Lockheed Martin Corporation (Bethesda, MD)

The processes for synthesizing metallic nanoparticles, including copper nanoparticles are discussed. The process involves the reaction of an insoluble complex of a metallic salt using a reducing agent in a reaction mixture containing an initial surfactant made of amine and a secondary amine second surfactant, and a diamine chelating agent as a third surfactant. More specifically, processes for forming copper nanoparticles may involve the formation of an initial solution that contains the copper salt, a primary initial surfactant made of amine and a secondary amine second surfactant and diamine chelating agent as the third surfactant, allowing an insoluble complex of the copper salt to form from the initial solution, combining a second solution containing a reducing agent with the insoluble complex, and forming copper nanoparticles from the insoluble complex. The copper nanoparticles typically measure 10 nanometers in size, with a maximum size of 3 nm to 6 nm. They also have a melting point of approximately 200.degree. C. or lower.

While lead has traditionally been employed in a variety of industrial applications, the current regulations require the phase out of lead in most commercial products. In 2006, rules were issued by the European Union that required the removal of lead from soldering and coatings that are used in electronic parts. Other countries have issued similar regulations.

Electronics and other connections made using lead-based soldering materials are typically highly reliable. Large capital expenditures have been made in the manufacturing infrastructure. There are concerns regarding the reliability of other methods of soldering and materials after the worldwide elimination of lead-based soldering material. There are many alternatives to soldering products based on lead have been created, with the Sn/Ag/Cu (SAC) system is among the most extensively used, these replacements typically have drawbacks that make them unsuitable for environments that are extreme, such as the ones found in automobiles or military vehicles, as well as space vehicles, for example. The SAC system has a highereutectic melting temperature (e.g., M.P. approximately.217.degree. C.) is more than traditional Sn/Pb (m.p. of 183.degree. C. for Sn/Pb 63/37 and 188.degree. C. for the 63/37 Sn/Pb, or 188.degree. Silver is a costly component of the SAC systems, and it’s not feasible to replace the lead-based soldering component with SAC systems. From a cost perspective it is clear that the SAC system can undesirably cause significantly higher production costs due to the material cost of silver, as well as the more durable components required to withstand the higher processing temperature. SAC systems could also lead to the formation of tin whiskers as well as increase the likelihood of electrical shorting.

As replacements for traditional lead-based soldering material, several compositions that are composed of metal nanoparticles were proposed. Nanoparticles may exhibit chemical and physical properties that sometimes differ significantly from the properties observed in the bulk material. Nanoparticles of metal with dimensions of less than 20 nm may have melting points that are considerably lower than bulk metal’s. Copper nanoparticles in particular are able to have a fusion temperature that is comparable to soldering products made from lead. Nanoparticles of copper that are smaller than 10 nanometers in size can fuse to an average temperature of 200.degree. C. or less which results in processing temperatures that are similar to traditional lead-based soldering substances. Nanoparticles of copper are also an option for replacing high-temperature soldering materials such as AuSn, due to their a lower initial temperature and a much greater reflow temperature.

While copper nanoparticles hold great interest because of their compatibility with existing soldering techniques, the creation of monodisperse copper nanoparticles has proven difficult to synthesize, especially in large quantities that are required for commercial production. Furthermore, it is difficult to protect reversibly copper nanoparticles in order to avoid their agglomeration with each other. Protection can sometimes be accomplished with a thin oxide coating or a surfactant, includingpolymers such as polyvinylpyrrolidone, but oftentimes these agents cannot be effectively removed in order that the copper nanoparticles can function as desired in soldering applications. Additionally, these agents could introduce contaminants or be considered contaminants that detrimentally affect the characteristics of the copper nanoparticles. The properties that are affected could include, for instance, electrical and thermal conductivity, mechanical strength, brittleness, and fracturetoughness.

In light of all this, it would be of great benefit to the science of process that can be scaled for the production of monodisperse metal particles especially copper nanoparticles with dimensions of 10nm or less. This invention meets this need and has advantages in this regard as well.

The methods that are described in this invention involve the reaction of an insoluble metal salt with reducing agents within the form of a mixture comprising a first surfactant and a second surfactant. These reactions may be utilized to produce metalnanoparticles. The first surfactant contains a primary amine. The second surfactant is an amino acid that is secondary. The third surfactant is diamine as a chelating agent.

Other examples include making a solution that contains copper salt, a suprafactant, and a second and a 3rd surfactant, permitting the creation of an insoluble copper salt complex in the first solution; mixing a 2nd solution that contains the reducing agent with this insoluble complex to create an reaction mixture, and creating copper nanoparticles using the compound that is insoluble. The first surfactant is comprised of an amine primary. The second surfactant is a secondary amine. The third surfactant contains diamine as a chelating agent.

Certain forms of nanoparticles of copper created by the procedures discussed in this document possess an average melting temperature of 200.degree. C. or less and include at the very least one of three surfactants: a first, second and third surfactants. Thefirst surfactant contains an amine primary. The second surfactant has a secondary amine. The third surfactant has diamine chelating agents.

The above description has described rather in general terms the main features of the disclosure described in order that the detailed description that follows can be better understood. Additional advantages and features of the disclosure will be described hereinafter,which form the subject of the claims.

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