CN106041352A - Silver nano-particle coated by organic acid silver, method for preparing silver nano-particle and application thereof - Google Patents
Silver nano-particle coated by organic acid silver, method for preparing silver nano-particle and application thereof Download PDFInfo
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- CN106041352A CN106041352A CN201610686226.0A CN201610686226A CN106041352A CN 106041352 A CN106041352 A CN 106041352A CN 201610686226 A CN201610686226 A CN 201610686226A CN 106041352 A CN106041352 A CN 106041352A
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- organic acid
- silver
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- acid silver
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- 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 discloses a silver nano-particle coated by organic acid silver, a method for preparing the silver nano-particle and application thereof. The silver nano-particle coated by the organic acid silver is characterized in that the silver nano-particle is coated by the organic acid silver, the average particle sizes of coated particles range from 6 nm to 12 nm, and the coated particles are uniformly dispersed. The method for preparing the silver nano-particle coated by the organic acid silver includes (1), mixing NaOH, organic acid and deionized water with one another to obtain first mixtures, heating the mixtures until the temperature of the first mixtures reaches a certain temperature, immediately adding silver nitrate into the first mixtures, stirring the silver nitrate and the first mixtures to obtain second mixtures, allowing the second mixtures to stand still, layering the second mixtures and acquiring upper-layer white waxy substances; (2), centrifuging, washing and drying the white substances obtained at the step (1), then heating the white substances in nitrogen until the temperature of the white substances reaches 220-280 DEG C and preserving heat for 80-100 min to obtain the silver nano-particle coated by the organic acid silver. The silver nano-particle, the method and the application have the advantages that the method is easy to implement and low in cost, is safe and reliable and has a broad industrial application prospect, and the prepared silver nano-particle coated by the organic acid silver can be used as brazing filler metal for electronic packaging.
Description
Technical field
The invention belongs to field of nanometer material technology, be particularly related to a kind of organic acid silver cladding nano-Ag particles and preparation side thereof
Method and application, nano-Ag particles prepared by the method by Coated with Organic Matter to avoid the reunion of nano-particle, can be directly as pricker
Material is applied to Electronic Packaging field.
Background technology
In microelectronics industry, leaded solder due to have disposable, wettability is good and the advantage such as cheap once
Through being widely deployed.But, lead and compound thereof are noxious substances, and environment and the mankind can be worked the mischief by life-time service, institute
Gradually prohibitted the use of by every country with solder containing pb.Currently used relatively broad lead-free brazing have Sn-Bi, Sn-Ag-Cu and
Sn-Cu etc., these solders have low-melting feature.But, when electronic package material needs high temperature resistant, this kind of solder is with regard to nothing
Method meets needs.Silver has higher electrical conductivity, thermal conductivity and thermal fatigue resistance, additionally, silver point higher (960 DEG C),
Therefore silver is appropriate high temperature resistant electronic package material.When the size reduction of Argent grain is to Nano grade, owing to size is imitated
Its fusing point should be caused to significantly reduce, and therefore nanometer silver can reach to connect temperature relatively low as solder for Electronic Packaging field,
And use the purpose that temperature is higher.
Nanometer silver preparation method is more, including liquid chemical method, ionizing radiation reduction, laser ablation, vacuum evaporation and light
Electrochemical reducings etc., liquid chemical method has the advantages such as with low cost and technique is simple compared with additive method.Cao Yang et al.
Solution phase chemical reduction is used to prepare the nano-Ag particles that mean diameter is 20～30nm；Zou Guisheng et al. uses liquid phase equally
Chemical reduction method, prepares the mean diameter nano-Ag particles as 40nm with PVP and silver nitrate for raw material.Due to nano-particle table
Face can be higher, and agglomeration easily occurs, and therefore, prepares good dispersion and the little Coated with Organic Matter nanometer silver solder of size is electricity
One of key technology of sub-encapsulation field.
Summary of the invention
For the problem that reunion involved during liquid chemical method prepares nanometer silver in prior art and particle diameter are bigger, this
Bright purpose is to provide a kind of organic acid silver cladding nano-Ag particles and its preparation method and application.The organic acid that the present invention prepares
Dispersed nano-silver particles is good, do not reunite, particle diameter is less for silver cladding, can be directly as solder for Electronic Packaging.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of organic acid silver cladding nano-Ag particles, it is characterised in that described nano-Ag particles is coated with by organic acid silver, quilt
The mean particle size of cladding is 6～12nm, and is uniformly dispersed.The structural representation of described organic acid silver cladding nano-Ag particles
As shown in Figure 1.
