CN111069593A - High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof - Google Patents

High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof Download PDF

Info

Publication number
CN111069593A
CN111069593A CN201911389974.2A CN201911389974A CN111069593A CN 111069593 A CN111069593 A CN 111069593A CN 201911389974 A CN201911389974 A CN 201911389974A CN 111069593 A CN111069593 A CN 111069593A
Authority
CN
China
Prior art keywords
copper alloy
nitrate
coated copper
silver
alloy particles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201911389974.2A
Other languages
Chinese (zh)
Inventor
沈仙林
周斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henan Jinqu Yintong Metal Material Co ltd
Original Assignee
Henan Jinqu Yintong Metal Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henan Jinqu Yintong Metal Material Co ltd filed Critical Henan Jinqu Yintong Metal Material Co ltd
Priority to CN201911389974.2A priority Critical patent/CN111069593A/en
Publication of CN111069593A publication Critical patent/CN111069593A/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention relates to the technical field of silver-coated copper alloy particles for flexible circuits, in particular to a high-performance silver-coated copper alloy particle for a flexible circuit and a preparation method thereof. The high-performance silver-coated copper alloy particles for the flexible circuit at least comprise the following components in parts by weight: 100 portions of nitrate ion-exchanged 130 portions, 50 portions to 70 portions of reducing agent, 1.2 portions to 1.8 portions of dispersing agent and 120 portions of ammonia ion-exchanged 130 portions; the nitrate is silver nitrate and copper nitrate. According to the invention, the silver-coated copper alloy particles are prepared from nitrate, a reducing agent, a dispersing agent and ammonia water, and the prepared silver-coated copper alloy particles are regular in morphology, uniform in size distribution, narrow in particle size distribution, free of agglomeration phenomenon, excellent in performance and capable of being widely applied to flexible circuits.

