Preparation method and device of metallized slurry for packaging substrate

Abstract

The method comprises the following steps: S1, preparing a salt solution of metal A ions and a solution containing elemental metal B particles, wherein the reducibility of the metal B is greater than that of the metal A; s2, simultaneously introducing a salt solution of metal A ions and a solution containing elemental metal B particles into the reaction container, and synchronously applying negative pressure into the reaction container, so that the salt solution of the metal A ions and the solution containing the elemental metal B particles form a turbulent flow state in the reaction container, and carrying out a replacement reaction, and replacing outer-layer atoms of the elemental metal B particles with the elemental nano metal A to form a multiphase composite core-shell material, thereby obtaining the metallized slurry for the packaging substrate. According to the preparation method of the metallization slurry for the packaging substrate, the uniformity of the obtained multiphase composite core-shell material is ensured on the premise of simplifying the preparation method, improving the production efficiency and facilitating industrial production, and then the performance stability of the metallization slurry is ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of metallization slurry, and in particular to a method and a device for preparing metallization slurry for a packaging substrate. Background Art

[0002] The package substrate is composed of an electronic circuit carrier (substrate material) and a copper electrical interconnection structure (such as electronic circuits, vias, etc.). In the production process of the package substrate, in order to improve the conductivity of its surface and the connection reliability with other electronic components, it is often necessary to apply a metallization slurry inside the hole or on the surface of the package substrate to metallize the package substrate. With the development of electronic technology, the traditional metallization slurry prepared by mixing single-element nano-metal particles with solvents can no longer meet the actual use requirements.

[0003] The above problems put forward higher requirements on the performance of metallization paste: (1) ensure reliable mechanical connection; (2) ensure high electrical conductivity to achieve high-speed transmission between substrate and chip; (3) have high thermal conductivity and effectively dissipate heat to prevent chip overheating and damage; (4) low-temperature interconnection to avoid large thermal stress caused by different thermal expansion of substrate, chip and interconnection materials due to large temperature changes. In this context, multiphase composite materials with special physical and chemical properties have become a research hotspot for metallization paste.

[0004] At present, multiphase composite core-shell materials generally include the following preparation methods: (1) coprecipitation method, first synthesizing metal single substance particles or metal compound particles as the inner core, and then growing another metal single substance particle or metal compound particle on the surface of the inner core by coprecipitation method to form an outer shell, thereby obtaining a multiphase composite core-shell material. However, in the above preparation method, due to the relatively fast reaction speed, the chemical reaction is usually completed when the reactants are not 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 consistency and poor uniformity; (2) electrochemical reaction method, depositing different materials on a conductive substrate through electrochemical reaction to form a core-shell structure. However, due to the influence of factors such as the complexity of the electrode surface reaction and the electrolyte solution, the above method results in poor uniformity of the multiphase composite core-shell material.

[0005] In summary, the existing preparation methods of multi-phase composite core-shell materials all have the defect of poor product uniformity, which leads to poor stability of key properties such as conductivity and shear strength of the metallization slurry prepared using the multi-phase composite core-shell material, limiting the application of the metallization slurry. Summary of the invention

[0006] The purpose of the present invention is to propose a method for preparing a metallization paste for a packaging substrate, which is beneficial to ensure the uniformity of the obtained multi-phase composite core-shell material under the premise of 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.

[0007] Another object of the present invention is to propose a device for preparing metallization slurry for packaging substrates, which, when combined with a method for preparing metallization slurry for packaging substrates, is conducive to ensuring the uniformity of the obtained multi-phase composite core-shell material, and further ensuring the performance stability of the metallization slurry.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] A method for preparing a metallization paste for a packaging substrate comprises the following steps:

[0010] S1. preparing a salt solution of metal A ions and a solution containing elemental metal B particles, wherein the reducing property of the metal B is greater than that of the metal A;

[0011] S2. The salt solution of metal A ions and the solution containing single-substance metal B particles are introduced into the reaction container at the same time, and negative pressure is applied to the reaction container simultaneously, so that the salt solution of metal A ions and the solution containing single-substance metal B particles form a turbulent state in the reaction container, and a replacement reaction is carried out, so that the outer atoms of the single-substance metal B particles are replaced by single-substance nanometal A, forming a multi-phase composite core-shell material, and obtaining a metallization slurry for packaging substrates.

[0012] Further, step S2 is specifically as follows: simultaneously introducing gas, a salt solution of metal A ions and a solution containing single-substance metal B particles into a reaction container, and simultaneously applying negative pressure to the reaction container, so that the gas, the salt solution of metal A ions and the solution containing single-substance metal B particles all form a turbulent state in the reaction container, and the salt solution of metal A ions and the solution containing single-substance metal B particles undergo a replacement reaction, so that the outer atoms of the single-substance metal B particles are replaced by single-substance nanometal A, forming a multiphase composite core-shell material, and obtaining a metallization slurry for a packaging substrate;

[0013] The gas is any one of an inert gas and a reducing gas.

