CN114289710A - Method for plating nickel on surface of nano zirconia reinforced phase in brazing filler metal - Google Patents
Method for plating nickel on surface of nano zirconia reinforced phase in brazing filler metal Download PDFInfo
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Abstract
According to the method for plating the surface of the nano zirconia reinforcement phase in the brazing filler metal with nickel, firstly, chemical nickel plating treatment is carried out on the surface of nano zirconia based on a series of processes of acidizing treatment, dispersing agent treatment, ultrasonic treatment, drying treatment, segmented decomposition reaction, cooling and the like on pretreated zirconia powder, and then the prepared nickel-plated zirconia powder is applied to a brazing lap joint process. The nickel-plated zirconia powder prepared by the method has the advantages of similar density to that of the brazing filler metal, high particle stability, no reaction when being applied to the brazing process, excellent mechanical property and low cost of high-grade nano particles. According to the brazing overlapping process, the shear strength is improved after welding, the wettability is also improved, the melting point is not changed greatly and is slightly increased, and the integral service performance is not influenced.
Description
Technical Field
The application relates to the technical field of lead-free solders, in particular to a method for plating nickel on the surface of a nano zirconia reinforced phase in a solder.
Background
The traditional Sn-Pb alloy has been widely used in the field of welding due to the characteristics of low melting point, good wettability and the like, and in recent years, the toxicity of lead can cause harm to tissues, nerves and blood of a human body, thereby limiting the application of the Sn-Pb alloy. In view of this, more and more researchers are beginning to focus on the study of lead-free solders. Among these lead-free solders, the most predominant ones are tin-based solders, and typical binary lead-free solders include Sn-Ag series, Sn-Cu series, Sn-Zn series, Sn-Bi series, Sn-In series, and the like. At most, Sn-Ag-Cu alloy is used as a typical ternary lead-free solder, and the SnAgCu solder is recommended to be the best substitute of the Sn-Pb solder due to good wettability, high mechanical property and excellent fatigue resistance. Among the SnAgCu-based lead-free solders, much attention has been paid to Sn-3.0Ag-0.5Cu, Sn-3.8Ag-0.7Cu and Sn-3.9Ag-0.6Cu solders.
However, the above 3 solders have a general problem of high content of Ag element, which inevitably increases the cost of the solder. In order to better meet the market demand, the development of a low-silver lead-free solder which not only meets the performance requirement but also reduces the cost becomes a hot spot of the current domestic and foreign research. However, as the content of Ag is reduced, problems such as an increase in melting temperature and a significant decrease in wettability are also caused to the SnAgCu solder.
In order to improve the comprehensive performance of the lead-free solder, performance improvement can be realized by adding some reinforcing phases. In the related art, the commonly used types of reinforcing phases are metal nanoparticle reinforcement, composite nanoparticle reinforcement, and advanced nanoparticle reinforcement. The added metal nano particles mainly contain Mn, Zn and Al, but in the service process of electronic packaging, interfaces formed by the metal particles react to generate brittle substances, so that the reliability of welding spots is influenced. Meanwhile, when the metal nanoparticles are added, the wettability of the solder is lowered to some extent. The high-grade nano enhancement mainly refers to the addition of some expensive nano substances such as graphene, carbon nanotubes and the like, and although the substances have the advantages of high strength, good conductivity and the like, the mass production is limited due to the cost factor.
Disclosure of Invention
The application provides a method for plating nickel on the surface of a nano zirconia reinforcing phase in a brazing filler metal, and solves the problems that the interface formed by conventional commonly used reinforcing phase metal particles can react to generate a brittle substance, the reliability of a welding spot is influenced and the like.
The technical scheme adopted by the application for solving the technical problems is as follows:
the application provides a method for plating nickel on the surface of a nano zirconia reinforcing phase in a brazing filler metal, which comprises the following steps:
acidizing the pretreated zirconia powder;
mixing the zirconium oxide powder subjected to acidification treatment and nickel nitrate powder according to the mass ratio of 1:0.4 to obtain first mixed powder;
adding a certain amount of water into the first mixed powder to obtain a first mixed solution, wherein the amount of the added water is determined according to the amount of water required by adding water into the acidified zirconia powder and stirring the acidified zirconia powder into paste;
adding a dispersing agent into the first mixed solution, and stirring to obtain a second mixed solution;
carrying out ultrasonic treatment and drying treatment on the second mixed solution to obtain second mixed powder;
placing the second mixed powder in a tube furnace to perform a segmented decomposition reaction under the atmosphere of first protective gas;
and after the segmented decomposition reaction is finished, furnace cooling is carried out, and the nickel-plated zirconium oxide powder is obtained after cooling is finished.
