阅读说明：本技术 一种纳米颗粒掺杂实现高温服役焊锡膏及其制备方法 (High-temperature service solder(ing) paste and preparation method thereof is realized in a kind of doping of nano particle ) 是由 吴玫 于 2019-09-11 设计创作，主要内容包括：本发明属于一种纳米颗粒掺杂实现高温服役焊锡膏,具体适用于焊接后服役温度高于270℃以上的应用,包括锡合金、纳米金属、稀土合金和助焊膏,所述的锡合金粉末为锡银合金粉末、锡锑合金粉末和锡铜合金粉末的一种或者两种的混合物；纳米金属粉末为铜粉、镍粉、钛粉、钴粉和金粉的一种或者多种混合物；所述的助焊膏的有效成分包括氢化松香、二乙二醇单己醚、丁二酸、甲基苯骈三氮唑和柠檬酸；其制作方法包括制备锡合金粉末、纳米金属粉末、稀土合金粉末、助焊膏和混合几个步骤,采用本技术方案的发明,通过在锡膏中添加一定比例的纳米单质金属颗粒或合金颗粒,并添加相对应的纳米辅助添加剂,制备成本低于纳米焊膏,且易于实现,应用范围更广泛。(It is adulterated the invention belongs to a kind of nano particle and realizes high-temperature service solder(ing) paste, it is particularly applicable to the applications that service temperature after welding is higher than 270 DEG C or more, including tin alloy, nano metal, rare earth alloy and weld-aiding cream, the tin alloy powder is one or two kinds of mixture of sn-ag alloy powder, tin pewter powder and gun-metal powder；Nano metal powder is one or more kinds of mixtures of copper powder, nickel powder, titanium valve, cobalt powder and bronze；The effective component of the weld-aiding cream includes hydrogenated rosin, diethylene glycol monohexyl ether, succinic acid, methylbenzotriazole and citric acid；Its production method includes preparation tin alloy powder, nano metal powder, rare earth alloy powder, weld-aiding cream and the several steps of mixing; using the invention of the technical program; by adding a certain proportion of nano simple substance metallic particles or alloying pellet in tin cream; and add corresponding nanometer auxiliary additive; preparation cost is lower than nano-solder paste; and be easily achieved, application range is more extensive.)

1. high-temperature service solder(ing) paste is realized in a kind of nano particle doping, it is characterised in that: including tin alloy powder, Nano metal powder End, rare earth alloy powder and weld-aiding cream, wherein the tin alloy powder is sn-ag alloy powder, tin pewter powder and tin One or two kinds of mixture of copper alloy powder；Nano metal powder is the one of copper powder, nickel powder, titanium valve, cobalt powder and bronze Kind or a variety of mixtures；The effective component of the weld-aiding cream includes hydrogenated rosin, diethylene glycol monohexyl ether, succinic acid, first Base benzotriazole and citric acid.

2. high-temperature service solder(ing) paste is realized in nano particle doping according to claim 1, it is characterised in that: the tin closes Bronze end further includes having leypewter powder.

3. high-temperature service solder(ing) paste is realized in nano particle doping according to claim 2, it is characterised in that: the tin closes In bronze end, by mass percentage, tin 1%~98%: lead 0%~95%, silver 0.5%~5%: copper 0.01%~1%: antimony 5%~30%.

4. high-temperature service solder(ing) paste is realized in nano particle doping according to claim 1, it is characterised in that: the nanometer In metal powder, by mass percentage, copper 2%~60%: nickel 0.5%~15%: titanium 0.1%~5%: cobalt 0.1%~5%: Gold 0.1%~10%.

5. high-temperature service solder(ing) paste is realized in nano particle doping according to claim 1, it is characterised in that: the rare earth In alloy powder, according to mass percent, rare earth alloy powder 0.01%~2%: Nano metal powder 98%~99.9%.

6. high-temperature service solder(ing) paste is realized in nano particle doping according to claim 1, it is characterised in that: described helps weldering In cream, by mass percentage, hydrogenated rosin 3%~8%: diethylene glycol monohexyl ether 1%~6%: succinic acid 0.1%~0.8%, Methylbenzotriazole 0.03%~0.1% and citric acid 0.01%~0.2%.

