CN112658277A - Chemical reaction method for preparing Ag3Method for Sn solder nano additive - Google Patents
Chemical reaction method for preparing Ag3Method for Sn solder nano additive Download PDFInfo
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- CN112658277A CN112658277A CN202011443154.XA CN202011443154A CN112658277A CN 112658277 A CN112658277 A CN 112658277A CN 202011443154 A CN202011443154 A CN 202011443154A CN 112658277 A CN112658277 A CN 112658277A
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 60
- 239000000654 additive Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000000996 additive effect Effects 0.000 title claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 150
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 30
- 238000005406 washing Methods 0.000 claims abstract description 29
- 239000007787 solid Substances 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- PPQJCISYYXZCAE-UHFFFAOYSA-N 1,10-phenanthroline;hydrate Chemical compound O.C1=CN=C2C3=NC=CC=C3C=CC2=C1 PPQJCISYYXZCAE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910017692 Ag3Sn Inorganic materials 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 6
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910052709 silver Inorganic materials 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- -1 silver ions Chemical class 0.000 claims description 6
- 101710134784 Agnoprotein Proteins 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000003466 welding Methods 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 7
- 230000010355 oscillation Effects 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 229910052718 tin Inorganic materials 0.000 description 19
- 239000002105 nanoparticle Substances 0.000 description 16
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 15
- 239000000203 mixture Substances 0.000 description 10
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- 238000005476 soldering Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910020836 Sn-Ag Inorganic materials 0.000 description 3
- 229910020988 Sn—Ag Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910020830 Sn-Bi Inorganic materials 0.000 description 2
- 229910018728 Sn—Bi Inorganic materials 0.000 description 2
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229910020816 Sn Pb Inorganic materials 0.000 description 1
- 229910020922 Sn-Pb Inorganic materials 0.000 description 1
- 229910008783 Sn—Pb Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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Abstract
The invention relates to a chemical reaction method for preparing Ag3A method of Sn solder nano additive belongs to the technical field of welding additive. The invention adds SnCl2·2H2Mixing O with anhydrous ethanol to obtain solution A, and mixing AgNO3Mixing with ammonia water to obtain solution B, adding NaBH4Mixing with absolute ethyl alcohol uniformly to obtain solution C; dissolving 1, 10-phenanthroline monohydrate in absolute ethyl alcohol to form a solution D, and dissolving PVP in absolute ethyl alcohol to form a solution E; uniformly mixing the solution A and the solution B to obtain an A-B mixed solution, and dropwise adding the solution E into the A-B, uniformly stirring the mixed solution, then dropwise adding the solution C, and carrying out oscillation reaction until no bubbles are generated to obtain a seed crystal solution; dropwise adding the solution D into the seed crystal solution for reaction, carrying out solid-liquid separation, and washing the solid to obtain Ag3Sn solder nano additive. The method for preparing the nano-scale solder additive through the chemical reaction can improve the stability of the welding point after welding, improve the welding performance of the lead-free solder and improve the reliability, and has convenient operation and simple process.
Description
Technical Field
The invention relates to a chemical reaction method for preparing Ag3A method of Sn solder nano additive belongs to the technical field of welding additive.
Background
The Sn-Pb solder is widely applied to the electronic industry as a traditional soldering material, is an important soldering material in the electronic packaging technology, can provide physical connection and realize the signal transmission function between electronic components as a connecting material, and the Sn-37Pb can meet the requirements of the development of lead-free solder, but the development of the lead-free solder is limited due to the toxicity and the mechanical defects of the lead-free solder. Lead-free solder is vigorously developed by related research institutions and production units to replace tin-lead solder, so that the industrial layout is optimized. The Sn binary alloy solder with more application and development potential at present mainly comprises Sn-Ag, Sn-Bi, Sn-Ag and the like, and ternary or even polynary solder alloys derived on the basis of the Sn-Ag, and the development of the Sn-Bi binary alloy solder and the lead-free solder at present mainly comprisesThe rare earth elements, the nano-phase and the metal elements are mainly added, and researches show that the addition of the new elements is beneficial to improving the mechanical properties of the tin-based solder alloy, particularly the yield strength and the plasticity, and can influence the melting point, the wettability and the like of the tin-based solder alloy. However, at present, Sn-3.0Ag-0.5Cu lead-free solder contains a large amount of Ag, so that the problem of over-high cost exists in the practical application process; meanwhile, the addition of excessive Ag element can cause a great amount of coarse Ag in welding spots3Sn intermetallic compound (MC), resulting in a decrease in the reliability of the solder joint. Therefore, the application range of low-Ag lead-free solder paste in the electronic manufacturing industry is gradually expanding, but the low-Ag lead-free solder paste has the defects of too high melting point, poor wettability, poor mechanical property of a welding joint and the like. Research shows that the composite soldering paste formed by adding the nano particles into the soldering paste is an effective method for improving the processing performance of the soldering paste and improving the reliability of a welded joint.