[0014] Furthermore, step S2 is specifically as follows: introducing gas, a salt solution of metal A ions and a solution containing elemental metal B particles into the reaction container in step S2, and simultaneously applying negative pressure to the reaction container, 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, and the salt solution of metal A ions and the solution containing elemental metal B particles undergo a replacement reaction under heating and / or ultrasonic conditions, so that the outer atoms of the elemental metal B particles are replaced by elemental nanometal A, forming a multiphase composite core-shell material, and obtaining a metallization slurry for packaging substrates.

[0015] Further, in step S2, the inert gas is any one or more of nitrogen, carbon dioxide, argon and helium;

[0016] The reducing gas is any one of hydrogen gas and carbon monoxide gas.

[0017] Furthermore, in step S2, the mixing ratio of the salt solution of the metal A ions and the solution containing the elemental metal B particles is (0.1-10):1, calculated by volume ratio.

[0018] Further, in step S1, the metal A includes any one of copper, zinc, nickel and silver;

[0019] The metal B includes any one of aluminum, magnesium, copper, zinc, nickel and silver.

[0020] A preparation device for metallization slurry for packaging substrate, used to implement the above-mentioned preparation method for metallization slurry for packaging substrate, comprising a storage container 1, an air inlet pipe, a first discharge pipe, a reaction container, an air pump and a collection container, wherein the storage container, the first discharge pipe, the reaction container and the collection container are interconnected from top to bottom; the outlet of the collection container is interconnected with the inlet of the air pump, and the collection container and the air pump are arranged in parallel;

[0021] The air inlet pipe is located above the reaction container, the end of the air inlet pipe and the end of the first discharge pipe are located at the same horizontal plane, and the outlet of the air inlet pipe is connected to the outlet of the first discharge pipe and the inlet of the reaction container, and the air inlet pipe is used to transport the inert gas or the reducing gas to the reaction container;

[0022] The air intake pipe is provided with a second valve for opening and closing the air intake pipe;

[0023] The first discharge pipe is provided with a first valve for opening and closing the first discharge pipe;

[0024] The material storage container, the first valve and the first discharge pipe form a set of discharge components. There are at least two sets of discharge components, and the two sets of discharge components are respectively located on the left and right sides of the air inlet pipe.

[0025] Furthermore, the reaction container includes a reaction tube and a water bath ultrasonic pot, the reaction tube is located inside the water bath ultrasonic pot, 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, and the outlet of the reaction tube is interconnected with the inlet of the collection container; the water bath ultrasonic pot is used to heat and / or ultrasonicate the reaction tube.

[0026] Furthermore, the reaction tube comprises a feed section, a reaction section and a discharge section which are sequentially connected from top to bottom, the feed section and the discharge section are both vertically arranged, the shapes of the feed section and the discharge section are both linear, the shape of the reaction section is spiral, and the spiral axis of the reaction section extends horizontally.

[0027] 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;

[0028] The feed pipe is provided with a third valve for opening and closing the feed pipe;

[0029] The discharge port, the feed pipe, the third valve and the collection container form a group of collection components, and the number of the collection components is multiple, and the multiple groups of the collection components are arranged in parallel, and the outlet of the collection container of the collection component located at the end of the second discharge pipe is connected to the inlet of the vacuum pump;

[0030] There are multiple communicating tubes, and the collecting containers of two adjacent collecting assemblies are connected to each other through a communicating tube;

[0031] The connecting pipe is provided with a fourth valve for opening and closing the connecting pipe.

[0032] The technical solution provided by the present invention may include the following beneficial effects:

[0033] 1. In the technical solution, the metal type in the salt solution of metal A ions is metal A, and the metal type in the solution containing elemental metal B particles is metal B, and the reducing property of metal B is greater than that of metal A, so that when the above two solutions are mixed, elemental metal B can spontaneously replace the metal A ions in the salt solution of metal A ions, and in the process of the replacement reaction, the outer atoms of the elemental metal B particles are replaced by elemental nanometal A, forming a core-shell structure of elemental nanometal A encapsulating elemental metal B particles (i.e., a multiphase composite core-shell material).

[0034] 2. The salt solution of metal A ions and the solution containing elemental metal B particles are introduced into the reaction vessel 5 at the same time, and negative pressure is applied to the reaction vessel 5 simultaneously, so that the salt solution of metal A ions and the solution containing elemental metal B particles form a turbulent state in the reaction vessel 5, and a turbulent environment is constructed. In this turbulent environment, the salt solution of metal A ions and the solution containing elemental metal B particles move irregularly in the reaction vessel 5 and mix with each other, ensuring that the two solutions undergo a replacement reaction in a fully and evenly mixed state, greatly improving the uniformity of the replacement reaction, and effectively avoiding the problem of uneven reaction caused by local concentration differences, thereby ensuring the consistency of the shape and size of the obtained multiphase composite core-shell material, with extremely high uniformity. At the same time, this turbulent environment can promote the salt solution of metal A ions and the solution containing elemental metal B particles to fully react in the reaction vessel 5, effectively avoiding the inconsistency in shape and size of the multiphase composite core-shell material caused by incomplete reaction, which is also conducive to ensuring the uniformity of the multiphase composite core-shell material. In addition, the constructed turbulent environment can effectively avoid the agglomeration of the obtained multi-phase composite core-shell material, which is also conducive to ensuring the uniformity of the multi-phase composite core-shell material. That is, the technical solution ensures the uniformity of the multi-phase 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. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 It is a structural schematic diagram of a device for preparing metallization paste for a packaging substrate of the present invention.

