water of pottery-copper bonding substrate surface.
The invention has the beneficial effects as follows:
(1) electronickelling in the present invention is processed and is formed dense nickel dam; nickel dam is as transition layer between silver layer and copper; can effectively stop at high temperature copper to the diffusion of nickel dam; thereby stoped the diffusion of copper to silver layer; effectively protected silvering, therefore nickel dam mainly plays buffer action, and after electronickelling, the DBC substrate of magnetron sputtering silver uses nano mattisolda when high temperature sintering; can there is not oxidizing reaction in the metallic copper of DBC substrate surface, can not ooze out silvering surface.
(2) after electroless nickel layer, adopt the bonding strength of the silver-plated film of electro-plating method low, cannot meet the requirement of high bond strength.The present invention adopts magnetically controlled sputter method silver-plated, can in vacuum chamber, use ion gun effects on surface to clean, then direct plated film, effectively stoped surface contamination, therefore nano mattisolda is after sintering, after nano mattisolda and electronickelling, the bonding strength of the DBC substrate of magnetron sputtering silver is good, and bonding force is higher.
(3) in processing step of the present invention, avoid employing prussiate, therefore can not produce detrimentally affect to environment, environmental protection.
Embodiment
In the present invention, the ultimate principle of processing step is as follows:
(1) for the migration that stops copper atom, at DBC substrate surface, electroplate transition layer nickel, electronickelling is by the galvanic effect in the external world, carries out electrolytic reaction in solution, thereby at substrate surface, deposits the process of last layer nickel metal.Adopt NiSO
4make electrolyte solution, DBC substrate connects power cathode, and pure nickel plate connects power anode, and after energising, metallic nickel enters plating solution with ionic condition, and constantly to cathodic migration, finally on negative electrode, obtaining electron reduction is metallic nickel, forms gradually metallic nickel plated layer.
(2) because nickel and silver can not dissolve each other, after electroless nickel layer, adopt the bonding strength of electro-plating method silvered film low.In vacuum chamber, use ion gun to carry out magnetron sputtering silver after Ion Cleaning to electroless nickel layer surface, not only prevented the pollution on nickel layer surface, also make nickel and silver form covalent linkage, thereby improved bonding strength, form good silvering.
Below by specific embodiment, the present invention is described in further detail:
Embodiment 1
The cleaning pre-treatment of DBC substrate.To DBC substrate, use 10% sodium hydroxide solution to clean 30s, flowing water cleans up; The dilute nitric acid solution of use 25% carries out Passivation Treatment to DBC substrate, and DBC substrate surface exposes after copper crystal grain, and flowing water cleans up; To DBC substrate, use 10% dilute hydrochloric acid solution to clean 30s, flowing water cleans up, by washed with de-ionized water; With filter paper, suck the deionized water of DBC substrate surface.
The electronickelling technique of DBC substrate.Nickel plating solution formula is: single nickel salt 250g/L, nickelous chloride 40g/L, boric acid 35g/L keep 20mA/cm at 50 ℃ of temperature
2cathode current density 7min, negative electrode and annode area are than being 1:1, electronickelling instrument is electrochemical workstation, uses heating magnetic stirring apparatus heat and stir in electronickelling process.
The magnetron sputtering silver process of DBC substrate, institute's use equipment is ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment.To DBC substrate after nickel plating, use flowing water to clean, dehydrated alcohol ultrasonic cleaning, after drying up, puts into ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment; After equipment vacuumizes, use ion gun to nickel plating after the surface of DBC substrate carry out Ion Cleaning, concrete technology parameter: line is 5ml left and right, sparking voltage is 50V, and heater current is about 7.5A, and acceleration voltage is about 100V, line voltage is about 500V, scavenging period 4min; Magnetron sputtering silver is carried out on surface to DBC substrate after nickel plating, concrete technology parameter: argon flow amount is about 30ml, and during build-up of luminance, air pressure is about 2Pa, and during magnetron sputtering silver, pressure maintains 0.3Pa left and right, and d.c. sputtering power is 0.1A × 0.2KV, sputtering time 15min.