Description

High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof
Technical Field
The invention relates to the technical field of silver-coated copper alloy particles for flexible circuits, in particular to a high-performance silver-coated copper alloy particle for a flexible circuit and a preparation method thereof.
Background
Flexible Circuits (also called membrane Circuits) are special Circuits formed by mounting electronic components on a flexible substrate, which is usually a polymer material such as polyimide plastic, polyetheretherketone, or transparent conductive terylene. Its advantages include light weight, thin thickness, and high flexibility.
The electronic paste material is a novel nanometer functional material integrating materials, chemical engineering and electronic technology, and is a basic material of integrated circuits, sensitive elements, surface assembled components, displays, various electronic discrete elements and the like. The electronic paste mainly comprises three parts: a conductive phase (functional phase), a binder phase (glass phase) and an organic vehicle. The electronic paste is usually in a fluid state, solid powder in the paste is thinned uniformly, the particle size distribution is uniform, conductive phase particles are in a spherical or flaky shape, and the average particle size of a binder phase is smaller than 1 mm. The organic carrier phase can be matched with the organic carrier phase and the organic carrier phase according to different requirements, so that the compatibility and the product consistency are good. Electronic paste has many classification methods, and is mainly divided into conductive paste, resistance paste, thick film paste, dielectric paste, welding paste and the like according to the application; the main components are as follows: noble metal electronic paste, base metal electronic paste and composite component electronic paste. The electronic paste is a main functional material necessary for chip resistors, capacitors, potentiometers, thick film circuits, hybrid integrated circuits, flexible circuits and the like.
The conductive phases used in the electronic paste include carbon, metal and metal oxide. Carbon black in carbon-based materials has good conductivity, but is difficult to crush and disperse, and difficult to process. TiO 22Metal oxides such as PdO have poor conductivity, and it is difficult to fabricate high-quality electrodes. The metal powder material is a common conductive phase and mainly comprises metal powder with low resistivity such as Au, Ag, Cu, Ni and the like. Wherein, the cost of Au and Ag powder is higher; cu, Ni powders are relatively inexpensive but are easily oxidized when the temperature is increased.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides high-performance silver-coated copper alloy particles for flexible circuits, comprising at least the following components in parts by weight: 100 portions of nitrate ion-exchanged 130 portions, 50 portions to 70 portions of reducing agent, 1.2 portions to 1.8 portions of dispersing agent and 120 portions of ammonia ion-exchanged 130 portions; the nitrate is silver nitrate and copper nitrate.
As a preferable technical scheme, the paint at least comprises the following components in parts by weight: 115 parts of nitrate, 60 parts of reducing agent, 1.5 parts of dispersing agent and 125 parts of ammonia water.
As a preferable technical scheme, the concentration of the ammonia water is 10 wt%.
As a preferable technical scheme, the nitrate comprises, by weight, 90-110 parts of silver nitrate and 10-20 parts of copper nitrate.
As a preferable technical scheme, the molar ratio of the silver nitrate to the copper nitrate is (7-13): 1.
as a preferred technical scheme, the reducing agent is at least one selected from ascorbic acid, formaldehyde, hydrazine hydrate, sodium hypophosphite and sodium borohydride.
In a preferred embodiment, the dispersing agent is at least one selected from polyvinylpyrrolidone, gelatin, and gum arabic.
As a preferable technical scheme, the weight ratio of the reducing agent to the silver nitrate is (0.4-0.7): 1.
as a preferable technical scheme, the weight ratio of the dispersant to the nitrate is 1: (72-84).
The second aspect of the invention provides a preparation method of high-performance silver-coated copper alloy particles for a flexible circuit, which at least comprises the following steps:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at the temperature of 120-.
Has the advantages that: according to the invention, the silver-coated copper alloy particles are prepared from nitrate, a reducing agent, a dispersing agent and ammonia water, and the prepared silver-coated copper alloy particles are regular in morphology, uniform in size distribution, narrow in particle size distribution, free of agglomeration, excellent in performance, low in cost and capable of being widely applied to flexible circuits.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
fig. 1 is an SEM image of high-performance silver-coated copper alloy particles for a flexible circuit.
Fig. 2 is a TEM image of high performance silver-coated copper alloy particles for flexible circuits.
Fig. 3 is an SEDA diagram of high performance silver-coated copper alloy particles for flexible circuits.
Fig. 4 is a graph showing a particle size distribution of high-performance silver-clad copper alloy particles for a flexible circuit.
Detailed Description
The technical features in the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, but the scope of protection of the present invention is not limited thereto.
"preferred", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides a high-performance silver-coated copper alloy particle for a flexible circuit, which at least comprises the following components in parts by weight: 100 portions of nitrate ion-exchange resin 130 portions, 50 portions to 70 portions of reducing agent, 1.2 portions to 1.8 portions of dispersing agent and 120 portions of ammonia water ion-exchange resin 130 portions.
In a preferred embodiment, at least the following ingredients are included in parts by weight: 115 parts of nitrate, 60 parts of reducing agent, 1.5 parts of dispersing agent and 125 parts of ammonia water.
In a preferred embodiment, the nitrates are silver nitrate and copper nitrate.
In a preferred embodiment, the nitrate comprises 90-110 parts of silver nitrate and 10-20 parts of copper nitrate in parts by weight.
In a more preferred embodiment, the nitrate comprises 100 parts by weight of silver nitrate and 15 parts by weight of copper nitrate.
In a preferred embodiment, the molar ratio of silver nitrate to copper nitrate is (7-13): 1.
in a preferred embodiment, the reducing agent is selected from at least one of ascorbic acid, formaldehyde, hydrazine hydrate, sodium hypophosphite, sodium borohydride.
In a more preferred embodiment, the reducing agent is ascorbic acid.
In a preferred embodiment, the weight ratio of the reducing agent to the silver nitrate is (0.4-0.7): 1.
in a more preferred embodiment, the weight ratio of reducing agent to silver nitrate is 0.6: 1.
the reduction potential of the ascorbic acid is greatly influenced by the pH value of the system, when the pH value of the system is controlled to be 4.5-5, the ascorbic acid has good reduction capability and high reaction speed, the number of generated crystal nuclei is increased, and the size distribution of the prepared alloy particles is uniform.
In a preferred embodiment, the dispersing agent is selected from at least one of polyvinylpyrrolidone, gelatin, gum arabic.
In a more preferred embodiment, the dispersing agent is gum arabic.
The CAS number of the Arabic gum is 9000-01-5.
In a preferred embodiment, the weight ratio of the dispersant to the nitrate is 1: (72-84).
In a preferred embodiment, the concentration of the aqueous ammonia is 10 wt%.
The introduction of the dispersing agent can change the growth speed of crystal faces and protect the surfaces of particles to prevent agglomeration. The applicant found that when gum arabic is used as the dispersant, and the weight ratio of the dispersant to the nitrate is controlled to be 1: (72-84), when the pH value of the system is 4.5-5, the prepared silver-coated copper alloy particles are regular in shape and uniform in size distribution. The applicant speculates that possible reasons are: on one hand, the Arabic gum is structurally provided with an acidic group and has the characteristic of relatively stable acidic environment; on the other hand, the Arabic gum has strong adsorption capacity, can provide a polymer chain layer and is strongly adsorbed on the surface of the particles to form a protective layer, so that the particles are prevented from being aggregated due to approach; meanwhile, under a specific condition, the steric effect existing between the Arabic gums increases the distance between the particles, so that the particles are not contacted tightly, and the silver-copper alloy particles are prevented from colliding and agglomerating with each other.