By such scheme, it is preferable that described organic acid silver is lauric acid silver or ascorbic acid silver.
The preparation method of a kind of organic acid silver cladding nano-Ag particles, it is characterised in that comprise the following steps:
(1) NaOH, organic acid and deionized water are mixed, be heated to uniform temperature, add silver nitrate immediately, stirring, quiet
Put layering, take the waxy substance of upper strata white；
(2) by whiteness centrifuge washing in above-mentioned steps (1), dry, in nitrogen, be then heated to 220～280 DEG C,
Insulation 80～100min, prepares organic acid silver cladding nano-Ag particles.
By such scheme, it is preferable that the mol ratio of described NaOH, organic acid, deionized water and silver nitrate is: 1:1～
1.1:2000～2500:1～2.
By such scheme, it is preferable that described organic acid is lauric acid or ascorbic acid.
By such scheme, it is preferable that described in step (1), heating-up temperature is 75～85 DEG C.
By such scheme, it is preferable that described in step (1), mixing time is 1.5h.
By such scheme, it is preferable that centrifuge washing described in step (2) is particularly as follows: at the centrifugal rotational speed of 7000r/min
Under, to wash respectively for several times with deionized water and ethanol, each wash time is 10min, it is therefore an objective to go the removal of impurity.
By such scheme, it is preferable that drying temperature described in step (2) is 70～80 DEG C, and the time is 6～8h.
The present invention also provides for above-mentioned organic acid silver cladding nano-Ag particles as the solder application in Electronic Packaging field.
The ultimate principle of the present invention is as follows:
First pass through liquid chemical method and first prepare organic acid silver, then obtain organic acid silver cladding by the decomposition of organic acid silver and receive
Rice Argent grain.Due to the organic acid active aldehyde radical of silver, reproducibility aldehyde radical can be as the reduction of metal ion and metal cluster
The place of nucleation；Organic acid silver has long linear molecular structure, and intermolecular and intramolecular hydrogen bond effect defines molecular level
On separate space, the growth for nanoparticle provides good template, and this template hinders granule and grows up further, plays
Cladding nano-Ag particles also prevents its effect reunited.
Compared to prior art, the beneficial effects of the present invention is:
(1) the organic acid silver cladding dispersed nano-silver particles obtained by the present invention is uniform, soilless sticking phenomenon；
(2) the organic acid silver cladding nano-Ag particles size obtained by the present invention is little, and mean diameter only has 6～12nm,
There is under room temperature good stability；
(3) preparation method of the present invention is simple to operate, safe and reliable, with low cost, it is easy to implementing, prospects for commercial application is wide
Wealthy.
Accompanying drawing explanation
Fig. 1 is the structural representation of organic acid silver of the present invention cladding nano-Ag particles.
Fig. 2 is the lauric acid silver cladding nano-Ag particles TEM figure that embodiment 1 uses prepared by lauric acid.
Fig. 3 is the ascorbic acid silver cladding nano-Ag particles TEM figure that embodiment 2 uses prepared by ascorbic acid.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
Use lauric acid etc. to prepare organic acid silver cladding nano-Ag particles for raw material, specifically comprise the following steps that
(1) by lauric acid and the deionized water mixing of 600ml of NaOH, 0.016mol of 0.015mol, and it is heated to 80
DEG C, adding the silver nitrate of 0.015mol immediately, after stirring 1.5h, be layered after standing, the waxy substance taking out upper strata white i.e. wraps
Lauric acid silver containing a small amount of impurity；
(2) by White waxy material deionized water in above-mentioned steps (1) and ethanol eccentric cleaning 3 times, 1 time respectively, from
Heart speed is 7000r/min, and each scavenging period is 10min, it is therefore an objective to go the removal of impurity；Then being baked to, temperature is 80 DEG C,
Drying time is 6h；Finally, nitrogen is heated to 250 DEG C, is incubated 90min, obtain powder lauric acid silver cladding nanometer silver
Grain.
Fig. 2 is the TEM photo of the lauric acid silver cladding nano-Ag particles that the present embodiment prepares.Can be seen that nano-Ag particles
Being uniformly dispersed, soilless sticking phenomenon, particle diameter is less, and mean diameter is about 6.5nm.