Disclosure of Invention
Aiming at the problems that in the prior art, the nano-scale solder additive nanoparticles mainly take pure metal nanoparticles such as Ag, Ni, Mg and the like as solder alloy additives and are widely applied to soldering paste; however, introduction of new elements generates new intermetallic compounds, which may raise the mechanical properties and wettability of the alloy and also cause problems such as increase in melting point and decrease in stability.
The invention provides a chemical reaction method for preparing Ag3The Sn solder nanometer additive is prepared through reduction reaction to prepare simple Ag and Sn matter under the action of PVP, and dispersing and coordinating under the action of 1, 10-phenanthroline to react the simple Ag and Sn matter to produce Ag3Sn, and by controlling the concentration of the reaction solution, a mixture containing different nano-particles can be generated to obtain pure Ag3A Sn nanoparticle compound. Ag3Sn is a stable intermetallic compound in the solder alloy, so that the service life of a welding spot can be better prolonged, and the alloy structure can be refined.
Chemical reaction method for preparing Ag3The method for Sn solder nano additive comprises the following steps:
(1) SnCl2·2H2Mixing O with anhydrous ethanol to obtain solution A, and mixing AgNO3Mixing with ammonia water to obtain solution B, adding NaBH4Mixing with absolute ethyl alcohol uniformly to obtain solution C; dissolving 1, 10-phenanthroline monohydrate in absolute ethyl alcohol to form a solution D, and dissolving PVP in absolute ethyl alcohol to form a solution E;
(2) maintaining the temperature at 20-60 ℃, uniformly mixing the solution A and the solution B to obtain an A-B mixed solution, dropwise adding the solution E into the A-B mixed solution, reacting for 20-30min, dropwise adding the solution C, and oscillating and reacting until no bubbles are generated to obtain a seed crystal solution;
(3) maintaining the temperature at 20-60 deg.C, adding solution D into the seed crystal solution dropwise for reaction for 25-30 hr, separating solid and liquid, washing the solid, and vacuum drying to obtain Ag3Sn solder nano additive.
The molar ratio of the silver ions in the solution B to the stannous ions in the solution A in the step (1) is 2-4:1, and the volumes of the solution A, the solution B, the solution C, the solution D and the solution E are equal.
SnCl in the solution A2·2H2The concentration of O is 0.02-0.03 g/mol, and AgNO is contained in the solution B3The concentration of the NaBH is 0.04-0.06 g/mol, and the NaBH is added into the solution C4The concentration of the compound is 0.1-0.2g/mol, the concentration of the 1, 10-phenanthroline monohydrate in the solution D is 0.06-0.15 g/mol, and the concentration of the PVP in the solution E is 0.087g/mol-0.104 g/mol.
And (3) sequentially using pure water, absolute ethyl alcohol, pure water, acetone and absolute ethyl alcohol as solvents for washing the solid in the step (3), and washing the solid in a centrifugal washing mode, wherein the first washing rotation speed is 1500-1800r/min, the time is 10-12min, the rest rotation speeds are 1000-1200r/min, and the time is 8-10 min.
Further, the dropping speed of the solution E is 0.05-0.1mL/s, the dropping speed of the solution C is 0.05-0.1mL/s, and the dropping speed of the solution D is 0.05-0.1 mL/s.