[0036] Among them: a storage container 1, a first valve 2, an air inlet pipe 3, a first discharge pipe 4, a reaction container 5, a reaction tube 51, a water bath ultrasonic pot 52, an air pump 6, a collection container 7, a second discharge pipe 8, a feed pipe 9, and a connecting pipe 10. DETAILED DESCRIPTION

[0037] Embodiments of the present invention are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and cannot be understood as limiting the present invention.

[0038] The present technical solution provides a method for preparing a metallization paste for a packaging substrate, comprising the following steps:

[0039] S1. Preparing a salt solution of metal A ions and a solution containing elemental metal B particles, wherein the reducing property of the metal B is greater than that of the metal A;

[0040] S2. The salt solution of metal A ions and the solution containing elemental metal B particles are introduced into the reaction container 5 at the same time, and negative pressure is applied to the reaction container 5 simultaneously, so that the salt solution of metal A ions and the solution containing elemental metal B particles form a turbulent state in the reaction container 5, and a replacement reaction is carried out, so that the outer atoms of the elemental metal B particles are replaced by elemental nanometal A, forming a multiphase composite core-shell material, and obtaining a metallization slurry for packaging substrates.

[0041] In order to solve the defect that the multi-phase composite core-shell material obtained in the prior art has poor uniformity, thereby affecting the performance stability of the metallization slurry, the present technical scheme proposes a method for preparing a metallization slurry for a packaging substrate, including 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 a replacement reaction). By optimizing the preparation process, optimizing the types of raw materials and constructing a turbulent environment, it is beneficial to simplify the preparation method, improve production efficiency and facilitate industrial production, thereby ensuring the uniformity of the obtained multi-phase composite core-shell material and further ensuring the performance stability of the metallization slurry to meet actual usage requirements.

[0042] Specifically, in the technical scheme, the metal type in the salt solution of metal A ions is metal A, and the metal type in the solution containing elemental metal B particles is metal B, and the reducibility of metal B is greater than that of metal A, so that when the above two solutions are mixed, elemental metal B can spontaneously replace the metal A ions in the salt solution of metal A ions, and in the process of the replacement reaction, the outer atoms of the elemental metal B particles are replaced by elemental nanometal A, forming a core-shell structure of elemental nanometal A encapsulating elemental metal B particles (i.e., a multiphase composite core-shell material).

[0043] More specifically, this solution simultaneously introduces a salt solution of metal A ions and a solution containing elemental metal B particles into the reaction vessel 5, and simultaneously applies negative pressure to the reaction vessel 5, so that the salt solution of metal A ions and the solution containing elemental metal B particles both form a turbulent state in the reaction vessel 5, thereby constructing a turbulent environment. In this turbulent environment, the salt solution of metal A ions and the solution containing elemental metal B particles move irregularly in the reaction vessel 5 and mix with each other, ensuring that the two solutions undergo a replacement reaction in a fully and evenly mixed state, greatly improving the uniformity of the replacement reaction, and effectively avoiding the problem of uneven reaction caused by local concentration differences, thereby ensuring the consistency of the shape and size of the obtained multiphase composite core-shell material, which has extremely high uniformity. At the same time, this turbulent environment can promote the salt solution of metal A ions and the solution containing elemental metal B particles to fully react in the reaction vessel 5, effectively avoiding the inconsistency in shape and size of the multiphase composite core-shell material caused by incomplete reaction, which is also conducive to ensuring the uniformity of the multiphase composite core-shell material. In addition, the constructed turbulent environment can effectively avoid the agglomeration of the obtained multi-phase composite core-shell material, which is also conducive to ensuring the uniformity of the multi-phase composite core-shell material. That is, the technical solution ensures the uniformity of the multi-phase 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.

[0044] Furthermore, the preparation method of the technical solution is simple, and the constructed turbulent environment is not only conducive to accelerating the mass transfer process of the reactants and promoting the mixing between the reactants, but also conducive to increasing the probability of collision and reaction of the reactant molecules per unit time, thereby increasing the reaction rate. The above-mentioned synergistic effect not only greatly improves the production efficiency, but also lays a solid foundation for the realization of industrialized production.

[0045] Preferably, in step S1, the particle size of the single substance B particles is 20 to 80 nm.

[0046] By limiting the particle size of the single metal B particles, it can be ensured that the multiphase composite core-shell material generated during the reaction has a relatively uniform particle size distribution, which is conducive to reducing the particle size difference of the multiphase composite core-shell material and improving the uniformity of the multiphase composite core-shell material. In addition, when the particle size of the single metal B particles is in the range of 20 to 80 nm, its specific surface area is large, the number of surface atoms is large, and the number of reactive sites increases, which is conducive to increasing the replacement reaction rate between it and the metal A ions in the salt solution of the metal A ions, thereby improving production efficiency and being more conducive to industrial production.