7. the preparation method that high-temperature service solder(ing) paste is realized in nano particle doping according to claim 1, it is characterised in that: Include the following steps,

Step 1, prepares tin alloy powder, and preparation tin alloy powder includes preparing sn-ag alloy powder, gun-metal powder and tin Antimony alloy powder, specific step is as follows,

A. the raw material for refining tin silver master alloy is added to intermediate frequency furnace by feed inlet according to the tin silver ratio of mass percent 3:7 In, the temperature of intermediate frequency furnace is set as 1100-1200 DEG C, and it arrives after temperature tilting furnace, obtained master alloy is poured into rustless steel container, Cooling is spare；

B. the raw material for refining tin copper master alloy is added to intermediate frequency by feed inlet according to the tin copper ratio of mass percent 1:10 In furnace, the temperature of intermediate frequency furnace is set as 1100-1200 DEG C, obtained master alloy is poured into rustless steel container, cooling is spare；

C. the raw material for refining tin antimony master alloy is added to vacuum by feed inlet according to the tin antimony ratio of mass percent 1:10 In furnace, the temperature of vacuum drying oven is set as 650-800 DEG C, obtained master alloy is poured into rustless steel container, cooling is spare；

D. by the one of which of the master alloy obtained from step a, b, c or two kinds pour into rustless steel container with mass percent 10% glass putty is sufficiently mixed at 200-300 DEG C of temperature, and stirring after sixty minutes, stands 180 minutes, it is spare that alloy is made；

E. when temperature is reduced to 150-180 DEG C, it is 0.6%~12% that mass percent is added in alloy obtained above Potassium metal powder stirs 60 minutes, and temperature is risen to 200-300 DEG C, is stood after twenty minutes, is scooped out cooling, it is spare to be made into alloy；

F. it is spare to be prepared into tin alloy powder by sizing screening by powder atomization molding equipment for above-mentioned alloy；

Step 2 prepares nano metal powder,

G. by copper, nickel, titanium, cobalt, gold it is one of carry out melting or it is a variety of be smelted into alloy, set by nanometer powder molding It is standby, it is screened by centrifugal classification, it is spare to be prepared into nano metal powder；

Step 3 prepares rare earth alloy powder,

H. it is spare to be prepared into rare earth alloy powder by sizing screening by powder compacting equipment for rare earth alloy；

Step 4 prepares weld-aiding cream,

I. the preparation of weld-aiding cream: 3%~8% hydrogenated rosin is added in reaction kettle after 120 DEG C~140 DEG C stirring fusings, is added 0.1%~0.8% fourth two is added in the diethylene glycol monohexyl ether uniform stirring for entering 1%~6% after being cooled to 80 DEG C~110 DEG C Acid and 0.03%~0.1% methylbenzotriazole uniform stirring, after being cooled to 40~50 DEG C be added 0.01%~0.2% Citric acid uniform stirring and after being cooled to room temperature, it is spare to be prepared into weld-aiding cream；

Step 5 is stirred into solder(ing) paste,

J. the weld-aiding cream of above-mentioned preparation and tin alloy powder, nano metal (or alloy) powder, rare earth alloy powder are successively added Enter in full-automatic planetary mixer, dispense after mixing evenly under vacuum conditions, is saved under the conditions of 2~10 DEG C.

8. the preparation method that high-temperature service solder(ing) paste is realized in nano particle doping according to claim 7, it is characterised in that: In the step one, prepares in tin alloy powder, further include preparing leypewter powder, the specific steps are according to quality The raw material for refining tin-lead master alloy is added in intermediate frequency furnace by the tin-lead ratio of percentage 63:37 by feed inlet, intermediate frequency furnace Temperature is set as 1300-1400 DEG C, arrives after temperature tilting furnace, obtained master alloy is poured into rustless steel container, cooling is spare.

9. the preparation method that high-temperature service solder(ing) paste is realized in nano particle doping according to claim 7, it is characterised in that: The tin alloy powder size has seven kinds of specifications, wherein 1#:75~150um, 2#:45~75um, 3#:25~45um, 4#: 20~38um, 5#:10~20um, 6#:5~15um, 7#:2~12um.

10. nano particle doping according to claim 7 realizes that the preparation method of high-temperature service solder(ing) paste, feature exist In: by mass percentage, the content of the nano metal powder is 3%~60%, 2~100nm of particle size range.