The invention has the beneficial effects that:
(1) the invention prepares Ag and Sn simple substances by reduction reaction under the action of PVP, and then leads Ag, Sn to be dispersed and coordinated under the action of 1, 10-phenanthroline,Sn simple substance reacts to generate Ag3Sn, and by controlling the concentration of the reaction solution, a mixture containing different nano-particles can be generated to obtain pure Ag3A Sn nanoparticle compound;
(2) the invention controls the concentration of the reaction solution, can obtain tin-based solder additives with different compositions, and when the ratio of the molar weight of the silver ions in the solution B to the molar weight of the stannous ions in the solution A is equal to 3, only Ag exists in the prepared nano additive3Sn nanoparticles;
(3) the method is convenient to operate and simple in process, can obtain the nano-scale additive, and is beneficial to improving the performance of the tin-based solder alloy.
Drawings
FIG. 1 is an SEM image of a tin-based solder nano-additive of example 1;
FIG. 2 is an atomic composition diagram of point 1 in FIG. 1;
FIG. 3 is an SEM image of a tin-based solder nano-additive of example 2;
fig. 4 is an SEM image of the tin-based solder nano-additive of example 3.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: chemical reaction method for preparing Ag3The method for Sn solder nano additive comprises the following steps:
(1) SnCl2·2H2Mixing O with anhydrous ethanol to obtain solution A, and mixing AgNO3Mixing with ammonia water to obtain solution B, adding NaBH4Mixing with absolute ethyl alcohol uniformly to obtain solution C; dissolving 1, 10-phenanthroline monohydrate in absolute ethyl alcohol to form a solution D, and dissolving PVP in absolute ethyl alcohol to form a solution E; wherein SnCl is contained in the solution A2·2H2The concentration of O is 0.028g/mol, and AgNO is contained in the solution B3The concentration of (A) is 0.051g/mol, NaBH in the solution C4The concentration of (a) is 0.15g/mol, and 1, 10-phenanthroline monohydrate in the solution DThe concentration of the silver ion in the solution B is 0.12g/mol, the concentration of PVP in the solution E is 0.09g/mol, and the volumes of the solution A, the solution B, the solution C, the solution D and the solution E are equal, so that the molar ratio of the silver ions in the solution B to the stannous ions in the solution A is less than 3:1, the dropping speed of the solution E is 0.18mL/s, and the dropping speed of the solution C is 0.20 mL/s;
(2) maintaining the temperature at 30 ℃ and stirring, uniformly mixing the solution A and the solution B to obtain an A-B mixed solution, dropwise adding the solution E into the A-B mixed solution to react for 22min, then dropwise adding the solution C, generating a black substance through oscillation reaction, releasing bubbles, releasing heat, and reacting for 50min until no bubbles are generated to obtain a seed crystal solution;
(3) maintaining the temperature at 30 ℃ and stirring, dropwise adding the solution D into the seed crystal solution, and reacting for 24 hours, wherein the dropwise adding speed of the solution D is 0.15 mL/s; solid-liquid separation, washing and vacuum drying the solid to obtain Ag3A Sn solder nano-additive; the solid washing method comprises the following steps of washing solid with solvents of pure water, absolute ethyl alcohol, pure water, acetone and absolute ethyl alcohol in sequence, and performing solid washing in a centrifugal washing mode, wherein the first washing rotation speed is 1600r/min, the time is 10min, the rest rotation speeds are 1200r/min, and the time is 8 min;
example Ag3The Sn solder nano additive is analyzed by an electronic scanner, the SEM picture of the Sn-based solder nano additive is shown in figure 1, the atomic composition picture of point 1 of figure 1 is shown in figure 2,
point 1 atomic composition of FIG. 1
The tin-based solder nano additive contains SnO2Impurities of SnO2And Ag3Ag in Sn nano-particle tin-based solder nano-additive3The mass ratio of the Sn nano particles is 82 percent, and the nano particles of the tin-based solder nano additive are concentrated at 100-200nm according to the particle size distribution.