[0047] Further explanation, step S2 specifically includes: simultaneously introducing gas, a salt solution of metal A ions, and a solution containing single-substance metal B particles into the reaction container 5, 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 single-substance 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 single-substance metal B particles undergo a replacement reaction, so that the outer atoms of the single-substance metal B particles are replaced by single-substance nanometal A, forming a multiphase composite core-shell material, and obtaining a metallization slurry for a packaging substrate;

[0048] The gas is any one of an inert gas and a reducing gas.

[0049] By simultaneously introducing gas, a salt solution of metal A ions, and a solution containing elemental metal B particles into the reaction vessel 5, a turbulent state of gas-liquid mixing is constructed in the container 5. The gas in the turbulent state can also promote the mixing uniformity and completeness of the salt solution of metal A ions and the solution containing elemental metal B particles, further ensuring the uniformity of the multiphase composite core-shell material. In addition, the turbulent state makes the gas evenly distributed in the reaction vessel, ensuring that the temperature and pressure environment in the reaction vessel 5 are more uniform, which is conducive to reducing the occurrence of local overheating or supercooling, improving the stability and controllability of the reaction, and also helping to ensure the uniformity of the multiphase composite core-shell material. That is, the technical solution introduces gas and makes the gas in a turbulent environment, making full use of its multiple advantages, and is also conducive to further ensuring the uniformity of the multiphase composite core-shell material, thereby ensuring the performance stability of the metallization slurry for the packaging substrate.

[0050] In addition, when the gas is an inert gas and a reducing gas, it can also avoid the oxidation reaction that may occur during the replacement reaction, which is beneficial to ensure the purity of the reaction and the uniformity of the multi-phase composite core-shell material. In addition, when the gas is a reducing gas, it can promote the reduction of metal A ions in the salt solution of metal A ions to single-substance nano-metal A and deposit them on the surface of single-substance metal B particles, which is also beneficial to obtain a multi-phase composite core-shell material.

[0051] Preferably, step S2 specifically comprises: introducing gas, a salt solution of metal A ions and a solution containing single-substance 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 single-substance 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 single-substance metal B particles undergo a replacement reaction, so that the outer atoms of the single-substance metal B particles are replaced by single-substance nanometal A, to form a multiphase composite core-shell material dispersion;

[0052] Separating the multiphase composite core-shell material dispersion to obtain the multiphase composite core-shell material;

[0053] The multiphase composite core-shell material is mixed with a solvent and a soldering flux to obtain a metallization paste for a packaging substrate.

[0054] Further optimization of the preparation method of the metallization paste for the packaging substrate is helpful to prepare and add corresponding solvents and flux according to actual needs, thereby improving the adaptability of the product.

[0055] It should be noted that the solvent may be ethanol, propanol, etc., and the specific type is not limited here.

[0056] The soldering flux may be zinc chloride, ammonium chloride, activated rosin soldering flux, etc., and the specific type is not limited here.

[0057] To further explain, step S2 specifically includes: introducing gas, salt solution of metal A ions and 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, salt solution of metal A ions and 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 replacement reaction under heating and / or ultrasonic conditions, so that the outer atoms of the elemental metal B particles are replaced by elemental nanometal A, forming a multiphase composite core-shell material, and obtaining a metallization slurry for packaging substrates.

[0058] When the replacement reaction is carried out under heating conditions, it can be ensured that the replacement reaction is carried out at the optimal temperature, thereby improving the quality and yield of the multiphase composite core-shell material. When the replacement reaction is carried out under ultrasonic conditions, the cavitation effect and microjet generated by the ultrasonic wave can enhance the mixing effect between the salt solution of metal A ions and the solution containing elemental metal B particles, promote the replacement reaction between the two solutions, and help improve production efficiency.

[0059] Further, in step S2, the inert gas is any one or more of nitrogen, carbon dioxide, argon and helium;

[0060] The reducing gas is any one of hydrogen gas and carbon monoxide gas.

[0061] The types of inert gas and reducing gas are optimized, and the preferred inert gas and reducing gas have a high cost-effectiveness, which is not only conducive to selecting suitable raw materials according to actual needs and improving the flexibility of the formula, but also conducive to saving production costs while ensuring the performance of the metallization slurry for the packaging substrate.

[0062] It should be noted that once the carbon dioxide bubbles encounter the pore surface of the porous material in the dissolved state, they will be more easily broken and dispersed, so that the carbon dioxide bubbles can be precipitated from the solution more efficiently. Therefore, in the present technical solution, when carbon dioxide is selected as the inert gas, the reaction vessel 5 needs to be configured with a porous material to separate the carbon dioxide bubbles from the solution more quickly, thereby facilitating the mixing uniformity of the reaction solution and creating more favorable conditions for the replacement reaction.

[0063] Further, in step S2, the mixing ratio of the salt solution of the metal A ions and the solution containing the elemental metal B particles is (0.1-10):1, calculated by volume ratio.