The second aspect of the invention provides a preparation method of high-performance silver-coated copper alloy particles for a flexible circuit, which at least comprises the following steps:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at the temperature of 120-.
In a preferred embodiment, the method for preparing the high-performance silver-coated copper alloy particles for the flexible circuit at least comprises the following steps:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at 125 ℃ at a stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 45min, adjusting the pH to be 5, reacting for 2.5h after the solution C is completely dropped, and finally performing aftertreatment to obtain the high-performance silver-coated copper alloy particles for the flexible circuit.
In a preferred embodiment, in the step (1), the weight ratio of the reducing agent to the first part of water is (2.5-3.5): 40.
in a more preferred embodiment, in the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
in a preferred embodiment, the volume ratio of the first part of water, the second part of water and the third part of water is (3-5): 1: (0.8-1.5).
In a more preferred embodiment, the volume ratio of the first, second and third water portions is 4: 1: 1.
in a preferred embodiment, the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 2-3 times, and drying in a vacuum drying oven at 50 deg.C for 3 h.
The reaction temperature can influence the molecular motion rate in the reaction process, and the applicant finds through a large number of experiments that when the reaction temperature is controlled to be 120-130 ℃, the shape of the prepared silver-coated copper alloy particles is regular and the size distribution is uniform. This is probably because the reducing power of ascorbic acid is strong under a specific temperature condition, resulting in an increase in the nucleation rate. When the reaction temperature is too low, the reducing capability of the ascorbic acid is weak, and the prepared silver-coated copper alloy particles are irregular in shape and uneven in size distribution; when the reaction temperature is too high, brownian motion of particles is accelerated due to a very fast reaction rate, so that silver-copper alloy particles frequently collide with each other, thereby causing particle agglomeration.
Hereinafter, the present invention will be described in more detail by way of examples, but it should be understood that these examples are merely illustrative and not restrictive. In addition, all the raw materials are commercially available if not particularly limited.
Examples
Example 1
Embodiment 1 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, comprising the following components in parts by weight: 115 parts of nitrate, 60 parts of reducing agent, 1.5 parts of dispersing agent and 125 parts of ammonia water.
The nitrate is silver nitrate and copper nitrate.
The nitrate comprises 100 parts of silver nitrate and 15 parts of copper nitrate in parts by weight.
The reducing agent is ascorbic acid.
The dispersing agent is Arabic gum.
The concentration of the ammonia water is 10 wt%.
Embodiment 1 of the present invention also provides a method for preparing high-performance silver-coated copper alloy particles for a flexible circuit, including the steps of:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at 125 ℃ at a stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 45min, adjusting the pH to be 5, reacting for 2.5h after the solution C is completely dropped, and finally performing aftertreatment to obtain the high-performance silver-coated copper alloy particles for the flexible circuit.
In the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
the volume ratio of the first part of water to the second part of water to the third part of water is 4: 1: 1.
the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 3 times, and drying in vacuum drying oven at 50 deg.C for 3 hr.
The SEM image of the high-performance silver-coated copper alloy particles for flexible circuits prepared in example 1 is shown in fig. 1.
A TEM image of high performance silver-coated copper alloy particles for flexible circuits prepared in example 1 is shown in fig. 2.
The SEDA chart of the high-performance silver-coated copper alloy particles for flexible circuits prepared in example 1 is shown in fig. 3.
The particle size distribution curve of the high-performance silver-coated copper alloy particles for the flexible circuit prepared in example 1 is shown in fig. 4.
Example 2
Embodiment 2 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, which comprises the following components in parts by weight: 100 parts of nitrate, 50 parts of reducing agent, 1.2 parts of dispersing agent and 120 parts of ammonia water.
The nitrate is silver nitrate and copper nitrate.
The nitrate comprises 90 parts of silver nitrate and 10 parts of copper nitrate in parts by weight.
The reducing agent is ascorbic acid.
The dispersing agent is Arabic gum.
The concentration of the ammonia water is 10 wt%.
Embodiment 2 of the present invention also provides a method for preparing high-performance silver-coated copper alloy particles for a flexible circuit, including the following steps:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at the temperature of 120 ℃ at the stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 40min, adjusting the pH to be 4.5, reacting for 2.5h after the solution C is completely dropped, and finally carrying out aftertreatment to prepare the high-performance silver-coated copper alloy particle for the flexible circuit.
In the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
the volume ratio of the first part of water to the second part of water to the third part of water is 4: 1: 1.
the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 3 times, and drying in vacuum drying oven at 50 deg.C for 3 hr.
Example 3
Embodiment 3 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, comprising the following components in parts by weight: 130 parts of nitrate, 70 parts of reducing agent, 1.8 parts of dispersing agent and 130 parts of ammonia water.
The nitrate is silver nitrate and copper nitrate.
The nitrate comprises, by weight, 110 parts of silver nitrate and 20 parts of copper nitrate.
The reducing agent is ascorbic acid.
The dispersing agent is Arabic gum.
The concentration of the ammonia water is 10 wt%.
Embodiment 3 of the present invention further provides a method for preparing high-performance silver-coated copper alloy particles for a flexible circuit, including the following steps:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at 130 ℃ at a stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 50min, adjusting the pH to be 5, reacting for 2.5h after the solution C is completely dropped, and finally performing aftertreatment to obtain the high-performance silver-coated copper alloy particles for the flexible circuit.
In the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
the volume ratio of the first part of water to the second part of water to the third part of water is 4: 1: 1.
the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 3 times, and drying in vacuum drying oven at 50 deg.C for 3 hr.
Example 4
Embodiment 4 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, and a method for preparing the high performance silver-coated copper alloy particle for the flexible circuit, which is the same as embodiment 1 except that the reducing agent is formaldehyde.
Example 5
Embodiment 5 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, and further provides a method for preparing the high performance silver-coated copper alloy particle for the flexible circuit, which is the same as embodiment 1 in specific implementation manner, except that the reducing agent is hydrazine hydrate.
Example 6
