Preparation method and apparatus for metallization slurry for package substrate
By creating a turbulent environment in the reaction vessel, the salt solution of metal A ions and the solution of elemental metal B particles are uniformly mixed to form a multiphase composite core-shell material, which solves the problem of poor uniformity in the prior art and achieves the performance stability and efficient production of metallized slurry.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- GUANGDONG UNIV OF TECH
- Filing Date
- 2024-12-25
- Publication Date
- 2026-07-02
AI Technical Summary
Existing methods for preparing multiphase composite core-shell materials suffer from poor product uniformity, leading to unstable properties such as conductivity and shear strength in metallized slurries, which limits their applications.
A turbulent flow is created in a reaction vessel by using a salt solution of metal A ions and a solution containing elemental metal B particles, and a displacement reaction is carried out to form a multiphase composite core-shell material. By optimizing the preparation method and device design, the uniformity and consistency of the reaction are ensured.
It improves the uniformity of multiphase composite core-shell materials and the performance stability of metallization slurries, simplifies the preparation process, increases production efficiency, and meets diverse application needs.
Smart Images
Figure CN2024142161_02072026_PF_FP_ABST
Abstract
Description
A method and apparatus for preparing metallization paste for packaging substrates.
[0001] Cross-reference of related applications
[0002] This application claims priority to Chinese Patent Application No. 202411905521.1, filed on December 23, 2024, entitled "A method and apparatus for preparing metallization paste for packaging substrate", the entire contents of which are incorporated herein by reference. Technical Field
[0003] This invention relates to the field of metallization paste technology, and in particular to a method and apparatus for preparing a metallization paste for packaging substrates. Background Technology
[0004] A package substrate consists of an electronic circuit carrier (substrate material) and copper electrical interconnect structures (such as electronic circuits and vias). During the production of package substrates, to improve surface conductivity and the reliability of connections with other electronic components, metallization paste is often applied to the holes or surface of the package substrate for metallization treatment. With the development of electronic technology, traditional metallization pastes prepared by mixing elemental nano-metal particles with solvents can no longer meet practical application requirements.
[0005] The above issues place higher demands on the performance of metallization pastes: (1) ensuring reliable mechanical connections; (2) ensuring high electrical conductivity to achieve high-speed transmission between the substrate and the chip; (3) possessing high thermal conductivity to effectively dissipate heat and prevent chip overheating damage; and (4) low-temperature interconnection to avoid large thermal stresses caused by different degrees of thermal expansion of the substrate, chip, and interconnect materials due to excessive temperature changes. Against this background, multiphase composite materials with special physicochemical properties have become a research hotspot for metallization pastes.
[0006] Currently, multiphase composite core-shell materials are typically prepared using the following methods: (1) Coprecipitation method: First, metal elemental particles or metal compound particles are synthesized as the core, and then another metal elemental particle or metal compound particle is grown on the surface of the core to form the shell, thereby obtaining a multiphase composite core-shell material. However, in the above preparation methods, due to the relatively fast reaction rate, the chemical reaction is usually completed before the reactants are fully mixed or there are local concentration differences, resulting in the shape and size of the obtained multiphase composite core-shell material being difficult to maintain uniformity; (2) Electrochemical reaction method: Different materials are deposited on a conductive substrate through electrochemical reaction to form a core-shell structure. However, due to the complexity of the electrode surface reaction and the influence of factors such as the electrolyte solution, the above methods result in poor uniformity of the multiphase composite core-shell material.
[0007] In summary, existing methods for preparing multiphase composite core-shell materials all suffer from poor product uniformity, resulting in poor stability of key properties such as conductivity and shear strength in metallized pastes prepared using multiphase composite core-shell materials, thus limiting the application of metallized pastes. Summary of the Invention
[0008] The purpose of this invention is to provide a method for preparing metallization paste for packaging substrates, which is beneficial to ensure the uniformity of the obtained multiphase composite core-shell material while simplifying the preparation method, improving production efficiency and facilitating industrial production, thereby ensuring the performance stability of the metallization paste and overcoming the shortcomings of the prior art.
[0009] Another objective of this invention is to provide an apparatus for preparing metallization paste for packaging substrates, which, when used in conjunction with a method for preparing metallization paste for packaging substrates, helps to ensure the uniformity of the obtained multiphase composite core-shell material, thereby ensuring the performance stability of the metallization paste.
[0010] To achieve this objective, the present invention adopts the following technical solution:
[0011] A method for preparing a metallization paste for a packaging substrate includes the following steps:
[0012] S1. Prepare a salt solution of metal A ions and a solution containing elemental metal B particles, wherein the reducing power of metal B is greater than that of metal A;
[0013] S2. Simultaneously, a salt solution of metal A ions and a solution containing elemental metal B particles are introduced into the reaction vessel, and a negative pressure is applied to the reaction vessel at the same time, so that both the salt solution of metal A ions and the solution containing elemental metal B particles are in a turbulent state in the reaction vessel and undergo a displacement reaction, so that the outer atoms of the elemental metal B particles are replaced by elemental nano-metal A, forming a multiphase composite core-shell material, and obtaining a metallization paste for packaging substrate.