[0064] This technical solution optimizes the mixing ratio of the salt solution of metal A ions and the solution containing elemental metal B particles, which is not only conducive to more effective replacement reaction between the metal A ions in the salt solution of metal A ions and the elemental metal B in the solution containing elemental metal B particles, ensuring the uniformity of the multi-phase composite core-shell material, but also can reduce the residual unreacted metal A ions and improve the purity of the multi-phase composite core-shell material. In addition, by optimizing the mixing ratio of the salt solution of metal A ions and the solution containing elemental metal B particles, it is conducive to preparing multi-phase composite core-shell materials with different core-shell ratios to meet the needs of different application fields.

[0065] Further, in step S1, the metal A includes any one of copper, zinc, nickel and silver;

[0066] The metal B includes any one of aluminum, magnesium, copper, zinc, nickel and silver.

[0067] By optimizing the types of metal A and metal B, metallization paste for packaging substrates with different physical and chemical properties can be prepared to meet diverse application requirements.

[0068] A device for preparing metallization slurry for packaging substrate, used for realizing the above-mentioned method for preparing metallization slurry for packaging substrate, comprising a storage container 1, an air inlet pipe 3, a first discharge pipe 4, a reaction container 5, an air pump 6 and a collection container 7, wherein the storage container 1, the first discharge pipe 4, the reaction container 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 air pump 6, and the collection container 7 and the air pump 6 are arranged in parallel;

[0069] The air inlet pipe 3 is located above the reaction container 5, the end of the air inlet pipe 3 and the end of the first discharge pipe 4 are located at the same horizontal plane, and the outlet of the air inlet pipe 3 is connected to the outlet of the first discharge pipe 4 and the inlet of the reaction container 5, and the air inlet pipe 3 is used to transport the inert gas or the reducing gas to the reaction container 5;

[0070] The air intake pipe 3 is provided with a second valve for opening and closing the air intake pipe 3;

[0071] The first discharge pipe 4 is provided with a first valve 2 for opening and closing the first discharge pipe 4;

[0072] The material storage container 1 , the first valve 2 and the first discharge pipe 4 form a set of discharge components. There are at least two sets of the discharge components, and the two sets of the discharge components are respectively located on the left and right sides of the air inlet pipe 3 .

[0073] This scheme also proposes a device for preparing metallization slurry for packaging substrates, which, when combined with a method for preparing metallization slurry for packaging substrates, is conducive to ensuring the uniformity of the obtained multi-phase composite core-shell material, and further ensuring the performance stability of the metallization slurry.

[0074] Specifically, Figure 1 As shown, the preparation device of the present scheme includes a storage container 1, an air inlet pipe 3, a first discharge pipe 4, a reaction container 5, an air pump 6 and a collecting container 7, and the storage container 1, the first discharge pipe 4, the reaction container 5 and the collecting container 7 are interconnected from top to bottom; the outlet of the collecting container 7 is interconnected with the inlet of the air pump 6, and the collecting container 7 and the air pump 6 are arranged in parallel; the first discharge pipe 4 is provided with a first valve 2 for opening and closing the first discharge pipe 4; the outlet of the air inlet pipe 3 is interconnected with the outlet of the first discharge pipe 4 and the inlet of the reaction container 5, and the air inlet pipe 3 is used to transport the inert gas to the reaction container 5; a storage container 1, a first valve 2 and a first discharge pipe 4 are a group of discharge components, and at least two groups of discharge components are provided, and the two groups of discharge components are respectively located on the left and right sides of the air inlet pipe 3.

[0075] The working process of the device 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 discharging components. The first valve 2 and the second valve of the two groups of discharging components are opened synchronously, so that the air inlet pipe 3 conveys inert gas or reducing gas to the reaction container 5, and the salt solution of metal A ions and the solution containing elemental metal B particles flow into the reaction container 5. In this process, the vacuum pump 6 is started to form a turbulent state in the reaction container 5 for the gas, the salt solution of metal A ions and the solution containing elemental metal B particles. In this turbulent environment, the salt solution of metal A ions and the solution containing elemental metal B particles move irregularly in the reaction container 5 and mix with each other, so that the salt solution of metal A ions and the solution containing elemental metal B particles are fully and evenly mixed, and a replacement reaction occurs to obtain a multi-phase composite core-shell material with high uniformity, and then obtain a metallization slurry for packaging substrates.

[0076] Further description, the reaction container 5 includes a reaction tube 51 and a water bath ultrasonic pot 52, the reaction tube 51 is located inside the water bath ultrasonic pot 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, and the outlet of the reaction tube 51 is interconnected with the inlet of the collecting container 7; the water bath ultrasonic pot 52 is used to heat and / or ultrasonicate the reaction tube 51.