Embodiment 2
The cleaning pre-treatment of DBC substrate.To DBC substrate, use 10% sodium hydroxide solution to clean 20s, flowing water cleans up; The dilute nitric acid solution of use 25% carries out Passivation Treatment to DBC substrate, and DBC substrate surface exposes after copper crystal grain, and flowing water cleans up; To DBC substrate, use 10% dilute hydrochloric acid solution to clean 20s, flowing water cleans up, by washed with de-ionized water; With filter paper, suck the deionized water of DBC substrate surface.
The electronickelling technique of DBC substrate.Nickel plating solution formula is: single nickel salt 300g/L, nickelous chloride 45g/L, boric acid 40g/L keep 15mA/cm at 56 ℃ of temperature
2cathode current density 5min, negative electrode and annode area are than being 1:1, electronickelling instrument is electrochemical workstation, uses heating magnetic stirring apparatus heat and stir in electronickelling process.
The magnetron sputtering silver process of DBC substrate, institute's use equipment is ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment.To DBC substrate after nickel plating, use flowing water to clean, dehydrated alcohol ultrasonic cleaning, after drying up, puts into ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment; After equipment vacuumizes, use ion gun to nickel plating after the surface of DBC substrate carry out Ion Cleaning, concrete technology parameter: line is 4ml left and right, sparking voltage is 40V, and heater current is about 7A, and acceleration voltage is about 80V, line voltage is about 400V, scavenging period 3min; Magnetron sputtering silver is carried out on surface to DBC substrate after nickel plating, concrete technology parameter: argon flow amount is about 25ml, and during build-up of luminance, air pressure is about 1Pa, and during magnetron sputtering silver, pressure maintains 0.2Pa left and right, and d.c. sputtering power is 0.2A × 0.1KV, sputtering time 18min.
Embodiment 3
The cleaning pre-treatment of DBC substrate.To DBC substrate, use 10% sodium hydroxide solution to clean 40s, flowing water cleans up; The dilute nitric acid solution of use 25% carries out Passivation Treatment to DBC substrate, and DBC substrate surface exposes after copper crystal grain, and flowing water cleans up; To DBC substrate, use 10% dilute hydrochloric acid solution to clean 40s, flowing water cleans up, by washed with de-ionized water; With filter paper, suck the deionized water of DBC substrate surface.
The electronickelling technique of DBC substrate.Nickel plating solution formula is: single nickel salt 350g/L, nickelous chloride 50g/L, boric acid 45g/L keep 25mA/cm at 60 ℃ of temperature
2cathode current density 10min, negative electrode and annode area are than being 1:1, electronickelling instrument is electrochemical workstation, uses heating magnetic stirring apparatus heat and stir in electronickelling process.
The magnetron sputtering silver process of DBC substrate, institute's use equipment is ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment.To DBC substrate after nickel plating, use flowing water to clean, dehydrated alcohol ultrasonic cleaning, after drying up, puts into ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment; After equipment vacuumizes, use ion gun to nickel plating after the surface of DBC substrate carry out Ion Cleaning, concrete technology parameter: line is 6ml left and right, sparking voltage is 60V, and heater current is about 8A, and acceleration voltage is about 120V, line voltage is about 600V, scavenging period 5min; Magnetron sputtering silver is carried out on surface to DBC substrate after nickel plating, concrete technology parameter: argon flow amount is about 35ml, and during build-up of luminance, air pressure is about 3Pa, and during magnetron sputtering silver, pressure maintains 0.4Pa left and right, and d.c. sputtering power is 0.2A × 0.3KV, sputtering time 20min.
Although above in conjunction with the preferred embodiments of the present invention are described; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing from the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of a lot of forms, within these all belong to protection scope of the present invention.