[0014] Further, step S2 specifically involves: simultaneously introducing gas, a salt solution of metal A ions, and a solution containing elemental metal B particles into the reaction vessel, and simultaneously applying negative pressure to the reaction vessel, so that the gas, the salt solution of metal A ions, and the solution containing elemental metal B particles all form a turbulent state in the reaction vessel, and the salt solution of metal A ions and the solution containing elemental metal B particles undergo a displacement reaction, so that the outer atoms of the elemental metal B particles are replaced by elemental nano-metal A, forming a multiphase composite core-shell material, and obtaining a metallization paste for packaging substrate;
[0015] The gas is either an inert gas or a reducing gas.
[0016] Further, step S2 specifically involves: introducing gas, a salt solution of metal A ions, and a solution containing elemental metal B particles into the reaction vessel in step S2, and simultaneously applying negative pressure to the reaction vessel to create turbulent flow in the gas, the salt solution of metal A ions, and the solution containing elemental metal B particles. The salt solution of metal A ions and the solution containing elemental metal B particles undergo a displacement reaction under heating and / or ultrasonic conditions, causing the outer atoms of the elemental metal B particles to be replaced by elemental nano-metal A, forming a multiphase composite core-shell material, and obtaining a metallization paste for the packaging substrate.
[0017] Further, in step S2, the inert gas is any one or a combination of nitrogen, carbon dioxide, argon and helium;
[0018] The reducing gas is either hydrogen or carbon monoxide.
[0019] Further, in step S2, the mixing ratio of the salt solution of metal A ions and the solution containing elemental metal B particles is calculated according to the volume ratio as (0.1~10):1.
[0020] Furthermore, in step S1, the metal A includes any one of copper, zinc, nickel, and silver;
[0021] The metal B includes any one of aluminum, magnesium, copper, zinc, nickel, and silver.
[0022] An apparatus for preparing metallization paste for packaging substrates, used to implement the above-mentioned method for preparing metallization paste for packaging substrates, includes a storage container 1, an air inlet pipe, a first outlet pipe, a reaction vessel, a vacuum pump, and a collection container. The storage container, the first outlet pipe, the reaction vessel, and the collection container are interconnected from top to bottom. The outlet of the collection container is interconnected with the inlet of the vacuum pump, and the collection container and the vacuum pump are arranged side by side.
[0023] The inlet pipe is located above the reaction vessel. The end of the inlet pipe is at the same horizontal level as the end of the first outlet pipe. The outlet of the inlet pipe is connected to both the outlet of the first outlet pipe and the inlet of the reaction vessel. The inlet pipe is used to transport inert gas or reducing gas to the reaction vessel.
[0024] The air intake pipe is provided with a second valve for opening and closing the air intake pipe;
[0025] The first discharge pipe is equipped with a first valve for opening and closing the first discharge pipe;
[0026] The storage container, the first valve, and the first discharge pipe constitute a discharge assembly. At least two discharge assemblies are provided, and the two discharge assemblies are located on the left and right sides of the air inlet pipe, respectively.
[0027] Furthermore, the reaction vessel includes a reaction tube and a water bath ultrasonic cooker. The reaction tube is located inside the water bath ultrasonic cooker, and the inlet of the reaction tube is interconnected with the outlet of the first discharge pipe and the outlet of the air inlet pipe. The outlet of the reaction tube is interconnected with the inlet of the collection container. The water bath ultrasonic cooker is used to heat and / or sonicate the reaction tube.
[0028] Furthermore, the reaction tube includes a feeding section, a reaction section, and a discharge section connected sequentially from top to bottom. The feeding section and the discharge section are both vertically arranged and have a straight shape. The reaction section has a spiral shape, and the spiral axis of the reaction section extends horizontally.
[0029] Furthermore, it also includes a second discharge pipe, a feed pipe, and a connecting pipe. The inlet of the second discharge pipe is connected to the outlet of the discharge section, and the second discharge pipe is provided with a discharge port. The discharge port is connected to the inlet of the feed pipe, and the outlet of the feed pipe is connected to the inlet of the collection container.
[0030] The feed pipe is equipped with a third valve for opening and closing the feed pipe;
[0031] The discharge port, the feed pipe, the third valve and the collection container constitute a collection assembly. Multiple collection assemblies are provided, and the collection assemblies are arranged side by side. The outlet of the collection container of the collection assembly located at the end of the second discharge pipe is connected to the inlet of the air pump.
[0032] The number of the connecting pipes is set to multiple, and the collection containers of two adjacent collection components are connected to each other through one of the connecting pipes;
[0033] The connecting pipe is equipped with a fourth valve for opening and closing the connecting pipe.
[0034] The technical solution provided by this invention may include the following beneficial effects:
[0035] 1. In this technical solution, the metal in the salt solution containing metal A ions is metal A, and the metal in the solution containing elemental metal B particles is metal B. Metal B has a greater reducing power than metal A. When the two solutions are mixed, elemental metal B can spontaneously displace metal A ions from the salt solution containing metal A ions. During the displacement reaction, the outer atoms of elemental metal B particles are replaced by elemental nano-metal A, forming a core-shell structure (i.e., multiphase composite core-shell material) in which elemental nano-metal A encapsulates elemental metal B particles.
