CN106531348A - Nano silver paste preparation method - Google Patents

Nano silver paste preparation method Download PDF

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Publication number
CN106531348A
CN106531348A CN201610877125.1A CN201610877125A CN106531348A CN 106531348 A CN106531348 A CN 106531348A CN 201610877125 A CN201610877125 A CN 201610877125A CN 106531348 A CN106531348 A CN 106531348A
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CN
China
Prior art keywords
silver
nano
preparation
silver paste
glass powder
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Pending
Application number
CN201610877125.1A
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Chinese (zh)
Inventor
潘中海
司荣美
刘彩风
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Tianjin Baoxingwei Technology Co Ltd
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Tianjin Baoxingwei Technology Co Ltd
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Priority to CN201610877125.1A priority Critical patent/CN106531348A/en
Publication of CN106531348A publication Critical patent/CN106531348A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a nano silver paste preparation method. The method comprises the following steps: 0.15 g of silver nanowires and 50 g of boron aluminum titanium silicate glass powder are mixed in 3 to 1000, and a ball mill is used for mixing; the silver nanowires and the boron aluminum titanium silicate glass powder which are well mixed are put in a drying box for drying and set aside for use; 1 g of polyvinylpyrrolidone is completely dissolved in 80g of tributyl citrate, 4g of a leveling agent and 3 g of a defoamer are added for uniform dispersion, and a mixture is obtained; the silver nanowires and the boron aluminum titanium silicate glass powder which are dried are added to the mixture, and after complete stirring, a nano silver paste is obtained. According to the nano silver paste preparation method provided by the invention, through adopting the silver nanowires, the electrical conductivity and the thermal conductivity can be effectively improved, the curing temperature is reduced, the silver dosage is reduced, and the production cost is greatly reduced.