Technical field

It is adulterated the invention belongs to a kind of nano particle and realizes high-temperature service solder(ing) paste and preparation method thereof, it is particularly applicable to weld Connect the application that rear service temperature is higher than 270 DEG C or more.

Background technique

With the densification of the high speed, integrated circuit of communication equipment, the complexity of semiconductor devices is higher and higher, To encapsulation technology, more stringent requirements are proposed, with the expansion of multi-level packaging, can be to printed circuit board (PCB) multiple welding Raising speed of production after in first time A, face is welded, when welding followed by the face B, when secondary (multiple) welding, is printed electric The temperature of road plate (PCB) is higher, usually at 240 DEG C or more, when the solder(ing) paste using military service fusing point low (being usually all at 216 DEG C) When, since in secondary (or multiple) welding, the temperature of printed circuit board (PCB) is higher than the solder(ing) paste of low melting point, will cause The face the A low-melting solder(ing) paste of military service through welding can melt again, cause the face A being welded welding not firm, seriously affect The quality of welding, reduces properties of product；When using military service fusing point high solder(ing) paste, the fusing point of solder(ing) paste itself requires height, Although solve secondary (or repeatedly) welding, the face the A solder(ing) paste being welded is not easy the technical issues of being melted, the When the face an A weldering, high fusing point is needed, cost is also higher.In currently available technology, solder(ing) paste cannot fully meet requirement, The excessively high either performance of cost is not achieved or use scope is narrow.

Summary of the invention

It is adulterated the technical problem to be solved in the present invention is to provide a kind of nano particle and realizes high-temperature service solder(ing) paste, solve mesh The high technical problem of fusing point in the case that preceding solder(ing) paste is low in welding fusing point and adaptation service temperature is high.

In order to solve the above-mentioned technical problem, of the invention, a kind of nano particle doping realization high-temperature service solder(ing) paste, Yi Zhongna High-temperature service solder(ing) paste is realized in rice grain doping, including tin alloy powder, nano metal powder, rare earth alloy powder and helps weldering Cream, wherein the tin alloy powder is sn-ag alloy powder, one kind of tin pewter powder and gun-metal powder or two The mixture of kind；Nano metal powder is one or more kinds of mixtures of copper powder, nickel powder, titanium valve, cobalt powder and bronze；Described The effective component of weld-aiding cream includes hydrogenated rosin, diethylene glycol monohexyl ether, succinic acid, methylbenzotriazole and citric acid.

Further, limiting the tin alloy powder further includes having leypewter powder.

Further, it limits in the tin alloy powder, by mass percentage, tin 1%~98%: lead 0%~95%, Silver 0.5%~5%: copper 0.01%~1%: antimony 5%~30%.

Further, it limits in the nano metal powder, by mass percentage, copper 2%~60%: nickel 0.5%~ 15%: titanium 0.1%~5%: cobalt 0.1%~5%: gold 0.1%~10%.

Further, it limits in the rare earth alloy powder, according to mass percent, rare earth alloy powder 0.01%~ 2%: Nano metal powder 98%~99.9%.

Further, limit in the weld-aiding cream, by mass percentage, hydrogenated rosin 3%~8%: diethylene glycol list oneself Ether 1%~6%: succinic acid 0.1%~0.8%, methylbenzotriazole 0.03%~0.1% and citric acid 0.01%~ 0.2%.

The invention solves another technical problem be to provide a kind of doping of nano particle and realize high-temperature service scolding tin The preparation method of cream solves the solder(ing) paste system that fusing point is high in the case that above-mentioned this welding fusing point is low, and adaptation service temperature is high Preparation Method.

In order to solve the above-mentioned technical problem, of the invention, the preparation of high-temperature service solder(ing) paste is realized in a kind of nano particle doping Method includes the following steps,

Step 1, prepares tin alloy powder, and preparation tin alloy powder includes preparing sn-ag alloy powder, gun-metal powder With tin pewter powder, specific step is as follows,

A. in the raw material for refining tin silver master alloy being added to by feed inlet according to the tin silver ratio of mass percent 3:7 In frequency furnace, the temperature of intermediate frequency furnace is set as 1100-1200 DEG C, arrives after temperature tilting furnace, obtained master alloy is poured into stainless steel Container, cooling are spare；

