CN113463152A - Surface passivation treatment method for silver particles - Google Patents
Surface passivation treatment method for silver particles Download PDFInfo
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- CN113463152A CN113463152A CN202110782146.6A CN202110782146A CN113463152A CN 113463152 A CN113463152 A CN 113463152A CN 202110782146 A CN202110782146 A CN 202110782146A CN 113463152 A CN113463152 A CN 113463152A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/006—Nanoparticles
Abstract
The invention belongs to the field of electronic packaging materials, and discloses a silver particle surface passivation treatment method. The method comprises the following steps: dispersing silver particles in a passivation solution, inserting an inert electrode as an anode, and inserting a conductive porous meshed graphene electrode as a cathode, so that the silver particles are attached to the conductive porous meshed graphene electrode; electrifying the solution to enable Cr to be deposited on the surfaces of the silver particles on the conductive porous reticular graphene electrode to be passivated; applying ultrasonic oscillation or a high-frequency electric field to the conductive porous reticular graphene electrode to enable the passivated silver particles to fall off; then, enabling new unpassivated silver particles to be attached to the conductive porous meshed graphene electrode again, and repeating the steps of electrifying and applying ultrasonic oscillation or high-frequency electric field until all the silver particles are passivated; and (4) carrying out centrifugal drying on the solution to obtain passivated silver particles. The method can also use more than three conductive porous reticular graphene electrodes as a cathode and a filter screen to treat silver particles with different particle sizes.
Description
Technical Field
The invention belongs to the field of electronic packaging materials, and particularly relates to a surface passivation treatment method for silver particles.
Background
Nanoscale and microscale metal particles are key interconnect materials in electronic packaging, however, due to their small particle size, they are easily oxidized, limiting their further applications. The passivation of metal to form a layer of compact anti-oxidation film on the surface is an important solution and is widely used. The principle is to electrify metal in a passivation solution and form a passivation film. However, for micro-nano metal particles, how to electrify the particles, how to realize uniform passivation, and how to collect passivated metal particles are all problems to be solved. Thus, there is currently no prior art for passivation of the surface of metal particles.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a silver particle surface passivation treatment method.
The purpose of the invention is realized by the following technical scheme:
a surface passivation treatment method for silver particles, when the silver particles are single-size or multi-size silver particles, comprises the following steps:
(1) dispersing silver particles in a solution containing a passivation solution;
(2) mechanically stirring the solution, inserting an inert electrode in the solution as an anode, inserting a conductive porous reticular graphene electrode as a cathode, wherein the pore diameter D of a network on the conductive porous reticular graphene electrode and the pore diameter D of the maximum silver particles satisfy the following relationship: d <0.9D, thereby attaching silver particles to the conductive porous graphene mesh electrode;
(3) electrifying the solution to enable Cr to be deposited on the surfaces of the silver particles on the conductive porous reticular graphene electrode to be passivated; applying ultrasonic oscillation or high-frequency electric field to the conductive porous netted graphene electrode at an interval of 1-10min to enable the passivated silver particles to fall off; then, enabling new unpassivated silver particles to be attached to the conductive porous meshed graphene electrode again, and repeating the steps of electrifying and applying ultrasonic oscillation or high-frequency electric field until all the silver particles are passivated;
(4) carrying out centrifugal drying on the solution to obtain passivated silver particles;
when the silver particles are multi-size silver particles, the surface passivation treatment method comprises the following steps:
(a) dispersing silver particles in a solution containing a passivation solution, and putting the solution into a closed container;
(b) mechanically stirring the solution in the container, inserting an inert electrode into the solution from the side surface of the container to serve as an anode, arranging more than three conductive porous reticular graphene electrodes serving as a cathode and a filter screen in the container, wherein the shape of the conductive porous reticular graphene electrodes is the same as the cross section of the container; the conductive porous reticular graphene electrode has different network apertures which are arranged from top to bottom in the sequence from large to small, and the sizes of the network apertures satisfy the following relation D1＝(1.2～2)D2，D2＝(1.2～2)D3And so on;