[0036] 2. Simultaneously, a salt solution containing metal A ions and a solution containing elemental metal B particles are introduced into reaction vessel 5, and a negative pressure is applied to reaction vessel 5 at the same time, causing both the metal A ion salt solution and the solution containing elemental metal B particles to form a turbulent state within reaction vessel 5, thus creating a turbulent environment. Under this turbulent environment, the metal A ion salt solution and the solution containing elemental metal B particles move irregularly and mix with each other in reaction vessel 5, ensuring that the two solutions undergo a displacement reaction in a fully and uniformly mixed state. This greatly improves the uniformity of the displacement reaction and effectively avoids the problem of reaction inhomogeneity caused by local concentration differences, thereby ensuring the consistency of the shape and size of the obtained multiphase composite core-shell material, exhibiting extremely high uniformity. At the same time, this turbulent environment promotes the complete reaction of the metal A ion salt solution and the solution containing elemental metal B particles in reaction vessel 5, effectively avoiding inconsistencies in the shape and size of the multiphase composite core-shell material due to incomplete reaction, which also helps to ensure the uniformity of the multiphase composite core-shell material. Furthermore, the constructed turbulent environment effectively prevents the agglomeration of the obtained multiphase composite core-shell material, which also helps to ensure the uniformity of the multiphase composite core-shell material. In other words, this technical solution ensures the uniformity of the multiphase composite core-shell material and the performance stability of the metallization slurry by constructing a turbulent environment and making full use of its multiple advantages. Attached Figure Description
[0037] Figure 1 is a schematic diagram of the apparatus for preparing metallization paste for packaging substrates according to the present invention.
[0038] The components include: storage container 1, first valve 2, air inlet pipe 3, first discharge pipe 4, reaction container 5, reaction pipe 51, water bath ultrasonic cooker 52, vacuum pump 6, collection container 7, second discharge pipe 8, feed pipe 9, and connecting pipe 10. Detailed Implementation
[0039] Embodiments of the present invention are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.
[0040] This technical solution provides a method for preparing metallization paste for packaging substrates, including the following steps:
[0041] S1. Prepare a salt solution of metal A ions and a solution containing elemental metal B particles, wherein the reducing power of metal B is greater than that of metal A;
[0042] S2. Simultaneously, a salt solution of metal A ions and a solution containing elemental metal B particles are introduced into the reaction vessel 5, and a negative pressure is applied to the reaction vessel 5 at the same time, so that both the salt solution of metal A ions and the solution containing elemental metal B particles are in a turbulent state in the reaction vessel 5, and a displacement reaction is carried out, so that the outer atoms of the elemental metal B particles are replaced by elemental nano-metal A, forming a multiphase composite core-shell material, and obtaining a metallization paste for packaging substrate.
[0043] To address the issue of poor uniformity in existing multiphase composite core-shell materials, which affects the performance stability of metallization pastes, this technical solution proposes a method for preparing metallization paste for packaging substrates. The method comprises two steps: S1 (preparing a salt solution of metal A ions and a solution containing elemental metal B particles) and S2 (constructing a turbulent environment and performing a displacement reaction). By optimizing the preparation process, selecting the best raw materials, and constructing a turbulent environment, this method simplifies the preparation process, improves production efficiency, and facilitates industrial production while ensuring the uniformity of the obtained multiphase composite core-shell material. This, in turn, ensures the performance stability of the metallization paste to meet practical application requirements.
[0044] Specifically, in this technical solution, the metal in the salt solution containing metal A ions is metal A, and the metal in the solution containing elemental metal B particles is metal B. Furthermore, metal B has a greater reducing power than metal A. This allows elemental metal B to spontaneously displace metal A ions from the salt solution containing metal A ions when the two solutions are mixed. During the displacement reaction, the outer atoms of the elemental metal B particles are replaced by elemental nano-metal A, forming a core-shell structure (i.e., a multiphase composite core-shell material) in which elemental nano-metal A encapsulates elemental metal B particles.
[0045] More specifically, this method simultaneously introduces a salt solution containing metal A ions and a solution containing elemental metal B particles into reaction vessel 5, while applying negative pressure to reaction vessel 5 concurrently. This creates a turbulent environment where both the metal A ion salt solution and the solution containing elemental metal B particles are in a turbulent state. Under this turbulent environment, the metal A ion salt solution and the solution containing elemental metal B particles move irregularly and mix with each other in reaction vessel 5. This ensures that the two solutions undergo a displacement reaction in a fully and uniformly mixed state, greatly improving the uniformity of the displacement reaction and effectively avoiding the problem of uneven reaction caused by local concentration differences. This ensures the consistency of the shape and size of the obtained multiphase composite core-shell material, exhibiting extremely high uniformity. Simultaneously, this turbulent environment promotes the complete reaction of the metal A ion salt solution and the solution containing elemental metal B particles in reaction vessel 5, effectively avoiding inconsistencies in the shape and size of the multiphase composite core-shell material due to incomplete reaction, which also helps ensure the uniformity of the multiphase composite core-shell material. Furthermore, the constructed turbulent environment effectively prevents the agglomeration of the obtained multiphase composite core-shell material, which also helps to ensure the uniformity of the multiphase composite core-shell material. In other words, this technical solution ensures the uniformity of the multiphase composite core-shell material and the performance stability of the metallization slurry by constructing a turbulent environment and making full use of its multiple advantages.