Embodiment 6 of the present invention provides high performance silver-coated copper alloy particles for a flexible circuit, and further provides a method for preparing the high performance silver-coated copper alloy particles for the flexible circuit, which is the same as embodiment 1 in specific implementation manner, except that the reducing agent is sodium hypophosphite.
Example 7
Embodiment 7 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, and further provides a method for preparing the high performance silver-coated copper alloy particle for the flexible circuit, which is the same as embodiment 1 in specific implementation manner, except that the reducing agent is sodium borohydride.
Example 8
Embodiment 8 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, and further provides a method for preparing the high performance silver-coated copper alloy particle for the flexible circuit, which is the same as embodiment 1 except that the dispersant is polyvinylpyrrolidone (K30), and the polyvinylpyrrolidone (K30) has CAS number 9003-39-8.
Example 9
Embodiment 9 of the present invention provides a high performance silver-coated copper alloy particle for a flexible circuit, and a method for producing the high performance silver-coated copper alloy particle for the flexible circuit, which is the same as embodiment 1 except that the dispersant is gelatin having CAS number of 135151-90-5.
Example 10
Embodiment 10 of the present invention provides a high-performance silver-coated copper alloy particle for a flexible circuit, and a method for producing a high-performance silver-coated copper alloy particle for a flexible circuit, and the specific embodiment is the same as embodiment 1, except that the content of the dispersant is replaced with 1 part.
Example 11
Embodiment 11 of the present invention provides high-performance silver-coated copper alloy particles for a flexible circuit, and a method for producing the high-performance silver-coated copper alloy particles for the flexible circuit, and the specific embodiment is the same as embodiment 1, except that the content of the dispersant is replaced with 2 parts.
Example 12
Embodiment 12 of the present invention provides a high-performance silver-coated copper alloy particle for a flexible circuit, and a method for producing a high-performance silver-coated copper alloy particle for a flexible circuit, which is the same as embodiment 1 in specific embodiment, except that the method for producing a high-performance silver-coated copper alloy particle for a flexible circuit includes the steps of:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at 125 ℃ at a stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 45min, adjusting the pH to be 3.5, reacting for 2.5h after the solution C is completely dropped, and finally carrying out aftertreatment to prepare the high-performance silver-coated copper alloy particle for the flexible circuit.
In the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
the volume ratio of the first part of water to the second part of water to the third part of water is 4: 1: 1.
the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 3 times, and drying in vacuum drying oven at 50 deg.C for 3 hr.
Example 13
Embodiment 13 of the present invention provides a high-performance silver-coated copper alloy particle for a flexible circuit, and a method for producing a high-performance silver-coated copper alloy particle for a flexible circuit, which is the same as embodiment 1 in specific embodiment, except that the method for producing a high-performance silver-coated copper alloy particle for a flexible circuit includes the steps of:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at 125 ℃ at a stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 45min, adjusting the pH to be 6, reacting for 2.5h after the solution C is completely dropped, and finally performing aftertreatment to obtain the high-performance silver-coated copper alloy particles for the flexible circuit.
In the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
the volume ratio of the first part of water to the second part of water to the third part of water is 4: 1: 1.
the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 3 times, and drying in vacuum drying oven at 50 deg.C for 3 hr.
Example 14
Embodiment 14 of the present invention provides a high-performance silver-coated copper alloy particle for a flexible circuit, and a method for producing a high-performance silver-coated copper alloy particle for a flexible circuit, which is the same as embodiment 1 in specific embodiment, except that the method for producing a high-performance silver-coated copper alloy particle for a flexible circuit includes the steps of:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at 110 ℃ at a stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 45min, adjusting the pH to be 5, reacting for 2.5h after the solution C is completely dropped, and finally performing aftertreatment to obtain the high-performance silver-coated copper alloy particles for the flexible circuit.
In the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
the volume ratio of the first part of water to the second part of water to the third part of water is 4: 1: 1.
the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 3 times, and drying in vacuum drying oven at 50 deg.C for 3 hr.
Example 15
Embodiment 15 of the present invention provides a high-performance silver-coated copper alloy particle for a flexible circuit, and further provides a method for preparing a high-performance silver-coated copper alloy particle for a flexible circuit, and the specific implementation manner of the method is the same as that in embodiment 1, except that the method for preparing a high-performance silver-coated copper alloy particle for a flexible circuit includes the following steps:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at 140 ℃ at a stirring speed of 600r/min, adding the solution C and ammonia water, adjusting the dropping speed of the solution C and the ammonia water to control the whole dropping process to be 45min, adjusting the pH to be 5, reacting for 2.5h after the solution C is completely dropped, and finally performing aftertreatment to obtain the high-performance silver-coated copper alloy particles for the flexible circuit.
In the step (1), the weight ratio of the reducing agent to the first part of water is 3: 40.
the volume ratio of the first part of water to the second part of water to the third part of water is 4: 1: 1.
the post-treatment process comprises the following steps: centrifuging, washing with deionized water and ethanol for 3 times, and drying in vacuum drying oven at 50 deg.C for 3 hr.
Performance evaluation
Example 1: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method are regular in shape, uniform in particle size distribution, free of agglomeration and free of impurities.
Example 2: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method are regular in shape, uniform in particle size distribution, free of agglomeration and free of impurities.
Example 3: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method are regular in shape, uniform in particle size distribution, free of agglomeration and free of impurities.
Example 4: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, slight agglomeration and no impurities.
Example 5: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
Example 6: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, slight agglomeration and impurities.
Example 7: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and impurities.
Example 8: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
Example 9: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
Example 10: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
Example 11: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, slight agglomeration and no impurities.
Example 12: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
Example 13: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
Example 14: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
Example 15: the high-performance silver-coated copper alloy particles for the flexible circuit prepared by the method have irregular shapes, uneven particle size distribution, agglomeration phenomenon and no impurities.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. The use of some numerical ranges in the claims also includes sub-ranges within their range, and variations in these ranges are also to be construed as being covered by the appended claims where possible.

