CN107511602B - nano Ag-Cu soldering paste and preparation method and application thereof - Google Patents
nano Ag-Cu soldering paste and preparation method and application thereof Download PDFInfo
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- CN107511602B CN107511602B CN201710690344.3A CN201710690344A CN107511602B CN 107511602 B CN107511602 B CN 107511602B CN 201710690344 A CN201710690344 A CN 201710690344A CN 107511602 B CN107511602 B CN 107511602B
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
the invention discloses a nano Ag-Cu soldering paste and a preparation method and application thereof. The nano Ag-Cu soldering paste is prepared from Ag powder, Cu powder and glycerol according to the following proportion: the mass ratio of the Ag powder to the Cu powder is 2-4: 1; the mass ratio of the sum of the mass of the Ag powder and the Cu powder to the mass of the glycerol is 8-12: 1. Wherein the grain diameter of the Ag powder is 5-10 nm, and the grain diameter of the Cu powder is 20-60 nm. The preparation method of the nano Ag-Cu soldering paste comprises the following steps: and adding alcohol into the Ag powder and the Cu powder, grinding to obtain Ag-Cu mixed powder, and adding glycerol to prepare a viscous paste to obtain the nano Ag-Cu soldering paste. The nano Ag-Cu soldering paste can be used for preparing a copper-copper connecting piece, and comprises the following specific steps: and taking a proper amount of nano Ag-Cu soldering paste, uniformly coating the nano Ag-Cu soldering paste on the surfaces to be connected of the two copper base materials, closing the surfaces to be connected, and connecting. The nano Ag-Cu soldering paste provided by the invention has the advantages of strong oxidation resistance, good electrochemical migration resistance, high electrical conductivity and thermal conductivity, ideal joint shear strength and high reliability.
Description
Technical Field
the invention belongs to the field of nano connection, and particularly relates to nano Ag-Cu soldering paste and a preparation method and application thereof.
background
high power electronic devices are often accompanied by higher operating temperatures, and in order to meet the requirements of electronic packaging, solders with higher melting points are required. The melting points of the Cu and Ag blocks are 1080 ℃ and 960 ℃ respectively, which are far higher than the requirement of the solder on the melting point (usually about 200 ℃). In addition, both Cu and Ag are good electrical conductors, which also ensures stable transmission of electrical signals in electronic devices. Meanwhile, the cost can be reduced by adding the nano Cu particles. Therefore, the preparation and application of the nano Ag-Cu solder have important significance for the field of high-temperature electronic packaging.
The high melting points of Ag and Cu, however, lead to difficulties in connection because excessively high connection temperatures can damage the substrate and related components. And the solder containing Ag and Cu in the prior art also has the problems of poor electrochemical migration resistance, easy oxidation and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a nano Ag-Cu soldering paste and a preparation method and application thereof. The nano Ag-Cu soldering paste provided by the invention has the advantages of strong oxidation resistance, good electrochemical migration resistance, high electrical conductivity and thermal conductivity, low requirement on connection temperature when used for preparing a joint, ideal joint shear strength and high reliability when connected by the nano Ag-Cu soldering paste.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a nano Ag-Cu soldering paste is characterized by being prepared from Ag powder, Cu powder and glycerol according to a certain proportion.
According to the scheme, preferably, the mass ratio of the Ag powder to the Cu powder is 2-4: 1; the mass ratio of the sum of the mass of the Ag powder and the mass of the Cu powder to the mass of the glycerol is 8-12: 1.
According to the scheme, preferably, the grain size of the Ag powder is 5-10 nm, and the grain size of the Cu powder is 20-60 nm.
According to the scheme, preferably, the preparation method of the Ag powder with the particle size of 5-10 nm uses stearic acid, sodium hydroxide and silver nitrate as raw materials and is prepared by a liquid-phase chemical-thermal decomposition method, and the preparation method comprises the following specific steps:
(1) Dissolving sodium hydroxide and stearic acid in deionized water, heating to 80 ℃, and adding AgNO3stirring at constant temperature for 1h, and centrifuging and cleaning the upper white waxy substance; more preferably, the speed of the centrifugation is 7000r/min, the times of the cleaning are 4 times, and the cleaning time is 10 min;
(2) And (3) under the condition of introducing nitrogen, heating the white waxy substance after centrifugal cleaning in the step (1) to 250 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 90min to obtain nano silver particles with the particle size of 5-10 nm.
According to the scheme, preferably, the preparation method of the Cu powder with the particle size of 20-60 nm is characterized in that sodium hypophosphite and copper sulfate are used as raw materials and are prepared through a liquid-phase chemical reduction method, and the preparation method comprises the following specific steps:
(1) adding sodium hypophosphite and PVPAdding into diethylene glycol solution, heating to 80 deg.C, and adding CuSO4·5H2O, stirring at constant temperature for 1h, and taking purple black precipitate in the reaction solution;
(2) Centrifugally cleaning and drying the purple black precipitate obtained in the step (1) to obtain nano copper particles with the particle size of 20-60 nm; more preferably, the centrifugation rate is 7000r/min, the number of washes is 4, and each wash time is 10 min.