B. the raw material for refining tin copper master alloy is added to by feed inlet according to the tin copper ratio of mass percent 1:10 In intermediate frequency furnace, the temperature of intermediate frequency furnace is set as 1100-1200 DEG C, obtained master alloy is poured into rustless steel container, cooling is spare；

C. the raw material for refining tin antimony master alloy is added to by feed inlet according to the tin antimony ratio of mass percent 1:10 In vacuum drying oven, the temperature of vacuum drying oven is set as 650-800 DEG C, obtained master alloy is poured into rustless steel container, cooling is spare；

D. by the one of which of the master alloy obtained from step a, b, c or two kinds pour into rustless steel container with quality percentage Glass putty than 10% is sufficiently mixed at 200-300 DEG C of temperature, and stirring after sixty minutes, stands 180 minutes, it is spare that alloy is made；

E. when temperature is reduced to 150-180 DEG C, in alloy obtained above be added mass percent be 0.6%~ 12% potassium metal powder stirs 60 minutes, and temperature is risen to 200-300 DEG C, is stood after twenty minutes, is scooped out cooling, be made into conjunction Gold is spare；

F. it is spare to be prepared into tin alloy powder by sizing screening by powder atomization molding equipment for above-mentioned alloy；

Step 2 prepares nano metal powder,

G. by copper, nickel, titanium, cobalt, gold it is one of carry out melting or it is a variety of be smelted into alloy, formed by nanometer powder Equipment is screened by centrifugal classification, and it is spare to be prepared into nano metal powder；

Step 3 prepares rare earth alloy powder,

H. it is spare to be prepared into rare earth alloy powder by sizing screening by powder compacting equipment for rare earth alloy；

Step 4 prepares weld-aiding cream,

I. 120 DEG C~140 DEG C stirring fusings in reaction kettle the preparation of weld-aiding cream: are added in 3%~8% hydrogenated rosin Afterwards, 1%~6% diethylene glycol monohexyl ether uniform stirring is added, 0.1%~0.8% is added after being cooled to 80 DEG C~110 DEG C Succinic acid and 0.03%~0.1% methylbenzotriazole uniform stirring, after being cooled to 40~50 DEG C be added 0.01%~ 0.2% citric acid uniform stirring and after being cooled to room temperature, it is spare to be prepared into weld-aiding cream；

Step 5 is stirred into solder(ing) paste,

J. the weld-aiding cream of above-mentioned preparation and tin alloy powder, nano metal (or alloy) powder, rare earth alloy powder is first After be added in full-automatic planetary mixer, dispense, saved under the conditions of 2~10 DEG C after mixing evenly under vacuum conditions.

Further, the step of preparation method of high-temperature service solder(ing) paste is realized in the nano particle doping one, system are limited It further include preparing leypewter powder, the specific steps are according to the tin-lead of mass percent 63:37 in standby tin alloy powder The raw material for refining tin-lead master alloy is added in intermediate frequency furnace by ratio by feed inlet, and the temperature of intermediate frequency furnace is set as 1300- It 1400 DEG C, arrives after temperature tilting furnace, obtained master alloy is poured into rustless steel container, cooling is spare.

Further, the tin alloy powder that the preparation method of high-temperature service solder(ing) paste is realized in the nano particle doping is limited Size has seven kinds of specifications, wherein and 1#:75~150um, 2#:45~75um, 3#:25~45um, 4#:20~38um, 5#:10~ 20um, 6#:5~15um, 7#:2~12um.

Further, it limits the nano particle doping to realize in the preparation method of high-temperature service solder(ing) paste: by quality Percentage, the content of the nano metal powder are 3%~60%, 2~100nm of particle size range.

Using the invention of the technical program, a kind of nano particle doping realization high-temperature service solder(ing) paste, by tin cream A certain proportion of nano simple substance metallic particles or alloying pellet are added, and adds corresponding nanometer auxiliary additive, is prepared into This is lower than nano-solder paste, and is easily achieved, and application range is more extensive；Using the invention using the technical program, a kind of nanometer The preparation method of high-temperature service solder(ing) paste is realized in grain doping, by adding a certain proportion of nano simple substance metallic particles in tin cream Or alloying pellet, and corresponding nanometer auxiliary additive is added, reach service temperature answering higher than 300 DEG C or more after welding With preparation cost is lower than nano-solder paste, and service temperature is higher than conventional high temperature tin cream, and is easily achieved, and application range is more extensive.

Specific embodiment