Claims (10)

1. The high-performance silver-coated copper alloy particles for the flexible circuit are characterized by at least comprising the following components in parts by weight: 100 portions of nitrate ion-exchanged 130 portions, 50 portions to 70 portions of reducing agent, 1.2 portions to 1.8 portions of dispersing agent and 120 portions of ammonia ion-exchanged 130 portions; the nitrate is silver nitrate and copper nitrate.
2. The high-performance silver-coated copper alloy particles for flexible circuits according to claim 1, which comprises at least the following components in parts by weight: 115 parts of nitrate, 60 parts of reducing agent, 1.5 parts of dispersing agent and 125 parts of ammonia water.
3. The high-performance silver-coated copper alloy particles for a flexible circuit according to claim 1 or 2, wherein the concentration of the aqueous ammonia is 10% by weight.
4. The high-performance silver-coated copper alloy particles for flexible circuits according to claim 1, wherein said nitrate contains, by weight, 90 to 110 parts of silver nitrate and 10 to 20 parts of copper nitrate.
5. The high-performance silver-coated copper alloy particles for flexible circuits according to claim 4, wherein the molar ratio of silver nitrate to copper nitrate is (7-13): 1.
6. the high-performance silver-coated copper alloy particles for flexible circuits according to claim 1, wherein said reducing agent is at least one selected from the group consisting of ascorbic acid, formaldehyde, hydrazine hydrate, sodium hypophosphite and sodium borohydride.
7. The high-performance silver-coated copper alloy particles for flexible circuits according to claim 1, wherein said dispersing agent is at least one selected from the group consisting of polyvinylpyrrolidone, gelatin, and gum arabic.
8. The high-performance silver-coated copper alloy particles for flexible circuits according to claim 1 or 2, wherein the weight ratio of the reducing agent to silver nitrate is (0.4 to 0.7): 1.
9. the high-performance silver-coated copper alloy particles for flexible circuits according to claim 1 or 2, wherein the weight ratio of the dispersant to the nitrate is 1: (72-84).
10. A method for producing high-performance silver-coated copper alloy particles for flexible circuits according to any one of claims 1 to 9, comprising at least the steps of:
(1) dissolving a reducing agent in the first portion of water to obtain a solution A;
(2) dissolving a dispersing agent in the second part of water to obtain a solution B;
(3) dissolving nitrate in the third part of water to obtain a solution C;
(4) and stirring and mixing the solution A and the solution B at the temperature of 120-.
CN201911389974.2A 2019-12-30 2019-12-30 High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof Withdrawn CN111069593A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911389974.2A CN111069593A (en) 2019-12-30 2019-12-30 High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911389974.2A CN111069593A (en) 2019-12-30 2019-12-30 High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof

