CN109439997A - A kind of layer electrodes material of easy-sintering and preparation method thereof - Google Patents

A kind of layer electrodes material of easy-sintering and preparation method thereof Download PDF

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Publication number
CN109439997A
CN109439997A CN201811623022.8A CN201811623022A CN109439997A CN 109439997 A CN109439997 A CN 109439997A CN 201811623022 A CN201811623022 A CN 201811623022A CN 109439997 A CN109439997 A CN 109439997A
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China
Prior art keywords
parts
sintering
easy
layer electrodes
electrodes material
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CN201811623022.8A
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Chinese (zh)
Inventor
汪雪婷
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NANJING SHIHENG ELECTRONICS CO Ltd
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NANJING SHIHENG ELECTRONICS CO Ltd
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Priority to CN201811623022.8A priority Critical patent/CN109439997A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • C22C30/02Alloys containing less than 50% by weight of each constituent containing copper
    • 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
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/103Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor

Abstract

The invention discloses layer electrodes material of a kind of easy-sintering and preparation method thereof, which is made of by weight following raw material: 21~33 parts of copper nanoparticles, 10~15 parts of manganese dioxide, 6~10 parts of cobalt chlorides, 8~13 parts of nickel oxide, 2~5 parts of rubidium oxides, 15~18 parts of binders, 1~3 part of surfactant.The layer electrodes material has the characteristic of excellent electric conductivity and easy-sintering, the sintering character of coating is effectively increased by adding rare earth element, avoid the generation for secretly splitting phenomenon, preparation method carries out final process using inert gas, improve the elasticity of coating, the performance of easy-sintering improves the production efficiency of electrode, to reduce costs indirectly.