(c) a pump is arranged in the container, and the solution is driven to circularly flow from top to bottom through meshes of the conductive porous reticular graphene electrode, so that silver particles with different particle sizes are deposited and attached to the conductive porous reticular graphene electrode with corresponding sizes;
(d) electrifying the solution to enable Cr to be deposited on the surfaces of the silver particles on the conductive porous reticular graphene electrode to be passivated; turning the whole conductive porous netted graphene electrode in the container by 180 degrees at intervals of 1-10min, and applying ultrasonic vibration or a high-frequency electric field to enable the passivated silver particles to fall off; then repeating the steps (b) and (c) to enable new unpassivated silver particles to be attached to the conductive porous reticular graphene electrode again, and repeating the steps of electrifying and applying ultrasonic vibration or high-frequency electric field until all the silver particles are passivated;
(e) carrying out centrifugal drying on the solution to obtain passivated silver particles;
the pH value of the solution containing the passivation solution is 2-9, wherein the solvent is water, methanol or ethanol, and the solute is H2O2One or more of diaminotriazene, acrylic resin, epoxy resin, tannic acid, phytic acid and organic molybdate, and Cr3+、Cr6+、SO4 2-、Cl-、NO3 -A mixture of ions and alkali metal ions.
The size of the silver particles is 10nm-100 mu m.
The inert electrode in the step (2) and the step (b) is graphite.
And (d) keeping the temperature at-20-100 ℃ and the voltage at 0-100V in the passivation process in the step (3) and the step (d).
And (d) introducing air or oxygen while performing ultrasonic and stirring treatment on the solution in the passivation process in the steps (3) and (d).
The frequency f of the ultrasonic oscillation or high-frequency electric field in the step (3) and the step (d) is selected in various ways1,f2,f3) And satisfies the following relationship:
(0.5+n)ci/fi＝Li，i＝1,2,3
wherein n is an arbitrary natural number, c1Is the surface transverse wave sound velocity L of the conductive porous reticular graphene electrode1Is a conductive porous network graphene electrode characteristic dimension, c2Is the acoustic velocity of silver particle body, L2Is the characteristic size of silver particles, c3Is the sound velocity of the solution body sound wave, L3The distance between the anode electrode and the conductive porous reticular graphene electrode is shown.
After the passivation process in the step (3) and the step (d) is finished, the conductive porous netted graphene electrode is extracted and placed in another solution, and hexadecyltrimethylammonium bromide (CTAB) and a fatty acid salt small molecule surfactant are added into the other solution, so that the surface energy of silver particles is reduced, and the silver particles are promoted to fall off; and (3) applying ultrasonic oscillation to enable the passivated silver particles to fall off, and then carrying out centrifugal drying on the solution to obtain the passivated silver particles.
Compared with the prior art, the invention has the following advantages and effects: the invention provides a treatment method for passivating the surface of metal particles for the first time, can realize methods for passivating and collecting micro-nano silver particles, and is suitable for realizing the function of passivating particles with different sizes at one time.
Drawings
FIG. 1 is a process flow diagram of a process A for passivating a surface of a silver particle;
FIG. 2 is a process flow diagram of a surface passivation treatment method B for silver particles;
the method comprises the following steps of 1-silver particles, 2-solution containing passivation solution, 3-anode, 4-conductive porous reticular graphene electrode, 5-passivation layer, 6-mechanical stirring, 7-ultrasonic wave with specific frequency, 8-water circulation manufactured by using a pump, 9-large-aperture reticular graphene electrode, 10-medium-aperture reticular graphene electrode, 11-small-aperture reticular graphene electrode and 12-turnover graphene electrode.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
The frequency f of the ultrasonic oscillation or high-frequency electric field described in the following examples is variously selected (f)1,f2,f3) And satisfies the following relationship:
(0.5+n)ci/fi＝Li，i＝1,2,3
wherein n is an arbitrary natural number, c1Is the surface transverse wave sound velocity L of the conductive porous reticular graphene electrode1Is a conductive porous network graphene electrode characteristic dimension, c2Is the acoustic velocity of silver particle body, L2Is the characteristic size of silver particles, c3Is the sound velocity of the solution body sound wave, L3The distance between the anode electrode and the conductive porous reticular graphene electrode is shown.