Publications (1)

Publication Number Publication Date
CN111069593A true CN111069593A (en) 2020-04-28

Family

ID=70319299

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911389974.2A Withdrawn CN111069593A (en) 2019-12-30 2019-12-30 High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111069593A (en)

Similar Documents

Publication Publication Date Title
KR101301634B1 (en) Silver-copper composite powder having silver microparticule attached thereto, and method of production of the silver-copper composite powder
Singhai et al. Synthesis of ZnO nanoparticles for varistor application using Zn-substituted aerosol OT microemulsion
US4023961A (en) Method of producing powdered materials
CN108098191B (en) Preparation method of copper nanoparticle soldering paste and product thereof
CN110170650B (en) Method for preparing high-compactness and completely-coated silver-coated copper powder
KR20070097055A (en) Conductive ink
EP1475170B1 (en) Chain-structure metal powder, manufacturing method thereof, and conductivity-afforded material
KR20100096111A (en) Copper powder for electrically conductive paste, and electrically conductive paste
KR20150083934A (en) Catalyst for electroless plating, metallic coating film produced using same, and method for producing said metallic coating film
CN101805574A (en) Sintered type conductive adhesive adopting silver filling with surfaces subjected to activating treatment and preparation method thereof
CN103464779A (en) Method for adopting sliver-coated nano copper composite particles to prepare conductive ink
JP4853152B2 (en) Nickel-coated copper fine particles and manufacturing method thereof, dispersion using the same, manufacturing method thereof, and paste using the same
KR20150028970A (en) Silver powder
JP5764279B2 (en) Fine particles for forming fired body, fine particle dispersion solution for forming fired body, method for producing fine particle for forming fired body, and method for producing fine particle dispersion solution for forming fired body
CN1166475C (en) Process for preparing electric silver/graphite contact material by nano technique
CN113257455B (en) Low-temperature-sintered lead-free conductive silver paste
JP2004043892A (en) Fine particle of noble metal and manufacturing method therefor
JP2008121043A5 (en)
CN111069593A (en) High-performance silver-coated copper alloy particle for flexible circuit and preparation method thereof
KR20170139203A (en) With Ag coated Cu powder, Method for Fabricating the same, and paste composition that using the same
CN114639506B (en) Low-temperature fast-sintering conductive copper paste and preparation method thereof
JP2006307330A (en) Silver particulate having high dispersibility, method for producing the same, and its use
JP2017008402A (en) Silver-covered copper based fine particle, method for producing the same, silver-covered copper-based fine particle-dispersed liquid, and method for producing the same
CN115667169A (en) Preparation method of glass powder, silver paste and preparation method
TW201223876A (en) High concentration nano-silver colloid and preparation method for nano-silver colloid precursor

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20200428