Embodiment 2
Use ascorbic acid etc. to prepare organic acid silver cladding nano-Ag particles for raw material, specifically comprise the following steps that
(1) by ascorbic acid and the deionized water mixing of 550ml of NaOH, 0.015mol of 0.014mol, and it is heated to
80 DEG C, adding the silver nitrate of 0.02mol immediately, after stirring 1.5h, be layered after standing, the waxy substance taking upper strata white i.e. comprises
The ascorbic acid silver of a small amount of impurity；
(2) by White waxy material deionized water in above-mentioned steps (1) and ethanol eccentric cleaning 4 times, 1 time respectively, from
Heart speed is 7000r/min, and each scavenging period is 10min, it is therefore an objective to go the removal of impurity；Then being baked to, temperature is 75 DEG C,
Drying time is 8h；Finally, nitrogen is heated to 230 DEG C, is incubated 100min, obtain powder ascorbic acid silver cladding nanometer silver
Granule.
Fig. 3 is the TEM photo of the ascorbic acid silver cladding nano-Ag particles that the present embodiment prepares.Receive as can be seen from this figure
Rice Argent grain is uniformly dispersed, and soilless sticking phenomenon, particle diameter is little, and mean diameter is about 11.7nm.
Claims (10)
1. an organic acid silver cladding nano-Ag particles, it is characterised in that described nano-Ag particles is coated with by organic acid silver, is wrapped
The mean particle size covered is 6～12nm, and is uniformly dispersed.
Organic acid silver the most according to claim 1 cladding nano-Ag particles, it is characterised in that described organic acid silver is Laurel
Acid silver or ascorbic acid silver.
3. the preparation method of an organic acid silver cladding nano-Ag particles, it is characterised in that comprise the following steps:
(1) NaOH, organic acid and deionized water are mixed, be heated to uniform temperature, add silver nitrate immediately, stirring, stand and divide
Layer, takes the waxy substance of upper strata white；
(2) by whiteness centrifuge washing in above-mentioned steps (1), dry, in nitrogen, be then heated to 220～280 DEG C, insulation
80～100min, prepare organic acid silver cladding nano-Ag particles.
The preparation method of organic acid silver the most according to claim 3 cladding nano-Ag particles, it is characterised in that described
The mol ratio of NaOH, organic acid, deionized water and silver nitrate is: 1:1～1.1:2000～2500:1～2.
The preparation method of organic acid silver the most according to claim 3 cladding nano-Ag particles, it is characterised in that described organic
Acid is lauric acid or ascorbic acid.
The preparation method of organic acid silver the most according to claim 3 cladding nano-Ag particles, it is characterised in that step (1)
Described in heating-up temperature be 75～85 DEG C.
The preparation method of organic acid silver the most according to claim 3 cladding nano-Ag particles, it is characterised in that step (1)
Described in mixing time be 1.5h.
The preparation method of organic acid silver the most according to claim 3 cladding nano-Ag particles, it is characterised in that step (2)
Described in centrifuge washing particularly as follows: under the centrifugal rotational speed of 7000r/min, wash respectively for several times, often with deionized water and ethanol
Secondary wash time is 10min.
The preparation method of organic acid silver the most according to claim 3 cladding nano-Ag particles, it is characterised in that step (2)
Described in dry temperature be 70～80 DEG C, the time is 6～8h.
10. the cladding of organic acid silver described in claim 1 or 2 nano-Ag particles is as the solder application in Electronic Packaging field.
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Cited By (4)
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| CN107282918A (en) * | 2017-05-17 | 2017-10-24 | 宁波大学 | A kind of Silver nanorod/polymer/silver nanometer sheet core-shell nano material and its preparation method and application |
| CN107511602A (en) * | 2017-08-14 | 2017-12-26 | 武汉工程大学 | A kind of nanometer Ag Cu soldering paste and preparation method and application |
| CN111812163A (en) * | 2020-06-23 | 2020-10-23 | 武汉工程大学 | Semiconductor resistor type ethanol gas sensor and preparation method thereof |
| CN113385688A (en) * | 2021-05-27 | 2021-09-14 | 湖南诺尔得材料科技有限公司 | Preparation method and application of silver powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN107511602A (en) * | 2017-08-14 | 2017-12-26 | 武汉工程大学 | A kind of nanometer Ag Cu soldering paste and preparation method and application |
| CN111812163A (en) * | 2020-06-23 | 2020-10-23 | 武汉工程大学 | Semiconductor resistor type ethanol gas sensor and preparation method thereof |
| CN111812163B (en) * | 2020-06-23 | 2022-11-29 | 武汉工程大学 | Semiconductor resistor type ethanol gas sensor and preparation method thereof |
| CN113385688A (en) * | 2021-05-27 | 2021-09-14 | 湖南诺尔得材料科技有限公司 | Preparation method and application of silver powder |
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