The invention also provides a preparation method of the nano Ag-Cu soldering paste, which is characterized by comprising the following specific steps: and adding a proper amount of alcohol into the Ag powder and the Cu powder, grinding until the alcohol is completely volatilized to obtain uniform Ag-Cu mixed powder, and adding glycerol to prepare a viscous paste to obtain the nano Ag-Cu composite soldering paste.
the invention also provides application of the nano Ag-Cu soldering paste, which is characterized in that the nano Ag-Cu soldering paste is used as a solder for preparing a copper-copper connecting piece.
the invention also provides a copper-copper connecting piece which is characterized by being prepared by adopting the nano Ag-Cu soldering paste for connection. The schematic diagram of the invention for connecting copper by adopting the nano Ag-Cu soldering paste is shown in figure 1.
According to the scheme, preferably, the surfaces of the copper and the copper are plated with a Ni layer and an Ag layer, namely, the two base materials of the connecting piece of the copper and the copper are plated with Ni/Ag copper.
The invention also provides a preparation method of the copper and copper connecting piece, which is characterized by comprising the following steps:
Taking a proper amount of nano Ag-Cu soldering paste, uniformly coating the nano Ag-Cu soldering paste on the surfaces to be connected of the two copper base metals, butting the surfaces to be connected of the two copper base metals, and connecting under a certain pressure.
according to the scheme, preferably, the surfaces to be connected of the two copper base metals are both cleaned and dried. More preferably, the cleaning is ultrasonic cleaning with alcohol for at least 30 min.
According to the scheme, preferably, the pressure is 3-5 MPa.
According to the scheme, the connection temperature is preferably 280-350 ℃, and the time for keeping the temperature is 30-40 min.
According to the above scheme, more preferably, the method further comprises the following steps before the temperature of the connection is reached: keeping the temperature at 200-250 ℃ for 20-30 min.
The basic principle of the invention is as follows:
The invention mainly prepares the nano Ag-Cu soldering paste by adding nano Cu particles into the nano Ag solder, so that the prepared soldering paste has the excellent performances of nano Ag and Cu. When the size of the particles reaches the nanometer scale, the particles have high surface energy, which leads to a great reduction in melting point and sintering temperature. By utilizing the size effect of the nano Ag and the Cu, the solder can complete the mission of low-temperature packaging and high-temperature service. By utilizing the excellent electrochemical migration resistance of Cu and the good oxidation resistance of Ag, the nano Ag-Cu soldering paste has excellent characteristics which are not possessed by the conventional solder. These excellent characteristics can make the nano Ag-Cu solder paste better applied to the field of microelectronic packaging.
Compared with the prior art, the invention has the beneficial effects that:
(1) The nano Ag-Cu soldering paste provided by the invention has the excellent performances of Ag and Cu.
(2) the preparation method of the nano Ag-Cu soldering paste provided by the invention is simple, convenient to use, safe and reliable.
(3) The nano Ag-Cu soldering paste provided by the invention is relatively low in production cost, has excellent oxidation resistance, has good electrochemical mobility resistance and excellent electrical conductivity and thermal conductivity, and can be directly used as a solder in the field of electronic packaging. (4) The nano Ag-Cu soldering paste obtained by the invention is used for connecting copper base materials, the requirement on the connection temperature is low and is only 280-350 ℃, the joint interface layer of the obtained connecting piece is well combined, no defects such as cracks and pores are observed, and the shear strength is more than 20 MPa.
drawings
FIG. 1 is a schematic diagram of the present invention using nano Ag-Cu solder paste to connect copper.
FIG. 2 is an SEM photograph of the nano-Ag particles with a particle size of 5-10 nm prepared in example 1.
FIG. 3 is an SEM image of the Cu nanoparticles with a particle size of 20-60 nm prepared in example 1.
FIG. 4 is an XRD pattern of the nano Ag-Cu mixed powder prepared in example 1.
Fig. 5 is a micro-topography of the interface region of the copper/copper joint using the nano Ag-Cu paste prepared in application example 1.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
the preparation method of the nano Ag-Cu soldering paste comprises the following specific steps:
1. preparing Ag powder (nano silver particles with the particle size of 5-10 nm):
First, 0.6g sodium hydroxide and 4.65g stearic acid were dissolved in 600mL deionized water, heated to 80 ℃ and 2.5g AgNO added3After stirring for 1h at constant temperature, taking the upper white waxy substance, centrifuging and cleaning at the centrifuging speed of 7000r/min for 4 times (wherein deionized water is used for cleaning for 3 times, and alcohol is used for cleaning for 1 time), and the cleaning time is 10min each time. And then, heating the white waxy substance in a tubular furnace filled with nitrogen, wherein the heating rate of the tubular furnace is 5 ℃/min, and when the temperature is 250 ℃, keeping the temperature for 90min, and finally obtaining the nano silver particles with the particle size of 5-10 nm. Fig. 2 is an SEM image of the nano silver particles prepared in this example.