[0077] By setting the reaction vessel 5 to include a reaction tube 51 and a water bath ultrasonic pot 52, the water bath ultrasonic pot 52 can provide a uniform and controllable heating environment for the reaction tube 51, ensuring that the replacement reaction is carried out at an optimal temperature, thereby improving the quality and yield of the multiphase composite core-shell material. In addition, the water bath ultrasonic pot 52 can not only provide a heating function, but also ultrasonically treat the salt solution of the metal A ions and the solution containing the elemental metal B particles in the reaction tube 51. The cavitation effect and microjet generated by the ultrasonic wave can enhance the mixing effect between the two solutions, promote the replacement reaction between the two solutions, and help improve production efficiency. In addition, ultrasound can also destroy the agglomerates in the solution, making the multiphase composite core-shell material more dispersed and uniform, which is conducive to improving the uniformity of the multiphase composite core-shell material.

[0078] Further description, the reaction tube 51 includes a feed section, a reaction section and a discharge section which are sequentially connected from top to bottom, the feed section and the discharge section are both vertically arranged, the shapes of the feed section and the discharge section are both linear, the shape of the reaction section is spiral, and the spiral axis of the reaction section extends horizontally.

[0079] The reaction section adopts a spiral design, so that the salt solution of metal A ions and the solution containing elemental metal B particles will generate rotation and shear force when flowing through the reaction section, thereby enhancing the mixing effect between the two solutions, improving the efficiency and uniformity of the replacement reaction, thereby helping to improve the uniformity of the multiphase composite core-shell material. In addition, the spiral reaction section can extend the residence time of the salt solution of metal A ions and the solution containing elemental metal B particles in the reaction tube 51, improve the completeness of the reaction, and also help to improve the uniformity of the multiphase composite core-shell material. In addition, the horizontal setting of the reaction section is conducive to saving floor space and improving the compactness of the preparation device.

[0080] Further description, 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;

[0081] The feed pipe 9 is provided with a third valve for opening and closing the feed pipe 9;

[0082] The discharge port, the feed pipe 9, the third valve and the collection container 7 form a collection component. The number of the collection components is multiple, and the multiple collection components are arranged in parallel. The outlet of the collection container 7 of the collection component located at the end of the second discharge pipe 8 is connected to the inlet of the vacuum pump 6.

[0083] There are multiple communicating tubes 10, and the collecting containers 7 of two adjacent collecting assemblies are connected to each other through a communicating tube 10;

[0084] The connecting pipe 10 is provided with a fourth valve for opening and closing the connecting pipe 10 .

[0085] By setting up multiple collecting components, not only can the metallization slurry for the package substrate be collected synchronously by the collecting containers 7 of the multiple collecting components, thereby significantly improving the collection efficiency, but it is also conducive to making the metallization slurry for the package substrate more evenly distributed in the collecting containers 7 of the multiple collecting components, thereby reducing the accumulation and aggregation of the metallization slurry for the package substrate in the collecting container 7 of a single collecting component. In addition, each collecting component is equipped with a third valve, so that the operator can flexibly adjust the collection process as needed, thereby improving the flexibility of the device.

[0086] By providing the connecting pipe 10, the operator can flexibly adjust the distribution of the products in each collection container 7 as needed. For example, when a collection container 7 is about to overflow, part of the product can be transferred to an adjacent collection container 7 by opening the corresponding fourth valve, thereby avoiding overflow and waste of the metallization slurry for the packaging substrate and improving the flexibility of the device.

[0087] The technical solution of the present invention is further illustrated below through specific implementation methods.

[0088] Example 1

[0089] S1. Prepare a silver ammonia solution and a solution containing nano-copper; wherein the particle size of the nano-copper is 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; calculated by volume ratio, the mixing ratio of the silver ammonia solution and the solution containing nano-copper is 0.1:1;

[0090] S2. Nitrogen, silver ammonia solution and solution containing nano-copper are introduced into the reaction container 5 at the same time, and negative pressure is applied to the reaction container 5 simultaneously, so that the nitrogen, silver ammonia solution and solution containing nano-copper form turbulent state in the reaction container 5, and the silver ammonia solution and solution containing nano-copper undergo replacement reaction under heating condition of 80°C, so that the outer atoms of nano-copper are replaced by nano-silver, forming a multi-phase composite core-shell material, and obtaining metallization slurry for packaging substrate.

[0091] The shape and size of the multiphase composite core-shell material in the multiphase composite core-shell material 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 consistent, that is, the multiphase composite core-shell material in Example 1 had high uniformity.

[0092] In addition, under the same other conditions, the metallization slurry for packaging substrate obtained in Example 1 was coated on five substrates, and the surfaces of the five substrates coated with the metallization slurry for packaging substrate were covered with interconnection chips, and five interconnection devices were obtained after sintering. The shear strength of the five interconnection devices was tested using an IC packaging welding strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnection devices was tested using an ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnection devices are basically the same, proving that the metallization slurry for packaging substrate obtained in Example 1 has high performance stability.