[0046] Furthermore, the preparation method of this technical solution is simple, and the constructed turbulent environment not only accelerates the mass transfer process of reactants and promotes mixing between reactants, but also increases the probability of reactant molecules colliding and reacting per unit time, thereby increasing the reaction rate. These synergistic effects not only greatly improve production efficiency but also lay a solid foundation for industrial-scale production.
[0047] Preferably, in step S1, the particle size of the elemental B particles is 20-80 nm.
[0048] By limiting the particle size of elemental metal B particles, a more uniform particle size distribution can be ensured in the multiphase composite core-shell material generated during the reaction. This helps reduce particle size differences and improves the uniformity of the multiphase composite core-shell material. Furthermore, when the particle size of elemental metal B particles is in the range of 20–80 nm, its specific surface area is larger, the number of surface atoms is greater, and the number of reactive sites increases. This is beneficial for increasing the displacement reaction rate between metal B particles and metal A ions in the salt solution, thereby improving production efficiency and facilitating industrial production.
[0049] Further explanation: Step S2 specifically involves simultaneously introducing gas, a salt solution of metal A ions, and a solution containing elemental metal B particles into the reaction container 5, and simultaneously applying negative pressure to the reaction container 5, causing the gas, the salt solution of metal A ions, and the solution containing elemental metal B particles to all form a turbulent state within the reaction container 5. Furthermore, the salt solution of metal A ions and the solution containing elemental metal B particles undergo a displacement reaction, causing the outer atoms of the elemental metal B particles to be replaced by elemental nano-metal A, forming a multiphase composite core-shell material, and obtaining a metallization paste for the packaging substrate.
[0050] The gas is either an inert gas or a reducing gas.
[0051] By simultaneously introducing gas, a salt solution containing metal A ions, and a solution containing elemental metal B particles into reaction vessel 5, a turbulent gas-liquid mixing state is created within vessel 5. The turbulent gas also promotes the uniformity of mixing and the completeness of the reaction between the metal A ion salt solution and the solution containing elemental metal B particles, further ensuring the homogeneity of the multiphase composite core-shell material. Furthermore, the turbulent state ensures a uniform gas distribution within the reaction vessel, resulting in more uniform temperature and pressure environments within reaction vessel 5. This helps reduce the occurrence of localized overheating or overcooling, improving the stability and controllability of the reaction, which also contributes to ensuring the homogeneity of the multiphase composite core-shell material. In other words, this technical solution, by introducing gas and creating a turbulent environment, fully utilizes its multiple advantages to further ensure the homogeneity of the multiphase composite core-shell material, thereby ensuring the performance stability of the metallization paste used in the packaging substrate.
[0052] Furthermore, when the gas is an inert or reducing gas, it can avoid oxidation reactions that may occur during the displacement reaction, thus ensuring the purity of the reaction and the uniformity of the multiphase composite core-shell material. Additionally, when the gas is a reducing gas, it can promote the reduction of metal A ions in the salt solution to elemental nano-metal A, which then deposits on the surface of elemental metal B particles, also contributing to the formation of multiphase composite core-shell materials.
[0053] Preferably, step S2 specifically involves: introducing gas, a salt solution of metal A ions, and a solution containing elemental metal B particles into the reaction container 5 in step S2, and simultaneously applying negative pressure to the reaction container 5, so that the gas, the salt solution of metal A ions, and the solution containing elemental metal B particles all form a turbulent state in the reaction container 5, and the salt solution of metal A ions and the solution containing elemental metal B particles undergo a displacement reaction, so that the outer atoms of the elemental metal B particles are replaced by elemental nano-metal A, forming a multiphase composite core-shell material dispersion;
[0054] The dispersion of multiphase composite core-shell material was separated to obtain the multiphase composite core-shell material;
[0055] Multiphase composite core-shell material is mixed with solvent and flux to obtain metallization paste for packaging substrate.
[0056] Further optimization of the preparation method of metallization paste for packaging substrates will facilitate the preparation of pastes with appropriate solvents and fluxes according to actual needs, thereby improving the adaptability of the products.
[0057] It should be noted that solvents can include ethanol and propanol, and the specific type is not limited here.
[0058] Fluxes can be zinc chloride, ammonium chloride, and activated rosin fluxes, etc., and the specific types are not limited here.
[0059] Further explanation: Step S2 specifically involves introducing gas, a salt solution of metal A ions, and a solution containing elemental metal B particles into the reaction container 5 in step S2, and simultaneously applying negative pressure to the reaction container 5 to create turbulent flow in the gas, the salt solution of metal A ions, and the solution containing elemental metal B particles. The salt solution of metal A ions and the solution containing elemental metal B particles undergo a displacement reaction under heating and / or ultrasonic conditions, causing the outer atoms of the elemental metal B particles to be replaced by elemental nano-metal A, forming a multiphase composite core-shell material, and obtaining a metallization paste for the packaging substrate.
[0060] When the displacement reaction is carried out under heating conditions, it can be ensured that the displacement reaction occurs at the optimal temperature, thereby improving the quality and yield of multiphase composite core-shell materials. When the displacement reaction is carried out under ultrasonic conditions, the cavitation effect and microjets generated by ultrasound can enhance the mixing effect between the salt solution of metal A ions and the solution containing elemental metal B particles, promoting the displacement reaction between the two solutions and thus improving production efficiency.
[0061] To further explain, in step S2, the inert gas is any one or a combination of nitrogen, carbon dioxide, argon, and helium;
[0062] The reducing gas is either hydrogen or carbon monoxide.