The temperature was maintained between-20 deg.C and 100 deg.C during the passivation process described in the examples below.
Example 1 silver particle surface passivation method a, the process flow is shown in fig. 1, where 1-silver particles, 2-solution containing passivation solution, 3-anode, 4-conductive porous reticular graphene electrode, 5-passivation layer, 6-mechanical stirring, 7-ultrasonic wave of specific frequency.
(1) Dispersing silver particles with the average size of 100nm in a solution containing a passivation solution; the solution containing the passivation solution has a pH value of 3, the solvent is ethanol, and the solute is H2O2、Cr3+、Cr6+、SO4 2-、Cl-、NO3 -A mixture of ions and alkali metal ions;
(2) mechanically stirring the solution, inserting graphite into the solution as an anode, and inserting a conductive porous reticular graphene electrode with the aperture of 80nm as a cathode, so that silver particles are attached to the conductive porous reticular graphene electrode;
(3) electrifying the solution, wherein the voltage is 5V, and depositing Cr on the surface of silver particles on the conductive porous reticular graphene electrode to passivate the silver particles; applying 12.5MHz ultrasonic vibration to the conductive porous meshed graphene electrode at an interval of 1min to enable the passivated silver particles to fall off; then, enabling new unpassivated silver particles to be attached to the conductive porous meshed graphene electrode again, and repeating the steps of electrifying and applying ultrasonic oscillation or high-frequency electric field until all the silver particles are passivated;
(4) and (4) carrying out centrifugal drying on the solution to obtain passivated silver particles.
Example 2 silver particle surface passivation method B, the process flow is shown in fig. 2, where 1-silver particles, 2-solution containing passivation solution, 3-anode, 5-passivation layer, 6-mechanical stirring, 7-ultrasonic wave of specific frequency, 8-water circulation by pump, 9-large pore diameter mesh graphene electrode, 10-medium pore diameter mesh graphene electrode, 11-small pore diameter mesh graphene electrode, 12-reversed graphene electrode.
(a) Dispersing silver particles of 140nm, 110nm and 80nm in a solution containing passivation solution, and putting the solution into a closed container; the solution containing the passivation solution has a pH value of 7, the solvent is methanol, and the solute is acrylic resin and Cr3+、Cr6+、SO4 2-、Cl-、NO3 -A mixture of ions and alkali metal ions;
(b) mechanically stirring the solution in the container, inserting an inert electrode into the solution from the side surface of the container to serve as an anode, arranging three conductive porous reticular graphene electrodes serving as a cathode and a filter screen in the container, wherein the shape of the conductive porous reticular graphene electrodes is the same as the cross section of the container; the network pore diameters of the three conductive porous reticular graphene electrodes are respectively 120nm, 90nm and 60nm, and the three conductive porous reticular graphene electrodes are arranged from top to bottom in the sequence of the network pore diameters from large to small;
(c) a pump is arranged in the container, and the solution is driven to circularly flow from top to bottom through meshes of the conductive porous reticular graphene electrode, so that silver particles with different particle sizes are deposited and attached to the conductive porous reticular graphene electrode with corresponding sizes;
(d) electrifying the solution, wherein the voltage is 5V, and depositing Cr on the surface of silver particles on the conductive porous reticular graphene electrode to passivate the silver particles; turning the whole conductive porous meshed graphene electrode in the container by 180 degrees at an interval of 1min, and applying 12.5MHz ultrasonic vibration to enable the passivated silver particles to fall off; then repeating the steps (b) and (c) to enable new unpassivated silver particles to be attached to the conductive porous reticular graphene electrode again, and repeating the steps of electrifying and applying ultrasonic vibration or high-frequency electric field until all the silver particles are passivated;
(e) and (4) carrying out centrifugal drying on the solution to obtain passivated silver particles.