Optionally, the step of performing an acidification treatment on the pretreated zirconia powder includes:
putting zirconia powder into a planetary ball mill for ball milling treatment for 3 hours;
putting zirconium oxide powder subjected to ball milling treatment into a mixed acid solution, and performing ultrasonic treatment for 1 hour, wherein the mixed acid solution is hydrochloric acid and sulfuric acid with the volume ratio of 1: 1;
and after the ultrasonic treatment is finished, putting the mixed acid solution of the zirconium oxide powder into a reaction container, and adding distilled water for repeatedly washing until the solution is neutral.
Optionally, when the dispersant is added for stirring, the stirring process comprises the steps of manually stirring, and then placing on a magnetic stirrer for heating and stirring for 30 minutes.
Optionally, the subjecting the second mixed solution to an ultrasonic treatment and a drying treatment includes:
the second mixed solution was subjected to ultrasonic treatment for 1 hour, and then placed in a vacuum drying oven to be dried for 3 hours.
Optionally, the first protective gas includes hydrogen and argon, and the volume ratio of hydrogen to argon is 1: 9.
Optionally, the conditions of the step decomposition reaction include:
the set temperature decomposition process comprises the following steps: the first stage is at 220 deg.C for 1 hr, and the second stage is at 220-400 deg.C for 1 hr.
Optionally, the dispersant is urea, and the mass ratio of the urea to the zirconia powder is 1: 10.
A second aspect of the present application provides a braze lap process using the nickel-plated zirconia powder prepared according to any one of claims 1 to 7, the process comprising:
adding the nickel-plated zirconium oxide powder into the matrix SnAgCu powder according to the mass ratio of 0.1%, 0.3%, 0.5%, 0.7% and 1%, adding the flux paste, fully and uniformly stirring, and then carrying out a brazing lap joint experiment on a Cu plate in a brazing furnace at the temperature of 270 ℃.
Optionally, the flux paste is OM340 in an alpha model, and the mass ratio of the flux to the matrix SnAgCu powder is 1: 10.
The technical scheme provided by the application comprises the following beneficial technical effects:
according to the technical scheme, the method for plating the surface of the nano zirconia reinforcement phase in the brazing filler metal comprises the steps of carrying out chemical nickel plating treatment on the surface of the nano zirconia based on a series of processes of acidizing treatment, dispersing agent treatment, ultrasonic treatment, drying treatment, segmented decomposition reaction, cooling and the like on pretreated zirconia powder, and then applying the prepared nickel-plated zirconia powder to a brazing lap joint process. The nickel-plated zirconia powder prepared by the method has the advantages of similar density to that of the brazing filler metal, high particle stability, no reaction when being applied to the brazing process, excellent mechanical property and low cost of high-grade nano particles.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of a welded lap joint provided in an embodiment of the present application;
FIG. 2 is a TEM topography of a raw zirconia powder provided in an example of the present application;
FIG. 3 is a TEM morphology of the nickel-plated zirconia powder after nickel plating provided in the examples of the present application;
FIG. 4 is a TEM topography of the partially nickel-plated zirconia powder of FIG. 3 provided by an example of the present application;
FIG. 5 is a TEM morphology of the nickel-plated zirconia powder in the white box of FIG. 4 provided by an example of the present application;
FIG. 6 is an XRD pattern of a nickel-plated zirconia powder after nickel plating provided in examples of the present application;
FIG. 7 shows the shear strength with Ni-ZrO provided in the examples of the present application2Content variation tendencyA drawing;
FIG. 8 shows the contact angle as a function of Ni-ZrO during wetting, as provided in examples of the present application2A content variation trend graph;
FIG. 9 shows the melting point dependence of Ni-ZrO provided in the examples of the present application2And (4) a content change trend graph.
Detailed Description
In order to make the technical solutions in the present application better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application; it is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
When the matrix is SnAgCu powder (sn98.5ag1cu0.5) (hereinafter abbreviated as SAC 105), the cost can be reduced because the silver content is low, but the degradation of other properties such as mechanical properties and wettability is also accompanied; in contrast, in the present embodiment, the mechanical properties of SAC105 are improved by performing surface modification treatment and adding nano zirconia, but since nano zirconia is ceramic particles, it is unfavorable for wettability and conductivity, and therefore, it is necessary to perform chemical nickel plating treatment on the surface of nano zirconia. When the nickel-plated zirconia powder prepared by the method for plating the surface of the nano zirconia reinforcing phase in the brazing filler metal provided by the embodiment of the application is applied to a brazing and lapping process, the shear strength is improved after welding, the wettability is also improved, the melting point change is not large and is slightly increased, but the integral service performance is not influenced.