[0063] The selection of inert and reducing gases is optimized, and the selected inert and reducing gases have a high cost-performance ratio. This not only helps to select appropriate raw materials according to actual needs and improve the flexibility of the formulation, but also helps to save production costs while ensuring the performance of metallization paste for packaging substrates.
[0064] It should be noted that carbon dioxide bubbles, in their dissolved state, are more likely to break and disperse upon encountering the pore surface of a porous material, thus promoting more efficient precipitation of the carbon dioxide bubbles from the solution. Therefore, in this technical solution, when carbon dioxide is used as the inert gas, the reaction vessel 5 needs to be equipped with a porous material to allow the carbon dioxide bubbles to separate from the solution more quickly, thereby improving the mixing uniformity of the reaction solution and creating more favorable conditions for the displacement reaction.
[0065] To further explain, in step S2, the mixing ratio of the salt solution of metal A ions and the solution containing elemental metal B particles is (0.1~10):1, calculated by volume ratio.
[0066] This technical solution optimizes the mixing ratio of a salt solution containing metal A ions and a solution containing elemental metal B particles. This not only facilitates a more effective displacement reaction between metal A ions in the salt solution and elemental metal B particles in the solution, ensuring the homogeneity of the multiphase composite core-shell material, but also reduces the residue of unreacted metal A ions, thereby improving the purity of the multiphase composite core-shell material. Furthermore, optimizing the mixing ratio of the metal A ion salt solution and the solution containing elemental metal B particles allows for the preparation of multiphase composite core-shell materials with different core-shell ratios to meet the needs of various application fields.
[0067] To further explain, in step S1, the metal A includes any one of copper, zinc, nickel, and silver;
[0068] The metal B includes any one of aluminum, magnesium, copper, zinc, nickel, and silver.
[0069] By optimizing the types of metal A and metal B, metallization pastes for packaging substrates with different physical and chemical properties can be prepared to meet diverse application requirements.
[0070] An apparatus for preparing metallization paste for packaging substrates, used to implement the above-mentioned method for preparing metallization paste for packaging substrates, includes a storage container 1, an air inlet pipe 3, a first outlet pipe 4, a reaction vessel 5, a vacuum pump 6, and a collection container 7. The storage container 1, the first outlet pipe 4, the reaction vessel 5, and the collection container 7 are interconnected from top to bottom. The outlet of the collection container 7 is interconnected with the inlet of the vacuum pump 6, and the collection container 7 and the vacuum pump 6 are arranged side by side.
[0071] The inlet pipe 3 is located above the reaction vessel 5. The end of the inlet pipe 3 is at the same horizontal level as the end of the first outlet pipe 4. The outlet of the inlet pipe 3 is connected to the outlet of the first outlet pipe 4 and the inlet of the reaction vessel 5. The inlet pipe 3 is used to transport inert gas or reducing gas to the reaction vessel 5.
[0072] The air intake pipe 3 is provided with a second valve for opening and closing the air intake pipe 3;
[0073] The first discharge pipe 4 is provided with a first valve 2 for opening and closing the first discharge pipe 4;
[0074] The storage container 1, the first valve 2, and the first discharge pipe 4 constitute a discharge assembly. At least two discharge assemblies are provided, and the two discharge assemblies are located on the left and right sides of the air inlet pipe 3, respectively.
[0075] This solution also proposes an apparatus for preparing metallization paste for packaging substrates, which, when combined with the method for preparing metallization paste for packaging substrates, helps to ensure the uniformity of the obtained multiphase composite core-shell material, thereby ensuring the performance stability of the metallization paste.
[0076] Specifically, as shown in Figure 1, the preparation apparatus of this scheme includes a storage container 1, an inlet pipe 3, a first outlet pipe 4, a reaction vessel 5, a vacuum pump 6, and a collection container 7. The storage container 1, the first outlet pipe 4, the reaction vessel 5, and the collection container 7 are interconnected from top to bottom. The outlet of the collection container 7 is interconnected with the inlet of the vacuum pump 6, and the collection container 7 and the vacuum pump 6 are arranged side by side. The first outlet pipe 4 is provided with a first valve 2 for opening and closing the first outlet pipe 4. The outlet of the inlet pipe 3 is interconnected with both the outlet of the first outlet pipe 4 and the inlet of the reaction vessel 5. The inlet pipe 3 is used to transport inert gas to the reaction vessel 5. A storage container 1, a first valve 2, and a first outlet pipe 4 constitute a set of discharge components. At least two sets of discharge components are provided, and the two sets of discharge components are located on the left and right sides of the inlet pipe 3, respectively.
[0077] The workflow of this equipment is as follows: First, the salt solution of metal A ions and the solution containing elemental metal B particles are respectively loaded into the storage containers 1 of the two discharge components. Simultaneously, the first valve 2 and the second valve of the two discharge components are opened, allowing the inlet pipe 3 to supply inert or reducing gas to the reaction container 5, and allowing the salt solution of metal A ions and the solution containing elemental metal B particles to flow into the reaction container 5. During this process, the vacuum pump 6 is activated, causing the gas, the salt solution of metal A ions, and the solution containing elemental metal B particles to all form a turbulent state within the reaction container 5. Under this turbulent environment, the salt solution of metal A ions and the solution containing elemental metal B particles move irregularly and mix with each other in the reaction container 5, allowing for thorough and uniform mixing and a displacement reaction to occur, resulting in a highly uniform multiphase composite core-shell material, and ultimately, a metallization paste for packaging substrates.