2. Preparing Cu powder (nano copper particles with the particle size of 20-60 nm):
First, 0.7433g of sodium hypophosphite and 0.16g of PVP were added to 60ml of diethylene glycol solution and heated to 80 ℃ and 1.9974g of CuSO were added4·5H20, stirring at constant temperature for 1h, taking purple black precipitate in the reaction solution, centrifuging and cleaning at a centrifugation speed of 7000r/min for 4 times (wherein deionized water is used for cleaning for 3 times, and alcohol is used for cleaning for 1 time), and the cleaning time is 10min each time. And then drying the purple black precipitate to obtain the nano copper particles with the particle size of 20-60 nm. Fig. 3 is an SEM image of the nano-copper particles prepared in this example.
3. Preparing nano Ag-Cu soldering paste: mixing the nano Ag powder with the particle size of 5-10 nm and the nano Cu powder with the particle size of 20-60 nm respectively obtained in the steps 1 and 2 according to the mass ratio of 3:1, adding alcohol, grinding until the alcohol is completely volatilized to obtain uniformly mixed nano Ag-Cu mixed powder, adding glycerol with the mass being one tenth of the total mass of the nano Ag-Cu mixed powder, and blending into a viscous paste to obtain the nano Ag-Cu soldering paste.
FIG. 4 is an XRD spectrum of the mixed powder of Ag and Cu nanoparticles obtained in step 3 of this example.
Example 2
The preparation method of the nano Ag-Cu soldering paste comprises the following specific steps:
Steps 1 and 2 are the same as example 1;
Step 3, preparing the nano Ag-Cu soldering paste: mixing the nano Ag powder with the particle size of 5-10 nm and the nano Cu powder with the particle size of 20-60 nm respectively obtained in the steps 1 and 2 according to the mass ratio of 4:1, adding alcohol, grinding until the alcohol is completely volatilized to obtain uniformly mixed nano Ag-Cu powder, adding glycerol with the mass being one eighth of the total mass of the nano Ag-Cu powder, and preparing into a viscous paste to obtain the nano Ag-Cu soldering paste.
Application example 1
The connection plating of Ni/Ag copper by the nano Ag-Cu solder paste prepared in the embodiment 1 comprises the following specific steps:
1. And ultrasonically cleaning the two pieces of Ni/Ag plated copper in alcohol for 30min, and drying for later use.
2. Taking a small amount of the nano Ag-Cu soldering paste prepared in the embodiment 1, uniformly coating the nano Ag-Cu soldering paste on the surface to be connected plated with Ni/Ag copper, and closing the surface to be connected to obtain the Ni/Ag-plated copper/nano Ag-Cu soldering paste/Ni/Ag-plated copper part to be connected.
3. Putting the Ni/Ag-plated copper/nano Ag-Cu soldering paste/Ni/Ag-plated copper to-be-connected piece into a hot press, setting the pressure to be 5MPa, firstly preserving heat at the temperature of 200 ℃ for 20min, then preserving heat at the temperature of 350 ℃ for 30min, and then cooling to room temperature along with the furnace to obtain a final product Ni/Ag-plated copper/nano Ag-Cu soldering paste/Ni/Ag-plated copper joint.
The joint prepared in this example was tested for shear strength on a universal testing machine, and the results show: the average shear strength of the joint exceeds 20 MPa.
Fig. 5 is a microscopic morphology of the joint interface region of the Ni/Ag copper plated/nano Ag-Cu solder paste/Ni/Ag copper plated joint prepared by using the nano Ag-Cu solder paste in the present application embodiment, as can be seen from the figure, the interface bonding between the base material and the connection layer is good, and the solder layer is relatively uniform and dense.
Application example 2
The nano Ag-Cu soldering paste prepared in the embodiment 2 is adopted to connect and plate Ni/Ag copper under different processes, and the specific steps are as follows:
1. And ultrasonically cleaning the two pieces of Ni/Ag plated copper in alcohol for 30min, and drying for later use.
2. Taking a small amount of the nano Ag-Cu soldering paste prepared in the embodiment 2, uniformly coating the nano Ag-Cu soldering paste on the surface to be connected of the Ni/Ag-plated copper base material, and closing the surface to be connected to obtain the Ni/Ag-plated copper/nano Ag-Cu soldering paste/Ni/Ag-plated copper part to be connected.