Description

A kind of layer electrodes material of easy-sintering and preparation method thereof
Technical field
The invention belongs to electrode material fields, and in particular to a kind of layer electrodes material of easy-sintering and preparation method thereof.
Background technique
Layer electrodes are the technique in electrode surface attachment layer of metal film, and playing prevents metal oxidation (as corroded), are mentioned The effects of high-wearing feature, electric conductivity, reflective, corrosion resistance (copper sulphate etc.) and having improved aesthetic appearance.If layer electrodes are by coating Ingredient can then be divided into the single coat of metal, alloy layer and composite deposite three classes;If classification by use, protective plating can be divided into Layer, protective decorative coating, decorative coating, prosthetic coating, five kinds of functional coating.There is sintering temperature in traditional electrode coating Height is spent, the consumption energy causes the shortcomings that increased production cost.
CN107274960A discloses a kind of inorganic conductive electrode film and preparation method thereof, uses silver powder, ultra-fine mica Powder, bismuth oxide, zinc oxide, antimony oxide, boric acid, aluminium oxide, magnesia, quartz sand, lithium carbonate, basic copper carbonate are original Material, electrode film electric conductivity obtained is excellent, but sintering temperature is higher than technical solution of the present invention.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of layer electrodes material and preparation method thereof of easy-sintering, tool There is the characteristic of excellent electric conductivity and easy-sintering.
What the present invention made to be achieved through the following technical solutions:
A kind of layer electrodes material of easy-sintering, is made of by weight following raw material: 21~33 parts of copper nanoparticles, 10~ 15 parts of manganese dioxide, 6~10 parts of cobalt chlorides, 8~13 parts of nickel oxide, 2~5 parts of rubidium oxides, 15~18 parts of binders, 1~3 part of table Face activating agent.
Preferably, the binder is polyvinyl alcohol or carboxymethyl cellulose.
Preferably, the surfactant is sodium sulfate of polyethenoxy ether of fatty alcohol or fatty alcohol polyoxyethylene ether sulfuric acid Ammonium.
A kind of preparation method of the layer electrodes material of easy-sintering, comprising the following steps:
Binder and deionized water are placed in reconcile in reaction kettle by step 1) to be diluted, and 10~30min of stirring is spare;
Step 2) weighs manganese dioxide, cobalt chloride, nickel oxide, rubidium oxide by weight and is placed in vertical type vacuum sintering furnace, 1200~1500 DEG C of 2~4h of high-temperature calcination are vacuumized, are come out of the stove after being cooled to room temperature, mixing masterbatch is obtained;
Step 2) the mixing masterbatch is placed in ball mill by step 3), be added step 1) it is described containing binder go from Sub- water and copper nanoparticle carry out ball-milling treatment using Ceramic Balls, and 1500~2000r/min high-speed stirred, 2~4h is uniformly mixed;
The mixed slurry handled through step 3) is transferred in de-airing mixer by step 4), and surfactant is added, vacuumizes 200~300r/min stirs 30~60min, is re-filled with inert gas, and 200~300r/min continues 1~2h of stirring, obtains described The layer electrodes material of easy-sintering.
Preferably, the step 4) inert gas is argon gas.
Beneficial effects of the present invention are as follows:
Layer electrodes material of the invention, the characteristic with excellent electric conductivity and easy-sintering pass through addition rare earth member Element effectively increases the sintering character of coating, avoids the generation for secretly splitting phenomenon, and preparation method is carried out most using inert gas Processing eventually, improves the elasticity of coating, the performance of easy-sintering improves the production efficiency of electrode, to reduce costs indirectly.
Specific embodiment
Present invention is further elaborated in following combination specific embodiment.
Embodiment 1
A kind of layer electrodes material of easy-sintering, which is characterized in that be made of by weight following raw material: 21 parts of Nanometer Coppers Powder, 10 parts of manganese dioxide, 6 parts of cobalt chlorides, 8 parts of nickel oxide, 2 parts of rubidium oxides, 15 parts of binders, 1 part of surfactant.
Wherein, the binder uses polyvinyl alcohol, and the surfactant uses sodium sulfate of polyethenoxy ether of fatty alcohol.
Preparation method is as follows:
(1) 15 parts of polyvinyl alcohol and deionized water are placed in reconcile in reaction kettle and are diluted, stirring 10min is spare.
(2) 10 parts of manganese dioxide, 6 parts of cobalt chlorides, 8 parts of nickel oxide, 2 parts of rubidium oxides are weighed by weight is placed in vertical vacuum In sintering furnace, 1200 DEG C of high-temperature calcination 2h are vacuumized, are come out of the stove after being cooled to room temperature, obtains mixing masterbatch.
(3) (2) described mixing masterbatch is placed in ball mill, be added (1) made from deionized water containing binder and 21 parts of copper nanoparticles carry out ball-milling treatment using Ceramic Balls, and 1500r/min high-speed stirred 2h is uniformly mixed.
(4) mixed slurry handled through (3) is transferred in de-airing mixer, 1 part of fatty alcohol polyoxyethylene ether sulfuric acid is added Sodium vacuumizes 200r/min stirring 30min, is re-filled with argon gas, and 200r/min continues to stir 1h, obtains the electrode of the easy-sintering Coating material.
Embodiment 2
A kind of layer electrodes material of easy-sintering, which is characterized in that be made of by weight following raw material: 33 parts of Nanometer Coppers Powder, 15 parts of manganese dioxide, 10 parts of cobalt chlorides, 13 parts of nickel oxide, 5 parts of rubidium oxides, 18 parts of binders, 3 parts of surfactants.
Wherein, the binder uses carboxymethyl cellulose, and the surfactant uses fatty alcohol polyoxyethylene ether sulphur Sour ammonium.
Preparation method is as follows:
(1) 18 parts of carboxymethyl celluloses and deionized water are placed in reconcile in reaction kettle and are diluted, stirring 30min is spare.