[0078] Further explanation: The reaction vessel 5 includes a reaction tube 51 and a water bath ultrasonic cooker 52. The reaction tube 51 is located inside the water bath ultrasonic cooker 52, and the inlet of the reaction tube 51 is interconnected with the outlet of the first discharge pipe 4 and the outlet of the air inlet pipe 3. The outlet of the reaction tube 51 is interconnected with the inlet of the collection container 7. The water bath ultrasonic cooker 52 is used to heat and / or sonicate the reaction tube 51.
[0079] By configuring the reaction vessel 5, which includes a reaction tube 51 and a water bath ultrasonic bath 52, the water bath ultrasonic bath 52 provides a uniform and controllable heating environment for the reaction tube 51, ensuring that the displacement reaction proceeds at the optimal temperature, thereby improving the quality and yield of the multiphase composite core-shell material. Furthermore, the water bath ultrasonic bath 52 not only provides heating but also ultrasonically treats the salt solution of metal A ions and the solution containing elemental metal B particles within the reaction tube 51. The cavitation effect and microjets generated by the ultrasound enhance the mixing between the two solutions, promoting the displacement reaction and improving production efficiency. In addition, ultrasound can break down agglomerates in the solution, making the multiphase composite core-shell material more dispersed and uniform, thus improving its homogeneity.
[0080] To further explain, the reaction tube 51 includes a feeding section, a reaction section, and a discharge section connected sequentially from top to bottom. The feeding section and the discharge section are both vertically arranged and have a straight shape. The reaction section has a spiral shape and the spiral axis of the reaction section extends horizontally.
[0081] The reaction section employs a spiral design, which generates rotational and shear forces as the salt solution containing metal A ions and the solution containing elemental metal B particles flow through the reaction section. This enhances the mixing effect between the two solutions, improving the efficiency and uniformity of the displacement reaction, thus contributing to the homogeneity of the multiphase composite core-shell material. Furthermore, the spiral shape prolongs the residence time of the metal A ion salt solution and the solution containing elemental metal B particles within the reaction tube 51, improving the completeness of the reaction and further enhancing the homogeneity of the multiphase composite core-shell material. In addition, the horizontal arrangement of the reaction section saves floor space and improves the compactness of the preparation apparatus.
[0082] Further explanation: It also includes a second discharge pipe 8, a feed pipe 9, and a connecting pipe 10. The inlet of the second discharge pipe 8 is connected to the outlet of the discharge section, and the second discharge pipe 8 is provided with a discharge port. The discharge port is connected to the inlet of the feed pipe 9, and the outlet of the feed pipe 9 is connected to the inlet of the collection container 7.
[0083] The feed pipe 9 is provided with a third valve for opening and closing the feed pipe 9;
[0084] The discharge port, the feed pipe 9, the third valve and the collection container 7 constitute a collection assembly. Multiple collection assemblies are provided, and the collection assemblies are arranged side by side. The outlet of the collection container 7 of the collection assembly located at the end of the second discharge pipe 8 is connected to the inlet of the air pump 6.
[0085] The number of the connecting pipes 10 is set to be multiple, and the collection containers 7 of two adjacent collection components are connected to each other through one of the connecting pipes 10.
[0086] The connecting pipe 10 is provided with a fourth valve for opening and closing the connecting pipe 10.
[0087] By setting up multiple collection components, not only can the metallization paste for the encapsulation substrate be collected simultaneously through the collection containers 7 of multiple collection components, thus significantly improving collection efficiency, but it also facilitates a more uniform distribution of the metallization paste into the collection containers 7 of multiple collection components, reducing the accumulation and aggregation of the metallization paste in the collection container 7 of a single collection component. Furthermore, each collection component is equipped with a third valve, allowing operators to flexibly adjust the collection process as needed, improving the flexibility of the device.
[0088] By setting up the connecting pipe 10, the operator can flexibly adjust the product distribution in each collection container 7 as needed. For example, when a collection container 7 is about to overflow, the corresponding fourth valve can be opened to transfer some of the product to an adjacent collection container 7, thereby avoiding the overflow and waste of metallization paste for the encapsulation substrate and improving the flexibility of the device.
[0089] The technical solution of the present invention will be further illustrated below through specific embodiments.
[0090] Example 1
[0091] S1. Prepare a silver ammonia solution and a solution containing nano-copper; wherein the nano-copper has a particle size of 30 nm; the concentration of silver ions in the silver ammonia solution is 0.01 mol / L; the concentration of nano-copper in the solution containing nano-copper is 0.7 mol / L; the mixing ratio of the silver ammonia solution and the solution containing nano-copper is 0.1:1 according to the volume ratio.
[0092] S2. Simultaneously, nitrogen gas, silver ammonia solution, and a solution containing nano-copper are introduced into reaction vessel 5, and a negative pressure is applied to reaction vessel 5 at the same time, so that nitrogen gas, silver ammonia solution, and solution containing nano-copper are all in a turbulent state in reaction vessel 5. The silver ammonia solution and solution containing nano-copper undergo a displacement reaction under a heating condition of 80°C, so that the outer layer atoms of nano-copper are replaced with nano-silver, forming a multiphase composite core-shell material, and obtaining metallization paste for packaging substrate.