Example 3
The other steps are the same as the embodiment 1, and the difference is that after the passivation process in the step (3) is finished, the conductive porous meshed graphene electrode is extracted and placed in another solution, and hexadecyltrimethylammonium bromide (CTAB) and a fatty acid salt small molecule surfactant are added into the other solution, so that the surface energy of silver particles is reduced, and the shedding of the silver particles is promoted; applying ultrasonic vibration to lead the passivated silver particles to fall off; repeating the operation until all the silver particles are passivated; and then, carrying out centrifugal drying on the other solution to obtain passivated silver particles.
Example 4
The other steps are the same as the embodiment 2, and the difference is that after the passivation process in the step (d) is finished, the conductive porous reticular graphene electrode is extracted and placed in another solution, and hexadecyltrimethylammonium bromide (CTAB) and a fatty acid salt micromolecular surfactant are added into the other solution, so that the surface energy of silver particles is reduced, and the shedding of the silver particles is promoted; applying ultrasonic vibration to lead the passivated silver particles to fall off; repeating the operation until all the silver particles are passivated; and then, carrying out centrifugal drying on the other solution to obtain passivated silver particles.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A surface passivation treatment method for silver particles is characterized by comprising the following steps:
when the silver particles are single-size or multi-size silver particles, the surface passivation treatment method comprises the following steps:
(1) dispersing silver particles in a solution containing a passivation solution;
(2) mechanically stirring the solution, inserting an inert electrode in the solution as an anode, inserting a conductive porous reticular graphene electrode as a cathode, wherein the pore diameter D of a network on the conductive porous reticular graphene electrode and the pore diameter D of the maximum silver particles satisfy the following relationship: d <0.9D, thereby attaching silver particles to the conductive porous graphene mesh electrode;
(3) electrifying the solution to enable Cr to be deposited on the surfaces of the silver particles on the conductive porous reticular graphene electrode to be passivated; applying ultrasonic oscillation or high-frequency electric field to the conductive porous netted graphene electrode at an interval of 1-10min to enable the passivated silver particles to fall off; then, enabling new unpassivated silver particles to be attached to the conductive porous meshed graphene electrode again, and repeating the steps of electrifying and applying ultrasonic oscillation or high-frequency electric field until all the silver particles are passivated;
(4) carrying out centrifugal drying on the solution to obtain passivated silver particles;
when the silver particles are multi-size silver particles, the surface passivation treatment method comprises the following steps:
(a) dispersing silver particles in a solution containing a passivation solution, and putting the solution into a closed container;
(b) mechanically stirring the solution in the container, inserting an inert electrode into the solution from the side surface of the container to serve as an anode, arranging more than three conductive porous reticular graphene electrodes serving as a cathode and a filter screen in the container, wherein the shape of the conductive porous reticular graphene electrodes is the same as the cross section of the container; the conductive porous reticular graphene electrode has different network apertures which are arranged from top to bottom in the sequence from large to small, and the sizes of the network apertures satisfy the following relation D1＝(1.2～2)D2，D2＝(1.2～2)D3And so on;
(c) a pump is arranged in the container, and the solution is driven to circularly flow from top to bottom through meshes of the conductive porous reticular graphene electrode, so that silver particles with different particle sizes are deposited and attached to the conductive porous reticular graphene electrode with corresponding sizes;
(d) electrifying the solution to enable Cr to be deposited on the surfaces of the silver particles on the conductive porous reticular graphene electrode to be passivated; turning the whole conductive porous netted graphene electrode in the container by 180 degrees at intervals of 1-10min, and applying ultrasonic vibration or a high-frequency electric field to enable the passivated silver particles to fall off; then repeating the steps (b) and (c) to enable new unpassivated silver particles to be attached to the conductive porous reticular graphene electrode again, and repeating the steps of electrifying and applying ultrasonic vibration or high-frequency electric field until all the silver particles are passivated;
(e) carrying out centrifugal drying on the solution to obtain passivated silver particles;
the pH value of the solution containing the passivation solution is 2-9, wherein the solvent is water, methanol or ethanol, and the solute is H2O2One or more of diaminotriazene, acrylic resin, epoxy resin, tannic acid, phytic acid and organic molybdate, and Cr3+、Cr6+、SO4 2-、Cl-、NO3 -A mixture of ions and alkali metal ions.