(2) weigh by weight 15 parts of manganese dioxide, 10 parts of cobalt chlorides, 13 parts of nickel oxide, 5 parts of rubidium oxides be placed in it is vertical true In empty sintering furnace, 1500 DEG C of high-temperature calcination 4h are vacuumized, are come out of the stove after being cooled to room temperature, obtains mixing masterbatch.
(3) (2) described mixing masterbatch is placed in ball mill, be added (1) made from deionized water containing binder and 33 parts of copper nanoparticles carry out ball-milling treatment using Ceramic Balls, and 2000r/min high-speed stirred 4h is uniformly mixed.
(4) mixed slurry handled through (3) is transferred in de-airing mixer, 3 parts of fatty alcohol polyoxyethylene ether sulfuric acid is added Ammonium vacuumizes 300r/min stirring 1h, is re-filled with argon gas, and 300r/min continues to stir 2h, obtains the electrode plating of the easy-sintering Layer material.
Embodiment 3
A kind of layer electrodes material of easy-sintering, which is characterized in that be made of by weight following raw material: 28 parts of Nanometer Coppers Powder, 12 parts of manganese dioxide, 8 parts of cobalt chlorides, 9 parts of nickel oxide, 3 parts of rubidium oxides, 16 parts of binders, 2 parts of surfactants.
Wherein, the binder uses carboxymethyl cellulose, and the surfactant uses fatty alcohol polyoxyethylene ether sulphur Sour sodium.
Preparation method is as follows:
(1) 16 parts of carboxymethyl celluloses and deionized water are placed in reconcile in reaction kettle and are diluted, stirring 20min is spare.
(2) 12 parts of manganese dioxide, 8 parts of cobalt chlorides, 9 parts of nickel oxide, 3 parts of rubidium oxides are weighed by weight is placed in vertical vacuum In sintering furnace, 1300 DEG C of high-temperature calcination 3h are vacuumized, are come out of the stove after being cooled to room temperature, obtains mixing masterbatch.
(3) (2) described mixing masterbatch is placed in ball mill, be added (1) made from deionized water containing binder and 28 parts of copper nanoparticles carry out ball-milling treatment using Ceramic Balls, and 1800r/min high-speed stirred 3h is uniformly mixed.
(4) mixed slurry handled through (3) is transferred in de-airing mixer, 2 parts of fatty alcohol polyoxyethylene ether sulfuric acid is added Sodium vacuumizes 250r/min stirring 40min, is re-filled with argon gas, and 250r/min continues to stir 1.5h, obtains the electricity of the easy-sintering Pole coating material.
Comparative example 1 (rare earth element is not added)
A kind of layer electrodes material of easy-sintering, which is characterized in that be made of by weight following raw material: 21 parts of Nanometer Coppers Powder, 10 parts of manganese dioxide, 6 parts of cobalt chlorides, 8 parts of nickel oxide, 15 parts of binders, 1 part of surfactant.
Wherein, the binder uses polyvinyl alcohol, and the surfactant uses sodium sulfate of polyethenoxy ether of fatty alcohol.
Preparation method is as follows:
(1) 15 parts of polyvinyl alcohol and deionized water are placed in reconcile in reaction kettle and are diluted, stirring 10min is spare.
(2) 10 parts of manganese dioxide, 6 parts of cobalt chlorides, 8 parts of nickel oxide are weighed by weight to be placed in vertical type vacuum sintering furnace, 1200 DEG C of high-temperature calcination 2h are vacuumized, are come out of the stove after being cooled to room temperature, mixing masterbatch is obtained.
(3) (2) described mixing masterbatch is placed in ball mill, be added (1) made from deionized water containing binder and 21 parts of copper nanoparticles carry out ball-milling treatment using Ceramic Balls, and 1500r/min high-speed stirred 2h is uniformly mixed.
(4) mixed slurry handled through (3) is transferred in de-airing mixer, 1 part of fatty alcohol polyoxyethylene ether sulfuric acid is added Sodium vacuumizes 200r/min stirring 30min, is re-filled with argon gas, and 200r/min continues to stir 1h, obtains layer electrodes material.
Comparative example 2 (is not filled with inert gas)
A kind of layer electrodes material of easy-sintering, which is characterized in that be made of by weight following raw material: 21 parts of Nanometer Coppers Powder, 10 parts of manganese dioxide, 6 parts of cobalt chlorides, 8 parts of nickel oxide, 2 parts of rubidium oxides, 15 parts of binders, 1 part of surfactant.
Wherein, the binder uses polyvinyl alcohol, and the surfactant uses sodium sulfate of polyethenoxy ether of fatty alcohol.
Preparation method is as follows:
(1) 15 parts of polyvinyl alcohol and deionized water are placed in reconcile in reaction kettle and are diluted, stirring 10min is spare.
(2) 10 parts of manganese dioxide, 6 parts of cobalt chlorides, 8 parts of nickel oxide, 2 parts of rubidium oxides are weighed by weight is placed in vertical vacuum In sintering furnace, 1200 DEG C of high-temperature calcination 2h are vacuumized, are come out of the stove after being cooled to room temperature, obtains mixing masterbatch.
(3) (2) described mixing masterbatch is placed in ball mill, be added (1) made from deionized water containing binder and 21 parts of copper nanoparticles carry out ball-milling treatment using Ceramic Balls, and 1500r/min high-speed stirred 2h is uniformly mixed.
(4) mixed slurry handled through (3) is transferred in de-airing mixer, 1~3 part of fatty alcohol polyoxyethylene ether sulphur is added Sour sodium vacuumizes 200r/min stirring 30min, obtains layer electrodes material.
Test case 1
Layer electrodes material made from Examples 1 to 3 and comparative example 1~2 is coated on common copper electrode, electrode is set In vertical type vacuum sintering furnace, 1~2h of high-temperature calcination is vacuumized, the copper electrode with layer electrodes is made.Respectively to each copper Electrode is tested for the property, test result is as follows table 1.
1 the performance test results of table
1 data of consolidated statement, it can be deduced that, addition rare earth element can be obviously improved the sintering character of layer electrodes, and lazy Property atmosphere addition can effectively improve the elasticity of coating, which has excellent electric conductivity, the spy of easy-sintering Property can effectively improve the production efficiency of electrode, to reduce costs indirectly.