[0093] The shape and size of the multiphase composite core-shell material in the dispersion obtained in Example 1 were observed by electron microscopy. The results showed that the shape and size of the multiphase composite core-shell material obtained in Example 1 were relatively consistent, that is, the multiphase composite core-shell material in Example 1 had high uniformity.
[0094] In addition, under otherwise identical conditions, the metallization paste for the packaging substrate obtained in Example 1 was coated onto five substrates. Interconnect chips were then placed on the surfaces of all five substrates coated with the metallization paste, and after sintering, five interconnect devices were obtained. The shear strength of the five interconnect devices was tested using an IC packaging solder strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnect devices was tested using an ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnect devices are basically consistent, proving that the metallization paste for the packaging substrate obtained in Example 1 has high performance stability.
[0095] Example 2
[0096] S1. Prepare a copper sulfate solution and a solution containing zinc nanoparticles; wherein the particle size of the zinc nanoparticles is 40 nm; the concentration of copper ions in the copper sulfate solution is 0.02 mol / L; the concentration of zinc nanoparticles in the solution containing zinc nanoparticles is 1 mol / L; the mixing ratio of the copper sulfate solution and the solution containing zinc nanoparticles is 0.1:1 according to the volume ratio.
[0097] S2. Simultaneously, hydrogen gas, copper sulfate solution, and a solution containing nano-zinc are introduced into reaction vessel 5, and a negative pressure is applied to reaction vessel 5 at the same time, so that hydrogen gas, copper sulfate solution, and solution containing nano-zinc are all in a turbulent state in reaction vessel 5. The copper sulfate solution and solution containing nano-zinc undergo a displacement reaction under ultrasonic conditions, so that the outer layer atoms of nano-zinc are replaced by nano-copper, forming a multiphase composite core-shell material, and obtaining metallization paste for packaging substrate.
[0098] The shape and size of the multiphase composite core-shell material in the dispersion obtained in Example 2 were observed by electron microscopy. The results showed that the shape and size of the multiphase composite core-shell material obtained in Example 2 were relatively consistent, that is, the multiphase composite core-shell material in Example 2 had high uniformity.
[0099] In addition, under otherwise identical conditions, the metallization paste for the packaging substrate obtained in Example 2 was coated onto five substrates. Interconnect chips were then placed on the surfaces of all five substrates coated with the metallization paste, and after sintering, five interconnect devices were obtained. The shear strength of the five interconnect devices was tested using an IC packaging solder strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnect devices was tested using an ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnect devices are basically consistent, proving that the metallization paste for the packaging substrate obtained in Example 2 has high performance stability.
[0100] Example 3
[0101] Step S1. Prepare a silver nitrate solution and a solution containing nano-nickel; wherein the nano-nickel has a particle size of 50 nm; the concentration of silver ions in the silver nitrate solution is 0.03 mol / L; the concentration of nano-nickel in the solution containing nano-nickel is 0.8 mol / L; the mixing ratio of the silver nitrate solution and the solution containing nano-nickel is 2:1 according to the volume ratio.
[0102] S2. Argon gas, silver nitrate solution, and a solution containing nano-nickel are simultaneously introduced into reaction vessel 5, and a negative pressure is applied to reaction vessel 5 at the same time, so that argon gas, silver nitrate solution, and solution containing nano-nickel all form a turbulent state in reaction vessel 5. The silver nitrate solution and the solution containing nano-nickel undergo a displacement reaction under a heating condition of 100°C, so that the outer atoms of nano-nickel are replaced by nano-silver, forming a multiphase composite core-shell material, and obtaining a metallization paste for packaging substrate.
[0103] The shape and size of the multiphase composite core-shell material in the dispersion obtained in Example 3 were observed by electron microscopy. The results showed that the shape and size of the multiphase composite core-shell material obtained in Example 3 were relatively consistent, that is, the multiphase composite core-shell material in Example 3 had high uniformity.
[0104] In addition, under otherwise identical conditions, the metallization paste for the packaging substrate obtained in Example 3 was coated onto five substrates. Interconnect chips were then placed on the surfaces of all five substrates coated with the metallization paste, and after sintering, five interconnect devices were obtained. The shear strength of the five interconnect devices was tested using an IC packaging solder strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnect devices was tested using an ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnect devices are basically consistent, proving that the metallization paste for the packaging substrate obtained in Example 3 has high performance stability.
[0105] Comparative Example 1
[0106] The preparation method and raw materials used in Comparative Example 1 are the same as those in Example 1, except that Comparative Example 1 lacks step S2.
[0107] The shape and size of the multiphase composite core-shell material in the dispersion obtained in Comparative Example 1 were observed by electron microscopy. The results showed that the shape and size of the multiphase composite core-shell material obtained in Comparative Example 1 had poor uniformity, that is, the multiphase composite core-shell material in Comparative Example 1 had poor uniformity.
[0108] In addition, under identical conditions, the metallization paste obtained in Comparative Example 1 was applied to five substrates. Interconnect chips were then placed on the surfaces of all five substrates coated with the metallization paste, and after sintering, five interconnect devices were obtained. The shear strength of the five interconnect devices was tested using an IC package solder strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnect devices was tested using an ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnect devices fluctuated significantly, demonstrating that the performance stability of the metallization paste obtained in Comparative Example 1 is poor.