Description

A kind of preparation method of nanometer silver paste
Technical field
A kind of a kind of the present invention relates to electric slurry production technical field, more particularly to preparation method of nanometer silver paste.
Background technology
Silver conductive paste is widely used in conductor paste, silver powder as the solid shape of its particle of conductor paste, size, The factors such as size distribution directly affect conduction, thermal conductivity, and current silver conductive paste mainly adopts micron or submicron silver powder, this The conduction of a little slurries, poor thermal conductivity, solidification temperature are high, and silver-colored consumption is big, can not meet the requirement of new technology.
The content of the invention
Present invention seek to address that the deficiencies in the prior art, and a kind of preparation method of nanometer silver paste is provided.
The present invention for achieving the above object, is employed the following technical solutions:A kind of preparation method of nanometer silver paste, its feature exist In comprising the following steps:
(1) nano-silver thread of 0.15g and 50g boron manosil AS titanium glass powder are pressed into 3:1000 mixing, and it is mixed with ball mill 10-12h is closed, drum's speed of rotation is set to 28-36r/min;
(2) nano-silver thread and boron manosil AS titanium glass powder that mix in step (1) are put in drying box and are done Dry, baking temperature is 35-90 DEG C, and drying time is 3-4h, stand-by;
(3) 1g polyvinylpyrrolidones are substantially dissolved in 80g ATBCs, and add 4g levelling agents, 3g to disappear Infusion, and the sonic oscillation dispersion 15min in ultrasonic washing instrument so as to be uniformly dispersed, obtain mixture;
(4) dried nano-silver thread in step (2) and boron manosil AS titanium glass powder is added and mix obtained by step (4) In thing, it is sufficiently stirred for obtaining nanometer silver paste.
Particularly, the nano-silver thread in step (1) is obtained as follows:2g silver nitrate powders are weighed, in ultrasound It is dissolved in the ethylene glycol of 50mL under ripple auxiliary, obtains silver nitrate solution, places standby, then weigh 0.5g polyvinylpyrrolidines Ketone, is uniformly mixed in being slowly dissolved in the ethylene glycol of 50mL, places standby, by the silver nitrate solution for preparing in magnetic agitation Under be added drop-wise to gained mixed liquor in, control constant agitation speed and reaction temperature until reaction terminate, obtain nano silver colloidal sol, most Afterwards obtained nano silver colloidal sol is centrifuged, rotating speed is 9000r/min, after resulting precipitation is washed with ethanol, It is put into 40 DEG C of vacuum drying chambers and is dried 40min, obtains nano-silver thread.
Particularly, the levelling agent in step (3) refers to organic silicone oil.
Particularly, the defoamer in step (3) refers to the one kind or several in polysiloxanes, calcium carbonate or tricalcium phosphate Kind.
The invention has the beneficial effects as follows:The present invention provides a kind of preparation method of nanometer silver paste, by adopting nano-silver thread, Conduction and thermal conductivity is not only effectively increased, while reducing solidification temperature, and silver-colored consumption is reduced, is greatly reduced production Cost.
Specific embodiment
With reference to embodiment, the invention will be further described:
Embodiment 1
A kind of preparation method of nanometer silver paste, comprises the following steps:
(1) nano-silver thread of 0.15g and 50g boron manosil AS titanium glass powder are pressed into 3:1000 mixing, and it is mixed with ball mill 10h is closed, drum's speed of rotation is set to 28r/min;
(2) nano-silver thread and boron manosil AS titanium glass powder that mix in step (1) are put in drying box and are done Dry, baking temperature is 35 DEG C, and drying time is 4h, stand-by;
(3) 1g polyvinylpyrrolidones are substantially dissolved in 80g ATBCs, and add 4g organic silicone oils, 3g Polysiloxanes, and the sonic oscillation dispersion 15min in ultrasonic washing instrument so as to be uniformly dispersed, obtain mixture;
(4) dried nano-silver thread in step (2) and boron manosil AS titanium glass powder is added and mix obtained by step (4) In thing, it is sufficiently stirred for obtaining nanometer silver paste.
Nano-silver thread in step (1) is obtained as follows:2g silver nitrate powders are weighed, under ultrasonic assistant It is dissolved in the ethylene glycol of 50mL, obtains silver nitrate solution, places standby, then weigh 0.5g polyvinylpyrrolidones, it is slowly molten Solution is uniformly mixed in the ethylene glycol of 50mL, places standby, the silver nitrate solution of preparation is added drop-wise under magnetic stirring In gained mixed liquor, constant agitation speed and reaction temperature is controlled until reaction terminates, obtain nano silver colloidal sol, will be finally obtained Nano silver colloidal sol be centrifuged, rotating speed is 9000r/min, after resulting precipitation is washed with ethanol, is put into 40 DEG C Vacuum drying chamber is dried 40min, obtains nano-silver thread.
Embodiment 2
A kind of preparation method of nanometer silver paste, comprises the following steps:
(1) nano-silver thread of 0.15g and 50g boron manosil AS titanium glass powder are pressed into 3:1000 mixing, and it is mixed with ball mill 12h is closed, drum's speed of rotation is set to 36r/min;
(2) nano-silver thread and boron manosil AS titanium glass powder that mix in step (1) are put in drying box and are done Dry, baking temperature is 90 DEG C, and drying time is 3h, stand-by;
(3) 1g polyvinylpyrrolidones are substantially dissolved in 80g ATBCs, and add 4g organic silicone oils, 3g Calcium carbonate, and the sonic oscillation dispersion 15min in ultrasonic washing instrument so as to be uniformly dispersed, obtain mixture;
(4) dried nano-silver thread in step (2) and boron manosil AS titanium glass powder is added and mix obtained by step (4) In thing, it is sufficiently stirred for obtaining nanometer silver paste.
Nano-silver thread in step (1) is obtained as follows:2g silver nitrate powders are weighed, under ultrasonic assistant It is dissolved in the ethylene glycol of 50mL, obtains silver nitrate solution, places standby, then weigh 0.5g polyvinylpyrrolidones, it is slowly molten Solution is uniformly mixed in the ethylene glycol of 50mL, places standby, the silver nitrate solution of preparation is added drop-wise under magnetic stirring In gained mixed liquor, constant agitation speed and reaction temperature is controlled until reaction terminates, obtain nano silver colloidal sol, will be finally obtained Nano silver colloidal sol be centrifuged, rotating speed is 9000r/min, after resulting precipitation is washed with ethanol, is put into 40 DEG C Vacuum drying chamber is dried 40min, obtains nano-silver thread.
Above the present invention is exemplarily described, it is clear that the present invention is implemented and is not subject to the restrictions described above, As long as employing method of the present invention design and the various improvement that carry out of technical scheme, or not improved directly apply to other fields Close, within protection scope of the present invention.