Based on the above, in a first aspect, embodiments of the present application provide a method for plating nickel on a surface of a nano zirconia reinforcing phase in a solder, including the following steps:
and S1, acidifying the pretreated zirconia powder.
In the embodiment of the present application, firstly, the zirconium oxide powder needs to be acidified, which specifically includes:
firstly, putting zirconia powder into a planetary ball mill for ball milling treatment for 3 hours;
putting zirconium oxide powder subjected to ball milling treatment into a mixed acid solution, and performing ultrasonic treatment for 1 hour, wherein the mixed acid solution is hydrochloric acid and sulfuric acid with the volume ratio of 1: 1;
and after the ultrasonic treatment is finished, putting the mixed acid solution of the zirconium oxide powder into a reaction container, and adding distilled water for repeatedly washing until the solution is neutral.
S2, mixing the zirconium oxide powder after acidification treatment and the nickel nitrate powder according to the mass ratio of 1:0.4 to obtain first mixed powder.
In the embodiment of the application, the mixing of the zirconia powder and the nickel nitrate powder according to the mass ratio of 1:0.4 is the optimal proportion parameter obtained through multiple tests in the process method, and under the proportion, the finally prepared nickel-plated zirconia powder has the best performance parameters and can meet the actual use requirement.
And S3, adding a certain amount of water into the first mixed powder to obtain a first mixed solution, wherein the amount of the added water is determined according to the amount of water needed by adding water into the acidified zirconia powder and stirring the acidified zirconia powder into paste.
The amount of water required for adding water to make a paste is determined based on the determined amount of zirconia powder, and it is found from experimental data that about 7mL of water is required for 10g of zirconia powder.
And S4, adding a dispersing agent into the first mixed solution, and stirring to obtain a second mixed solution.
When the dispersing agent is stirred, the stirring is performed manually, and then the dispersing agent is placed on a magnetic stirrer to be heated and stirred for 30 minutes.
In some embodiments, the dispersant is urea in a mass ratio to zirconia powder of 1: 10.
And S5, carrying out ultrasonic treatment and drying treatment on the second mixed solution to obtain second mixed powder.
The ultrasonic and drying treatment of the second mixed solution comprises the following steps:
the second mixed solution was subjected to ultrasonic treatment for 1 hour, and then placed in a vacuum drying oven to be dried for 3 hours.
And S6, placing the second mixed powder in a tube furnace to perform a segmented decomposition reaction under the atmosphere of the first protective gas.
The first protective gas comprises hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1: 9.
The set temperature decomposition process comprises the following steps: the first stage is at 220 deg.C for 1 hr, and the second stage is at 220-400 deg.C for 1 hr.
And S7, after the segmented decomposition reaction is finished, furnace cooling is carried out, and the nickel-plated zirconium oxide powder is obtained after the cooling is finished.
The method for plating nickel on the surface of the nano zirconia reinforcing phase in the solder provided in the present application is further explained by a specific example.
Firstly, ball-milling zirconium oxide powder in a planetary ball mill for 3 hours, and then putting the zirconium oxide powder into a mixed acid solution of hydrochloric acid and sulfuric acid with the volume ratio of 1:1 for ultrasonic treatment for 1 hour. Adding distilled water, standing until the zirconia powder is completely precipitated into the bottom of the cup, and pouring out the supernatant. Adding distilled water, standing, and repeating the above steps until the solution is neutral.
The zirconia powder was subjected to a water absorption test, a certain amount of water was added to the zirconia powder and stirred into a paste, and the approximate volume of water required was recorded.
Weighing and mixing the zirconium oxide powder and the nickel nitrate powder after the acidification treatment according to the mass ratio of 1:0.4, adding water in the required proportion, then adding dispersant urea with the mass ratio of 1:10 to the zirconium oxide powder, manually stirring, then placing on a magnetic stirrer for heating and stirring for 30 minutes, then carrying out ultrasonic treatment on the mixture for 1 hour, and then drying in a vacuum drying oven for 3 hours.