Claims (5)

1. a kind of layer electrodes material of easy-sintering, which is characterized in that be made of by weight following raw material: 21~33 parts of nanometers Copper powder, 10~15 parts of manganese dioxide, 6~10 parts of cobalt chlorides, 8~13 parts of nickel oxide, 2~5 parts of rubidium oxides, 15~18 parts of bondings Agent, 1~3 part of surfactant.
2. a kind of layer electrodes material of easy-sintering according to claim 1, which is characterized in that the binder is poly- second Enol or carboxymethyl cellulose.
3. a kind of layer electrodes material of easy-sintering according to claim 1, which is characterized in that the surfactant is Sodium sulfate of polyethenoxy ether of fatty alcohol or fatty alcohol polyoxyethylene ether ammonium sulfate.
4. a kind of preparation method of the layer electrodes material of easy-sintering described in claim 1, which is characterized in that including following step It is rapid:
Binder and deionized water are placed in reconcile in reaction kettle by step 1) to be diluted, and 10~30min of stirring is spare;
Step 2) weighs manganese dioxide, cobalt chloride, nickel oxide, rubidium oxide by weight and is placed in vertical type vacuum sintering furnace, takes out true 1200~1500 DEG C of 2~4h of high-temperature calcination of sky, come out of the stove after being cooled to room temperature, and obtain mixing masterbatch;Step 3) will be described in step 2) Mixing masterbatch is placed in ball mill, deionized water and copper nanoparticle containing binder described in step 1) is added, using Ceramic Balls Ball-milling treatment is carried out, 1500~2000r/min high-speed stirred, 2~4h is uniformly mixed;
The mixed slurry handled through step 3) is transferred in de-airing mixer by step 4), and surfactant is added, vacuumize 200~ 300r/min stirs 30~60min, is re-filled with inert gas, 200~300r/min continues 1~2h of stirring, obtains the easy burning The layer electrodes material of knot.
5. a kind of preparation method of the layer electrodes material of easy-sintering according to claim 4, which is characterized in that step 4) The inert gas is argon gas.
CN201811623022.8A 2018-12-28 2018-12-28 A kind of layer electrodes material of easy-sintering and preparation method thereof Pending CN109439997A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103878346A (en) * 2014-03-12 2014-06-25 昆明理工大学 Preparing method of ceramic particle multi-scale enhanced metallic matrix composite materials
CN104425121A (en) * 2013-08-27 2015-03-18 三积瑞科技(苏州)有限公司 Embedded alloy inductor fabrication method
CN106024101A (en) * 2016-08-05 2016-10-12 代长华 Composite conducive ceramic slurry and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104425121A (en) * 2013-08-27 2015-03-18 三积瑞科技(苏州)有限公司 Embedded alloy inductor fabrication method
CN103878346A (en) * 2014-03-12 2014-06-25 昆明理工大学 Preparing method of ceramic particle multi-scale enhanced metallic matrix composite materials
CN106024101A (en) * 2016-08-05 2016-10-12 代长华 Composite conducive ceramic slurry and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
仝兴存: "《电子封装热管理先进材料》", 30 April 2016 *
唐代明: "《金属材料学》", 30 June 2014 *

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Application publication date: 20190308