Example 2: chemical reaction method for preparing Ag3The method for Sn solder nano additive comprises the following steps:
(1) SnCl2·2H2Mixing O with anhydrous ethanol to obtain solution A, and mixing AgNO3Mixing with ammonia water to obtain solution B, adding NaBH4Mixing with absolute ethyl alcohol uniformly to obtain solution C; dissolving 1, 10-phenanthroline monohydrate in absolute ethyl alcohol to form a solution D, and dissolving PVP in absolute ethyl alcohol to form a solution E; wherein SnCl is contained in the solution A2·2H2The concentration of O is 0.022g/mol, and AgNO is contained in the solution B3The concentration of (A) is 0.051g/mol, NaBH in the solution C4Has a concentration of 0.014g/mol, a concentration of 1, 10-phenanthroline monohydrate in the solution D of 0.010g/mol, a concentration of PVP in the solution E of 0.08g/mol, and volumes of the solution A, the solution B, the solution C, the solution D and the solution E are equal, so that a molar ratio of silver ions of the solution B to stannous ions in the solution A is 3: 1; the dropping speed of the solution E is 0.20mL/s, and the dropping speed of the solution C is 0.22 mL/s;
(2) maintaining the temperature at 35 ℃ and stirring, uniformly mixing the solution A and the solution B to obtain an A-B mixed solution, dropwise adding the solution E into the A-B mixed solution to react for 30min, then dropwise adding the solution C, generating a black substance through oscillation reaction, releasing bubbles, releasing heat, and reacting for 40min until no bubbles are generated to obtain a seed crystal solution;
(3) maintaining the temperature at 35 ℃ and stirring, dropwise adding the solution D into the seed crystal solution, and reacting for 30 hours, wherein the dropwise adding speed of the solution D is 0.16 mL/s; solid-liquid separation, washing and vacuum drying the solid to obtain Ag3A Sn solder nano-additive; the solid washing method comprises the following steps of washing solid with solvents of pure water, absolute ethyl alcohol, pure water, acetone and absolute ethyl alcohol in sequence, and washing the solid in a centrifugal washing mode, wherein the first washing rotation speed is 1800r/min, the time is 12min, the rest rotation speeds are 1200r/min, and the time is 10 min;
example Ag3The Sn solder nano additive is analyzed by an electronic scanner, the SEM picture of the Sn-based solder nano additive is shown in figure 2, and the Sn-based solder nano additive contains SnO2Impurities of SnO2And Ag3Sn nanoparticles, Ag in tin-based solder nano-additive3The mass ratio of the Sn nano particles is 98 percent, and the tin-based solder nano can be known from the particle size distributionThe nanoparticles of the rice additive were concentrated at 100-200 nm.
Example 3: chemical reaction method for preparing Ag3The method for Sn solder nano additive comprises the following steps:
(1) SnCl2·2H2Mixing O with anhydrous ethanol to obtain solution A, and mixing AgNO3Mixing with ammonia water to obtain solution B, adding NaBH4Mixing with absolute ethyl alcohol uniformly to obtain solution C; dissolving 1, 10-phenanthroline monohydrate in absolute ethyl alcohol to form a solution D, and dissolving PVP in absolute ethyl alcohol to form a solution E; wherein SnCl is contained in the solution A2·2H2The concentration of O is 0.024g/mol, AgNO is in the solution B3In solution C, the concentration of NaBH is 0.058g/mol4The concentration of (A) is 0.18g/mol, the concentration of 1, 10-phenanthroline monohydrate in the solution D is 0.012g/mol, the concentration of PVP in the solution E is 0.01g/mol, and the volumes of the solution A, the solution B, the solution C, the solution D and the solution E are equal, so that the mole of silver ions in the solution B and stannous ions in the solution A is more than 3: 1; the dropping speed of the solution E is 0.18mL/s, and the dropping speed of the solution C is 0.16 mL/s;
(2) maintaining the temperature at 40 ℃ and stirring, uniformly mixing the solution A and the solution B to obtain an A-B mixed solution, dropwise adding the solution E into the A-B mixed solution to react for 30min, then dropwise adding the solution C, generating a black substance through oscillation reaction, releasing bubbles, releasing heat, and reacting for 40min until no bubbles are generated to obtain a seed crystal solution;