[0109] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.
[0110] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values of the components and steps set forth in these embodiments do not limit the scope of the invention. It should also be understood that, for ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following figures denote similar items; therefore, once an item is defined in one figure, it need not be further discussed in subsequent figures.
[0111] It should be noted that the terms "first," "second," etc., used in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented in sequences other than those illustrated or described herein.
[0112] The technical principles of the present invention have been described above with reference to specific embodiments. These descriptions are merely for explaining the principles of the invention and should not be construed as limiting the scope of protection of the invention in any way. Based on this explanation, those skilled in the art can readily conceive of other specific embodiments of the invention without inventive effort, and these embodiments will all fall within the scope of protection of the present invention.
Claims
A method for preparing a metallization paste for a packaging substrate, characterized by The method comprises the following steps: S1. preparing a salt solution of metal A ions and a solution containing metal B particles, and the reducing property of the metal B is greater than that of the metal A; S2. simultaneously introducing the salt solution of metal A ions and the solution containing metal B particles into a reaction container, and synchronously applying negative pressure to the reaction container, so that the salt solution of metal A ions and the solution containing metal B particles form turbulent flow states in the reaction container, and a displacement reaction is performed to displace the outer atoms of the metal B particles with metal A nanoparticles to form a multi-phase composite core-shell material, thereby obtaining a metallized paste for packaging substrates. The preparation method of the metallization paste for packaging substrates according to claim 1, characterized in that, In step S2, the inert gas is any one or a combination of nitrogen, carbon dioxide, argon and helium; The reducing gas is any one of hydrogen and carbon monoxide gas. The preparation method of the metallization paste for packaging substrates according to claim 2, characterized in that, In step S2, the mixing ratio of the salt solution of metal A ions and the solution containing metal B particles is (0.1-10):1, calculated according to the volume ratio. The preparation method of the metallization paste for packaging substrates according to claim 2, characterized in that, In step S1, the metal A includes any one of copper, zinc, nickel and silver; The metal B includes any one of aluminum, magnesium, copper, zinc, nickel and silver. The preparation method of the metallization paste for packaging substrates according to claim 1, characterized in that, The preparation method of the metallized paste for packaging substrates according to any one of claims 1-6 comprises a storage container 1, a gas inlet pipe, a first discharge pipe, a reaction container, a gas pump and a collection container. The storage container, the first discharge pipe, the reaction container and the collection container are sequentially and mutually communicated from top to bottom. The outlet of the collection container and the inlet of the gas pump are mutually communicated, and the collection container and the gas pump are arranged side by side. The preparation method of the metallization paste for packaging substrates according to claim 1, characterized in that, A preparation device of a metallization paste for a packaging substrate, characterized by comprising the following steps of: The gas inlet pipe is located above the reaction container, the end of the gas inlet pipe is located at the same horizontal plane as the end of the first discharge pipe, and the outlet of the gas inlet pipe communicates with the outlet of the first discharge pipe and the inlet of the reaction container, and the gas inlet pipe is used to deliver inert gas or reducing gas to the reaction container. The gas inlet pipe is provided with a second valve for opening and closing the gas inlet pipe. The first discharge pipe is provided with a first valve for opening and closing the first discharge pipe. The storage container, the first valve and the first discharge pipe form a discharge assembly, and at least two discharge assemblies are provided, and the two discharge assemblies are located on the left and right sides of the gas inlet pipe. The preparation device of the metallization paste for packaging substrates according to claim 7, characterized in that, The reaction container includes a reaction pipe and a water bath ultrasonic pot, the reaction pipe is located inside the water bath ultrasonic pot, the inlet of the reaction pipe communicates with the outlet of the first discharge pipe and the outlet of the gas inlet pipe, and the outlet of the reaction pipe communicates with the inlet of the collection container; the water bath ultrasonic pot is used to heat and / or ultrasonic the reaction pipe. The preparation device of the metallization paste for packaging substrates according to claim 8, characterized in that, The reaction pipe includes a feeding section, a reaction section and a discharge section connected in sequence from top to bottom, the feeding section and the discharge section are vertically arranged, the shapes of the feeding section and the discharge section are linear, and the shape of the reaction section is spiral, and the spiral axis of the reaction section extends horizontally. The preparation device of the metallization paste for packaging substrates according to claim 9, characterized in that, It also includes a second discharge pipe, a feeding pipe and a communication pipe, the inlet of the second discharge pipe communicates with the outlet of the discharge section, and the second discharge pipe is provided with a discharge port; the discharge port communicates with the inlet of the feeding pipe, and the outlet of the feeding pipe communicates with the inlet of the collection container; The feeding pipe is provided with a third valve for opening and closing the feeding pipe; The discharge port, the feeding pipe, the third valve and the collection container form a collection assembly, and multiple collection assemblies are provided, the multiple collection assemblies are arranged side by side, and the outlet of the collection container of the collection assembly located at the end of the second discharge pipe communicates with the inlet of the air pump; The number of communication pipes is multiple, and the collection containers of adjacent two collection assemblies communicate with each other through a communication pipe; The communication pipe is provided with a fourth valve for opening and closing the communication pipe.