Claims (4)

1. a kind of preparation method of nanometer silver paste, it is characterised in that comprise the following steps:
(1) nano-silver thread of 0.15g and 50g boron manosil AS titanium glass powder are pressed into 3:1000 mixing, and with ball mill mixing 10- 12h, drum's speed of rotation are set to 28-36r/min;
(2) nano-silver thread and boron manosil AS titanium glass powder that mix in step (1) are put in drying box and are dried, done Dry temperature is 35-90 DEG C, and drying time is 3-4h, stand-by;
(3) 1g polyvinylpyrrolidones are substantially dissolved in 80g ATBCs, and add 4g levelling agents, 3g defoamers, And sonic oscillation disperses 15min in ultrasonic washing instrument so as to be uniformly dispersed, obtain mixture;
(4) dried nano-silver thread in step (2) and boron manosil AS titanium glass powder are added into mixture obtained by step (4) In, it is sufficiently stirred for obtaining nanometer silver paste.
2. a kind of preparation method of nanometer silver paste according to claim 1, it is characterised in that receiving in step (1) Rice silver wire is obtained as follows:2g silver nitrate powders are weighed, is dissolved under ultrasonic assistant in the ethylene glycol of 50mL, is obtained Silver nitrate solution, places standby, then weighs 0.5g polyvinylpyrrolidones, is slowly dissolved in stirring mixing in the ethylene glycol of 50mL Uniformly, place standby, the silver nitrate solution of preparation is added drop-wise in gained mixed liquor under magnetic stirring, control constant agitation speed Degree and reaction temperature terminate until reaction, obtain nano silver colloidal sol, are finally centrifuged obtained nano silver colloidal sol, turn Speed is 9000r/min, after resulting precipitation is washed with ethanol, is put into 40 DEG C of vacuum drying chambers and is dried 40min, obtain Nano-silver thread.
3. a kind of preparation method of nanometer silver paste according to claim 1, it is characterised in that the stream in step (3) Flat agent refers to organic silicone oil.
4. a kind of preparation method of nanometer silver paste according to claim 1, it is characterised in that disappearing in step (3) Infusion refers to one or more in polysiloxanes, calcium carbonate or tricalcium phosphate.
CN201610877125.1A 2016-09-30 2016-09-30 Nano silver paste preparation method Pending CN106531348A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112719284A (en) * 2020-12-18 2021-04-30 天津宝兴威科技股份有限公司 Preparation method of nano silver wire for flexible touch material
CN114049981A (en) * 2021-11-30 2022-02-15 重庆英诺维节能环保科技有限公司 Silver-tin nano material conductive silver paste and application thereof to vacuum glass

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1740405A (en) * 2005-09-23 2006-03-01 浙江大学 Silver nanometer wire synthesizing process
CN101310899A (en) * 2008-03-18 2008-11-26 江苏工业学院 Method for preparing silver nano-wire in large batch
CN101582328A (en) * 2009-06-26 2009-11-18 彩虹集团公司 Nanometer silver paste for terminal electrode of multi-layer ceramic capacitor and method for preparing same
CN103170645A (en) * 2013-03-27 2013-06-26 中国科学院深圳先进技术研究院 Preparation method of silver nanowires
CN104464887A (en) * 2014-11-17 2015-03-25 苏州斯迪克新材料科技股份有限公司 Nanometer silver wire conductive silver paste and preparing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1740405A (en) * 2005-09-23 2006-03-01 浙江大学 Silver nanometer wire synthesizing process
CN101310899A (en) * 2008-03-18 2008-11-26 江苏工业学院 Method for preparing silver nano-wire in large batch
CN101582328A (en) * 2009-06-26 2009-11-18 彩虹集团公司 Nanometer silver paste for terminal electrode of multi-layer ceramic capacitor and method for preparing same
CN103170645A (en) * 2013-03-27 2013-06-26 中国科学院深圳先进技术研究院 Preparation method of silver nanowires
CN104464887A (en) * 2014-11-17 2015-03-25 苏州斯迪克新材料科技股份有限公司 Nanometer silver wire conductive silver paste and preparing method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112719284A (en) * 2020-12-18 2021-04-30 天津宝兴威科技股份有限公司 Preparation method of nano silver wire for flexible touch material
CN114049981A (en) * 2021-11-30 2022-02-15 重庆英诺维节能环保科技有限公司 Silver-tin nano material conductive silver paste and application thereof to vacuum glass
CN114049981B (en) * 2021-11-30 2024-03-15 四川英诺维新材料科技有限公司 Silver tin nano material conductive silver paste and application thereof to vacuum glass

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Application publication date: 20170322