2. The method for passivating the surface of silver particles according to claim 1, wherein: the size of the silver particles is 10nm-100 mu m.
3. The method for passivating the surface of silver particles according to claim 1, wherein: the inert electrode in the step (2) and the step (b) is graphite.
4. The method for passivating the surface of silver particles according to claim 1, wherein: and (d) keeping the temperature at-20-100 ℃ and the voltage at 0-100V in the passivation process in the step (3) and the step (d).
5. The method for passivating the surface of silver particles according to claim 1, wherein: and (d) introducing air or oxygen while performing ultrasonic and stirring treatment on the solution in the passivation process in the steps (3) and (d).
6. The method for passivating the surface of silver particles according to claim 1, wherein: the frequency f of the ultrasonic oscillation or high-frequency electric field in the step (3) and the step (d) is selected in various ways1,f2,f3) And satisfies the following relationship:
(0.5+n)ci/fi＝Li，i＝1,2,3
wherein n is an arbitrary natural number, c1Is the surface transverse wave sound velocity L of the conductive porous reticular graphene electrode1Is a conductive porous network graphene electrode characteristic dimension, c2Is the acoustic velocity of silver particle body, L2Is the characteristic size of silver particles, c3Is the sound velocity of the solution body sound wave, L3The distance between the anode electrode and the conductive porous reticular graphene electrode is shown.
7. The method for passivating the surface of silver particles according to claim 1, wherein: after the passivation process in the step (3) and the step (d) is finished, extracting the conductive porous netted graphene electrode and placing the conductive porous netted graphene electrode into another solution, wherein hexadecyltrimethylammonium bromide and a fatty acid salt micromolecule surfactant are added into the other solution, so that the surface energy of silver particles is reduced, and the shedding of the silver particles is promoted; and (3) applying ultrasonic oscillation to enable the passivated silver particles to fall off, and then carrying out centrifugal drying on the solution to obtain the passivated silver particles.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6183545B1 (en) * | 1998-07-14 | 2001-02-06 | Daiwa Fine Chemicals Co., Ltd. | Aqueous solutions for obtaining metals by reductive deposition |
| CN1557880A (en) * | 2004-02-13 | 2004-12-29 | 黄德欢 | Process for preparing silver-based polynary nano composite powder |
| CN107217281A (en) * | 2017-05-26 | 2017-09-29 | 华中科技大学 | A kind of NEW TYPE OF COMPOSITE resistance tritium coating and preparation method thereof |
| CN109137524A (en) * | 2018-07-18 | 2019-01-04 | 开封大学 | A kind of preparation method of Ag doped silicon carbide nano wave-absorbing material |
| CN110628298A (en) * | 2019-08-09 | 2019-12-31 | 广州市千龙竞舞装饰材料有限公司 | Preparation method of imitation electroplating auxiliary agent for powder coating |
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- 2021-07-12 CN CN202110782146.6A patent/CN113463152A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6183545B1 (en) * | 1998-07-14 | 2001-02-06 | Daiwa Fine Chemicals Co., Ltd. | Aqueous solutions for obtaining metals by reductive deposition |
| CN1557880A (en) * | 2004-02-13 | 2004-12-29 | 黄德欢 | Process for preparing silver-based polynary nano composite powder |
| CN107217281A (en) * | 2017-05-26 | 2017-09-29 | 华中科技大学 | A kind of NEW TYPE OF COMPOSITE resistance tritium coating and preparation method thereof |
| CN109137524A (en) * | 2018-07-18 | 2019-01-04 | 开封大学 | A kind of preparation method of Ag doped silicon carbide nano wave-absorbing material |
| CN110628298A (en) * | 2019-08-09 | 2019-12-31 | 广州市千龙竞舞装饰材料有限公司 | Preparation method of imitation electroplating auxiliary agent for powder coating |
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