Putting the dried powder in the previous step into a tubular furnace to carry out segmented decomposition reaction under the protection of mixed atmosphere of hydrogen and argon in a ratio of 1:9, wherein the set temperature decomposition process comprises the following steps: the first stage is to preserve heat for 1 hour at 220 ℃, the second stage is to preserve heat for 1 hour at 220-400 ℃, and then the nickel-plated zirconia powder is obtained after furnace cooling and cooling are finished.
In a second aspect, the present application provides a braze welding and overlapping process, where the process uses the nickel-plated zirconia powder prepared as described above, as shown in fig. 1, and is a schematic view of a weld overlapping joint provided in an embodiment of the present application, and the process includes:
nickel-plated zirconium oxide powder (hereinafter referred to as Ni-ZrO)2) Respectively adding the solder paste into the SnAgCu powder of the matrix according to the mass ratio of 0.1%, 0.3%, 0.5%, 0.7% and 1%, then adding the solder paste, fully and uniformly stirring, and further carrying out a brazing lap joint experiment on a Cu plate in a brazing furnace at the temperature of 270 ℃.
Optionally, in some embodiments, the flux paste is OM340 in an alpha model, and a mass ratio of the flux to the matrix SnAgCu powder is 1: 10.
Scanning electron microscope analysis is performed on the raw zirconia powder and the nickel-plated zirconia powder prepared by the method provided by the embodiment of the application in the embodiment of the application, as shown in fig. 2, a TEM topography of the raw zirconia powder provided by the embodiment of the application is shown, fig. 3 is a TEM topography of the nickel-plated zirconia powder provided by the embodiment of the application, and comparing fig. 2 and 3, and fig. 4 and 5, it can be clearly seen that small particles deposited on the zirconia in the figures are visible, which indicates that nickel is successfully plated on the zirconia powder.
Meanwhile, in the embodiment of the present application, XRD analysis is performed on the nickel-plated zirconium oxide powder after nickel plating prepared by the method provided in the embodiment of the present application, as shown in fig. 6, XRD test is performed on the white square area in fig. 4, and the measured interplanar spacing d is 0.213nm and is very close to that of (111) inside Ni, so that the conclusion that the surface of the zirconium oxide powder is successfully plated with nickel can be obtained.
On the other hand, in the examples of the present application, the matrix (SAC 105) and Ni-ZrO of different compositions were also used2Weld joint shear strength, wetting angle of composite solders with different particulate Ni-ZrO2 content, and addition of Ni-ZrO2After the powder, the melting point of the matrix (SAC 105) was examined, as shown in fig. 2-4:
FIG. 2 shows a substrate (SAC 1) at a brazing temperature of 270 ℃ for a period of 3min05) And Ni-ZrO of different compositions2And (3) a change trend graph of the shear strength of the welding joint. As seen from FIG. 2, with Ni-ZrO2The increase of the mass percentage of 0.3%, 0.5%, 0.7% and 1% shows the trend of increasing first and then decreasing, and the increase of the mass percentage of 0.7% is 35% when the content is 0.7%, the reason is the dispersion strengthening effect, and the decrease of the mass percentage of 1% later is probably the agglomeration.
Wettability is considered to be one of the important characteristics of solder alloys in electronic packages, and if solder is in poor contact with a substrate, failure occurs quickly, and thus wettability of solder is critical to solder joint reliability. Therefore, composite solders of different particulate Ni — ZrO2 contents were investigated in this example. In general, wettability is expressed in terms of wetting angle. FIG. 3 shows the contact angle as a function of Ni-ZrO during wetting, as provided in the examples of the present application2A content variation trend graph; the Young's system shows that: the smaller the contact angle, the better the wettability, as can be seen from FIG. 3, the whole is added with Ni-ZrO2After the powder, the contact angle was lower than that of the substrate (SAC 105), with the contact angle being the smallest for the 0.7% component and the best wettability.
FIG. 4 shows the melting point dependence of Ni-ZrO provided in the examples of the present application2The content variation trend graph shows that: adding Ni-ZrO2After the powder, the melting point was slightly changed and slightly increased. Therefore, the brazing lap joint does not need to be additionally applied to melting at a higher temperature, the actual use requirement can be met, and the waste of heat resources is avoided.