[0093] Example 2

[0094] S1. Prepare a copper sulfate solution and a solution containing nano zinc; wherein the particle size of the nano zinc is 40 nm; the concentration of copper ions in the copper sulfate solution is 0.02 mol / L; the concentration of nano zinc in the solution containing nano zinc is 1 mol / L; and the mixing ratio of the copper sulfate solution and the solution containing nano zinc is 0.1:1 according to the volume ratio;

[0095] S2. Hydrogen, copper sulfate solution and solution containing nano zinc are introduced into the reaction container 5 at the same time, and negative pressure is applied to the reaction container 5 simultaneously, so that the hydrogen, copper sulfate solution and solution containing nano zinc form turbulent state in the reaction container 5, and the copper sulfate solution and solution containing nano zinc undergo replacement reaction under ultrasonic conditions, so that the outer atoms of nano zinc are replaced by nano copper, forming a multiphase composite core-shell material, and obtaining a metallization slurry for packaging substrate.

[0096] The shape and size of the multiphase composite core-shell material in the multiphase composite core-shell material 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 consistent, that is, the multiphase composite core-shell material in Example 2 had high uniformity.

[0097] In addition, under the same other conditions, the metallization slurry for packaging substrate obtained in Example 2 was coated on five substrates, and the surfaces of the five substrates coated with the metallization slurry for packaging substrate were covered with interconnection chips, and five interconnection devices were obtained after sintering. The shear strength of the five interconnection devices was tested using an IC packaging welding strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnection devices was tested using an ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnection devices are basically the same, proving that the metallization slurry for packaging substrate obtained in Example 2 has high performance stability.

[0098] Example 3

[0099] Step S1. Prepare a silver nitrate solution and a solution containing nano-nickel; wherein the particle size of the nano-nickel is 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; calculated by volume ratio, the mixing ratio of the silver nitrate solution and the solution containing nano-nickel is 2:1;

[0100] S2. Argon gas, silver nitrate solution and solution containing nano-nickel are introduced into the reaction container 5 at the same time, and negative pressure is applied to the reaction container 5 simultaneously, so that the argon gas, silver nitrate solution and solution containing nano-nickel form a turbulent state in the reaction container 5, and the acid silver solution and solution containing nano-nickel undergo a replacement reaction under heating conditions at a temperature of 100° C., so that the outer atoms of nano-nickel are replaced by nano-silver, forming a multi-phase composite core-shell material, and obtaining a metallization slurry for packaging substrates.

[0101] The shape and size of the multiphase composite core-shell material in the multiphase composite core-shell material 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 consistent, that is, the multiphase composite core-shell material in Example 3 had high uniformity.

[0102] In addition, under the same other conditions, the metallization slurry for packaging substrate obtained in Example 3 was coated on five substrates, and the surfaces of the five substrates coated with the metallization slurry for packaging substrate were covered with interconnection chips, and five interconnection devices were obtained after sintering. The shear strength of the five interconnection devices was tested using an IC packaging welding strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnection devices was tested using an ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnection devices are basically the same, proving that the metallization slurry for packaging substrate obtained in Example 3 has high performance stability.

[0103] Comparative Example 1

[0104] 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.

[0105] The shape and size of the multiphase composite core-shell material in the multiphase composite core-shell material dispersion obtained in Comparative Example 1 were observed by electron microscopy. The results showed that the shape and size consistency of the multiphase composite core-shell material obtained in Comparative Example 1 were poor, that is, the uniformity of the multiphase composite core-shell material in Comparative Example 1 was poor.

[0106] In addition, under the same other conditions, the metallization slurry for packaging substrate obtained in Comparative Example 1 was coated on five substrates, and the surfaces of the five substrates coated with the metallization slurry for packaging substrate were covered with interconnection chips, and five interconnection devices were obtained after sintering. The shear strength of the five interconnection devices was tested using an IC packaging welding strength tester (SERIES-4000-DONDESTER); the surface resistivity of the five interconnection devices was tested using a ST-2258C four-probe tester. The results show that the shear strength and resistivity of the five interconnection devices fluctuate greatly, proving that the performance stability of the metallization slurry for packaging substrate obtained in Comparative Example 1 is poor.

[0107] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0108] Unless otherwise specifically stated, the relative arrangement of the parts and steps described in these embodiments, numerical expressions and numerical values ​​do not limit the scope of the present invention. At the same time, it should be understood that, for ease of description, the sizes of the various parts shown in the accompanying drawings are not drawn according to the actual proportional relationship. The technology, method and equipment known to ordinary technicians in the relevant field may not be discussed in detail, but in appropriate cases, the technology, method and equipment should be regarded as a part of the authorization specification. In all examples shown and discussed here, any specific value should be interpreted as being merely exemplary, rather than as a limitation. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters represent similar items in the following drawings, so once a certain item is defined in an accompanying drawing, it does not need to be further discussed in subsequent drawings.

[0109] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the numbers used in this way can be interchanged where appropriate, so that the embodiments of the present application described herein can be implemented in an order other than those illustrated or described herein.

[0110] The technical principle of the present invention is described above in conjunction with specific embodiments. These descriptions are only for explaining the principle of the present invention and cannot be interpreted as limiting the scope of protection of the present invention in any way. Based on the explanations herein, those skilled in the art can associate other specific implementations of the present invention without paying creative labor, and these methods will fall within the scope of protection of the present invention.