Claims (2)
1. pottery-copper bonding substrate the process of surface treatment that connects chip based on nano mattisolda, is characterized in that, this technique is carried out according to following steps:
A. pottery-copper bonding substrate surface is cleaned to pre-treatment;
B. to pretreated pottery-copper bonding substrate, adopt electrochemical method to carry out electronickelling processing, described nickel plating solution is comprised of following formula: single nickel salt 250～350g/L, nickelous chloride 40～50g/L, boric acid 35～45g/L keep 15～25mA/cm at 50～60 ℃ of temperature
2cathode current density 5～10min, negative electrode and annode area, than being 1:1, stir nickel plating solution in electroplating process;
C. to the pottery-copper bonding substrate surface after electronickelling, adopt magnetron sputtering method to do silver-plated processing:
(1) to pottery-copper bonding substrate after electronickelling, use flowing water to clean;
(2) with dehydrated alcohol, carry out ultrasonic cleaning pottery-copper bonding substrate;
(3) dry up;
(4) pottery-copper bonding substrate after drying up is put into ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment, and ultrahigh vacuum(HHV) magnetic control and ion beam cleaning filming equipment are vacuumized;
(5) use ion gun to carry out Ion Cleaning to the surface that dries up standby pottery-copper bonding substrate, line is 4～6ml, and sparking voltage is 40～60V, heater current is 7～8A, acceleration voltage is 80～120V, and line voltage is 400～600V, scavenging period 3～5min;
(6) pottery-copper bonding substrate surface after Ion Cleaning is carried out to magnetron sputtering silver, argon flow amount is 25～35ml, during build-up of luminance, air pressure is 1～3Pa, during magnetron sputtering silver, pressure maintains 0.2～0.4Pa, d.c. sputtering electric current is (0.1～0.2) A, d.c. sputtering voltage is (0.1～0.3) KV, sputtering time 15～20min.
2. a kind of pottery-copper bonding substrate process of surface treatment that connects chip based on nano mattisolda according to claim 1, is characterized in that the cleaning pre-treatment of described step a is carried out in accordance with the following steps:
(1) to pottery-copper bonding substrate, use 10% sodium hydroxide solution to clean 20～40s;
(2) flowing water cleans up;
(3) use dilute nitric acid solution to carry out Passivation Treatment to pottery-copper bonding substrate;
(4) pottery-copper bonding substrate surface exposes after copper crystal grain, and flowing water cleans up;
(5) to pottery-copper bonding substrate, use dilute hydrochloric acid solution to clean 20～40s;
(6) flowing water cleans up;
(7) by washed with de-ionized water;
(8) with filter paper, suck the deionized water of pottery-copper bonding substrate surface.
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| WO2014015481A1 (en) * | 2012-07-25 | 2014-01-30 | 建业（惠州）电路版有限公司 | Method for treating circuit board surface |
| CN103331454A (en) * | 2013-07-02 | 2013-10-02 | 南京大学 | Nano-silver manufacturing technology |
| CN104201117B (en) * | 2014-08-26 | 2017-07-07 | 天津大学 | A kind of method that use ultrasonic wave added nano mattisolda sintering makes power model |
| CN104319241B (en) * | 2014-09-15 | 2017-01-18 | 天津大学 | A method for connecting a high-power GTO module by means of pressureless sintering |
| CN104392942A (en) * | 2014-11-05 | 2015-03-04 | 天津大学 | Method for encapsulating high-power IGBT device through performing non-pressure low-temperature sintering on nano silver soldering paste |
| CN109280895A (en) * | 2017-07-20 | 2019-01-29 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of the Mo/Ag laminar composite of high-densit, high interface cohesion |
| CN108520855B (en) * | 2018-05-11 | 2020-09-11 | 北京科技大学 | Method for improving reliability of ceramic copper-clad plate by using nano silver paste |
| CN109411372B (en) * | 2018-09-17 | 2020-10-13 | 天津大学 | Method for uniformly current-assisted sintering of nano-silver solder paste temperature field based on copper-clad ceramic substrate |
| CN113555274B (en) * | 2021-07-21 | 2023-06-02 | 江西圆融光电科技有限公司 | Chip cleaning method |
| CN114150314B (en) * | 2021-11-23 | 2024-02-13 | 中国航发北京航空材料研究院 | High corrosion-resistant composite silver layer and preparation process thereof |
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| US7923289B2 (en) * | 2006-03-31 | 2011-04-12 | International Rectifier Corporation | Process for fabricating a semiconductor package |
| CN100483763C (en) * | 2007-11-02 | 2009-04-29 | 长春市北方电子有限责任公司 | Method for preparing copper film thicken copper-coating ceramic substrate |
| CN101630676B (en) * | 2009-04-02 | 2011-05-11 | 嘉兴斯达微电子有限公司 | Novel isolated gate bipolar transistor module distributed with direct coated copper base plates |
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