3. Putting the Ni/Ag-plated copper/nano Ag-Cu soldering paste/Ni/Ag-plated copper to-be-connected piece into a hot press, setting the pressure to be 4MPa, firstly preserving the heat at the temperature of 250 ℃ for 25min, then preserving the heat at the temperature of 320 ℃ for 35min, and then cooling to the room temperature along with the furnace to obtain the final product copper/copper joint.
the obtained joint has uniform and compact connecting layer and good combination with the parent metal.
Claims (8)
1. A nanometer Ag-Cu soldering paste is characterized by being prepared from Ag powder, Cu powder and glycerol according to a certain proportion, wherein the grain diameter of the Ag powder is 5-10 nm, the grain diameter of the Cu powder is 20-60 nm,
The preparation method of the Ag powder with the particle size of 5-10 nm comprises the following steps:
(1) dissolving sodium hydroxide and stearic acid in deionized water, heating to 80 ℃, and adding AgNO3Stirring at constant temperature for 1h, and centrifuging and cleaning the upper white waxy substance;
(2) heating the white waxy substance centrifugally cleaned in the step (1) to 250 ℃ at a heating rate of 5 ℃/min and preserving heat for 90min under the condition of introducing nitrogen to obtain nano silver particles with the particle size of 5-10 nm;
The preparation method of the Cu powder with the particle size of 20-60 nm comprises the following steps:
(1) Adding sodium hypophosphite and PVP into diethylene glycol solution, heating to 80 ℃, and adding CuSO4·5H2o, stirring at constant temperature for 1h, and taking the purple black substances in the reaction solution;
And (2) centrifugally cleaning and drying the purple black substance obtained in the step (1) to finally obtain the nano copper particles with the particle size of 20-60 nm.
2. The nano Ag-Cu solder paste as claimed in claim 1, wherein the mass ratio of Ag powder to Cu powder is 2-4: 1; the mass ratio of the sum of the mass of the Ag powder and the mass of the Cu powder to the mass of the glycerol is 8-12: 1.
3. The preparation method of the nano Ag-Cu soldering paste as claimed in any one of claims 1 to 2, which is characterized by comprising the following steps:
and adding a proper amount of alcohol into the Ag powder and the Cu powder, grinding until the alcohol is completely volatilized to obtain uniform Ag-Cu mixed powder, and adding glycerol to prepare a viscous paste to obtain the nano Ag-Cu composite soldering paste.
4. use of a nano Ag-Cu solder paste according to any one of claims 1 to 2 as a solder for the preparation of copper-to-copper connectors.
5. A copper-to-copper connector, which is manufactured by using the nano Ag-Cu paste according to any one of claims 1 to 2, wherein the surfaces of the copper and the copper are plated with a Ni layer and an Ag layer.
6. the method of making a copper-to-copper interconnect of claim 5, comprising the steps of:
Taking a proper amount of nano Ag-Cu soldering paste, uniformly coating the nano Ag-Cu soldering paste on the surfaces to be connected of the two copper base metals, butting the surfaces to be connected of the two copper base metals, and connecting under a certain pressure.
7. the method for preparing a copper-copper connecting piece according to claim 6, wherein the pressure is 3 to 5 MPa; the temperature of the connection is 280-350 ℃, and the time for keeping the temperature is 30-40 min.
8. The method of making a copper to copper connection according to claim 7, further comprising the steps of, prior to reaching the temperature of said connection: keeping the temperature at 200-250 ℃ for 20-30 min.
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| CN110102934A (en) * | 2019-04-30 | 2019-08-09 | 周轻轩 | A kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material |
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| JP5580562B2 (en) * | 2009-09-09 | 2014-08-27 | 地方独立行政法人 大阪市立工業研究所 | Silver-copper mixed powder and bonding method using the same |
| EP2832472B1 (en) * | 2012-03-30 | 2021-07-28 | Applied Nanoparticle Laboratory Corporation | Composite nanometal paste containing copper filler and bonding method |
| CN102922177B (en) * | 2012-10-25 | 2014-08-13 | 哈尔滨工业大学 | Nano intermetallic compound soldering paste and preparation method thereof |
| CN105127609B (en) * | 2015-10-15 | 2017-03-08 | 哈尔滨工业大学 | Copper/galactic nucleus core-shell nanoparticles low-temperature sintering composite solder paste and preparation method thereof |
| CN106041352B (en) * | 2016-08-17 | 2018-05-01 | 武汉工程大学 | A kind of organic acid silver cladding nano-Ag particles and its preparation method and application |
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| CN109277722A (en) * | 2018-10-06 | 2019-01-29 | 天津大学 | A kind of preparation method for the Ag-Si nano-solder paste improving silver-colored electrochemical migration |
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