Claims

1. A method for preparing a metallization paste for a packaging substrate, characterized in that: The following steps are involved: S1. preparing a salt solution of metal A ions and a solution containing elemental metal B particles, wherein the reducing property of the metal B is greater than that of the metal A; S2. The salt solution of metal A ions and the solution containing single-substance metal B particles are introduced into the reaction container at the same time, and negative pressure is applied to the reaction container simultaneously, so that the salt solution of metal A ions and the solution containing single-substance metal B particles form a turbulent state in the reaction container, and a replacement reaction is carried out, so that the outer atoms of the single-substance metal B particles are replaced by single-substance nanometal A, forming a multi-phase composite core-shell material, and obtaining a metallization slurry for packaging substrates.

2. The method for preparing a metallization paste for a packaging substrate according to claim 1, characterized in that: Step S2 specifically comprises: introducing gas, a salt solution of metal A ions and a solution containing single-substance metal B particles into a reaction container at the same time, and simultaneously applying negative pressure to the reaction container, so that the gas, the salt solution of metal A ions and the solution containing single-substance metal B particles all form a turbulent state in the reaction container, and the salt solution of metal A ions and the solution containing single-substance metal B particles undergo a replacement reaction, so that the outer atoms of the single-substance metal B particles are replaced by single-substance nanometal A, forming a multiphase composite core-shell material, and obtaining a metallization slurry for a packaging substrate; The gas is any one of an inert gas and a reducing gas.

3. The method for preparing a metallization paste for a packaging substrate according to claim 2, characterized in that: Step S2 specifically comprises: introducing gas, a salt solution of metal A ions and a solution containing elemental metal B particles into the reaction container in step S2, and simultaneously applying negative pressure to the reaction container, 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, and the salt solution of metal A ions and the solution containing elemental metal B particles undergo a replacement reaction under heating and / or ultrasonic conditions, so that the outer atoms of the elemental metal B particles are replaced by elemental nanometal A, forming a multiphase composite core-shell material, and obtaining a metallization slurry for packaging substrates.

4. The method for preparing a metallization paste for a packaging substrate according to claim 2, characterized in that: In step S2, the inert gas is any one or more of nitrogen, carbon dioxide, argon and helium; The reducing gas is any one of hydrogen gas and carbon monoxide gas.

5. The method for preparing a metallization paste for a packaging substrate according to claim 1, characterized in that: In step S2, the mixing ratio of the salt solution of the metal A ions and the solution containing the elemental metal B particles is (0.1-10):1, calculated by volume ratio.

6. The method for preparing a metallization paste for a packaging substrate according to claim 1, 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.

7. A device for preparing metallization paste for packaging substrate, characterized in that: A method for preparing a metallization paste for a packaging substrate according to any one of claims 1 to 6, comprising a material storage container 1, an air inlet pipe, a first material outlet pipe, a reaction container, an air pump and a collection container, wherein the material storage container, the first material outlet pipe, the reaction container and the collection container are interconnected from top to bottom; the outlet of the collection container is interconnected with the inlet of the air pump, and the collection container and the air pump are arranged in parallel; The air inlet pipe is located above the reaction container, the end of the air inlet pipe and the end of the first discharge pipe are located at the same horizontal plane, and the outlet of the air inlet pipe is connected to the outlet of the first discharge pipe and the inlet of the reaction container, and the air inlet pipe is used to transport the inert gas or the reducing gas to the reaction container; The air intake pipe is provided with a second valve for opening and closing the air intake pipe; The first discharge pipe is provided with a first valve for opening and closing the first discharge pipe; The material storage container, the first valve and the first discharge pipe form a set of discharge components. There are at least two sets of discharge components, and the two sets of discharge components are respectively located on the left and right sides of the air inlet pipe.

8. The device for preparing metallization paste for packaging substrate according to claim 7, characterized in that: The reaction container comprises a reaction tube and a water bath ultrasonic pot, wherein the reaction tube is located inside the water bath ultrasonic pot, 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, and the outlet of the reaction tube is interconnected with the inlet of the collection container; the water bath ultrasonic pot is used to heat and / or ultrasonicate the reaction tube.

9. The device for preparing metallization paste for packaging substrate according to claim 8, characterized in that: The reaction tube comprises a feed section, a reaction section and a discharge section which are sequentially connected from top to bottom, the feed section and the discharge section are both vertically arranged, the shapes of the feed section and the discharge section are both linear, the shape of the reaction section is spiral, and the spiral axis of the reaction section extends horizontally.

10. The device for preparing metallization paste for packaging substrate according to claim 9, characterized in that: It also includes a second discharge pipe, a feed pipe and a connecting pipe, wherein 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; The feed pipe is provided with a third valve for opening and closing the feed pipe; The discharge port, the feed pipe, the third valve and the collection container form a group of collection components, and the number of the collection components is multiple, and the multiple groups of the collection components are arranged in parallel, and the outlet of the collection container of the collection component located at the end of the second discharge pipe is connected to the inlet of the vacuum pump; There are multiple communicating tubes, and the collecting containers of two adjacent collecting assemblies are connected to each other through a communicating tube; The connecting pipe is provided with a fourth valve for opening and closing the connecting pipe.

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