According to the technical scheme, the method for plating the surface of the nano zirconia reinforcement phase in the brazing filler metal by nickel and the brazing lapping process are characterized in that firstly, the chemical nickel plating treatment is carried out on the surface of the nano zirconia based on a series of processes of acidizing treatment, dispersing agent treatment, ultrasonic treatment, drying treatment, segmented decomposition reaction, cooling and the like on the pretreated zirconia powder, and then the prepared nickel-plated zirconia powder is applied to the brazing lapping process. The nickel-plated zirconia powder prepared by the method has the advantages of similar density to that of the brazing filler metal, high particle stability, no reaction when being applied to the brazing process, excellent mechanical property and low cost of high-grade nano particles.
It is noted that relational terms such as "first" and "second," and the like, may be 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. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an 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. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
It will be understood that the present application is not limited to what has been described above and shown in the accompanying drawings, and that various modifications and changes can be made without departing from the scope thereof. The scope of the application is limited only by the appended claims.
Claims (7)
1. A method for plating nickel on the surface of a nano zirconia reinforcing phase in a brazing filler metal is characterized by comprising the following steps:
acidizing the pretreated zirconia powder;
mixing the zirconium oxide powder subjected to acidification treatment and nickel nitrate powder according to the mass ratio of 1:0.4 to obtain first mixed powder;
adding a certain amount of water into the first mixed powder to obtain a first mixed solution, wherein the amount of the added water is determined according to the amount of water required by adding water into the acidified zirconia powder and stirring the acidified zirconia powder into paste;
adding a dispersing agent into the first mixed solution, and stirring to obtain a second mixed solution;
carrying out ultrasonic treatment and drying treatment on the second mixed solution to obtain second mixed powder;
placing the second mixed powder in a tube furnace to perform a segmented decomposition reaction under the atmosphere of first protective gas;
and after the segmented decomposition reaction is finished, furnace cooling is carried out, and the nickel-plated zirconium oxide powder is obtained after cooling is finished.
2. The method for plating nickel on the surface of the nano zirconia reinforcing phase in the brazing filler metal according to claim 1, wherein the step of acidifying the pretreated zirconia powder comprises the following steps:
putting zirconia powder into a planetary ball mill for ball milling treatment for 3 hours;
putting zirconium oxide powder subjected to ball milling treatment into a mixed acid solution, and performing ultrasonic treatment for 1 hour, wherein the mixed acid solution is hydrochloric acid and sulfuric acid with the volume ratio of 1: 1;
and after the ultrasonic treatment is finished, putting the mixed acid solution of the zirconium oxide powder into a reaction container, and adding distilled water for repeatedly washing until the solution is neutral.
3. The method for plating nickel on the surface of the nano zirconia reinforcing phase in the brazing filler metal according to claim 1, wherein the stirring by adding the dispersing agent comprises the steps of manually stirring and then placing on a magnetic stirrer to be heated and stirred for 30 minutes.
4. The method for plating nickel on the surface of nano zirconia reinforcing phase in solder according to claim 1, wherein the second mixed solution is subjected to ultrasonic and drying treatment, and the method comprises the following steps:
the second mixed solution was subjected to ultrasonic treatment for 1 hour, and then placed in a vacuum drying oven to be dried for 3 hours.
5. The method for plating nickel on the surface of the nano-zirconia reinforcing phase in the brazing filler metal according to claim 1, wherein the first protective gas comprises hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1: 9.
6. The method for plating nickel on the surface of nano zirconia reinforcing phase in the brazing filler metal according to claim 1, wherein the conditions of the step decomposition reaction comprise:
the set temperature decomposition process comprises the following steps: the first stage is at 220 deg.C for 1 hr, and the second stage is at 220-400 deg.C for 1 hr.
7. The method for plating nickel on the surface of the nano zirconia reinforcing phase in the brazing filler metal according to claim 1, wherein the dispersant is urea and the mass ratio of the urea to the zirconia powder is 1: 10.
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| US4602731A (en) * | 1984-12-24 | 1986-07-29 | Borg-Warner Corporation | Direct liquid phase bonding of ceramics to metals |
| CN1326910A (en) * | 2001-04-19 | 2001-12-19 | 宁波凌日表面工程有限公司 | Method for preparing nanometer metal ceramic composite powder |
| US20090087567A1 (en) * | 2007-10-02 | 2009-04-02 | National Taiwan University Of Science And Technology | Method of fabricating one-dimensional metallic nanostructure |
| CN101774019A (en) * | 2010-02-02 | 2010-07-14 | 中国地质大学（武汉） | Metal/nanometer zirconia composite spherical powder material used for gradient coating and preparation method thereof |
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