(3) maintaining the temperature at 40 ℃ and stirring, dropwise adding the solution D into the seed crystal solution, and reacting for 20 hours, wherein the dropwise adding speed of the solution D is 0.14 mL/s; solid-liquid separation, washing and vacuum drying the solid to obtain Ag3A Sn solder nano-additive; the solid washing method comprises the following steps of washing solid with solvents of pure water, absolute ethyl alcohol, pure water, acetone and absolute ethyl alcohol in sequence, and washing the solid in a centrifugal washing mode, wherein the first washing rotation speed is 1800r/min, the time is 12min, the rest rotation speeds are 1200r/min, and the time is 9 min;
example Ag3The Sn solder nano additive is analyzed by an electronic scanner, and an SEM image of the Sn solder nano additive is shown in figure 4, wherein the point 1 atom composition in figure 4See table 2, point 2 atomic composition in figure 4 see table 3,
TABLE 2 Point 1 atomic composition of FIG. 4
TABLE 3 Point 2 atomic composition of FIG. 4
The tin-based solder nano additive only contains Ag particles and Ag3Sn nanoparticles, Ag in tin-based solder nano-additive3The mass ratio of the Sn nano particles is 86 percent, and the nano particles of the tin-based solder nano additive are concentrated at 100-200nm according to the particle size distribution.
Claims (4)
1. Chemical reaction method for preparing Ag3The method for Sn solder nano additive is characterized by comprising the following specific steps:
(1) SnCl2·2H2Mixing O with anhydrous ethanol to obtain solution A, and mixing AgNO3Mixing with ammonia water to obtain solution B, adding NaBH4Mixing with absolute ethyl alcohol uniformly to obtain solution C; dissolving 1, 10-phenanthroline monohydrate in absolute ethyl alcohol to form a solution D, and dissolving PVP in absolute ethyl alcohol to form a solution E;
(2) maintaining the temperature at 20-60 ℃, uniformly mixing the solution A and the solution B to obtain an A-B mixed solution, dropwise adding the solution E into the A-B mixed solution, reacting for 20-30min, dropwise adding the solution C, and oscillating and reacting until no bubbles are generated to obtain a seed crystal solution;
(3) maintaining the temperature at 20-60 deg.C, adding solution D into the seed crystal solution dropwise for reaction for 25-30 hr, separating solid and liquid, washing the solid, and vacuum drying to obtain Ag3Sn solder nano additive.
2. Ag prepared by the chemical reaction method according to claim 13Method for Sn solder nano additiveThe method is characterized in that: the molar ratio of the silver ions in the solution B to the stannous ions in the solution A in the step (1) is 2-4:1, and the volumes of the solution A, the solution B, the solution C, the solution D and the solution E are equal.
3. Ag prepared by the chemical reaction method according to claim 1 or 23The method for Sn solder nano additive is characterized by comprising the following steps: SnCl in solution A2·2H2The concentration of O is 0.02-0.03 g/mol, and AgNO is contained in the solution B3The concentration of the NaBH is 0.04-0.06 g/mol, and the NaBH is added into the solution C4The concentration of the compound is 0.1-0.2g/mol, the concentration of the 1, 10-phenanthroline monohydrate in the solution D is 0.06-0.15 g/mol, and the concentration of PVP in the solution E is 0.087g/mol-0.104 g/mol.
4. Ag prepared by the chemical reaction method according to claim 13The method for Sn solder nano additive is characterized by comprising the following steps: and (3) sequentially using pure water, absolute ethyl alcohol, pure water, acetone and absolute ethyl alcohol as solvents for washing the solid in the step (3), and washing the solid in a centrifugal washing mode, wherein the first washing rotation speed is 1500-1800r/min, the time is 10-12min, the rest rotation speeds are 1000-1200r/min, and the time is 8-10 min.
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