CN105364082A - Method for preparing silver powder through radiation reduction - Google Patents
Method for preparing silver powder through radiation reduction Download PDFInfo
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- CN105364082A CN105364082A CN201410406488.8A CN201410406488A CN105364082A CN 105364082 A CN105364082 A CN 105364082A CN 201410406488 A CN201410406488 A CN 201410406488A CN 105364082 A CN105364082 A CN 105364082A
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Abstract
The invention discloses a method for preparing silver powder through radiation reduction. The method includes the following steps that 1%-40% of a silver source without nitrate, 0-1% of a dispersing agent, 0.1%-10% of an active particle collection agent, 0-1% of ammonia water with the weight concentration being 28% and 40%-96% of deionized water are stirred and mixed, and are put into a radiation source under the inert gas atmosphere so as to be subjected to a radiation reduction reaction while being stirred; and then the silver powder is collected from a reaction product. The method has the beneficial effects that the content of impurities of the silver powder product is low, the silver powder product can be directly applied without separating the impurities or can be applied after being slightly cleaned and then concentrated or dried, cleanliness and environment friendliness are achieved, and cost is low; and the method plays a great promoting role in the development of electronic devices and products.
Description
Technical field
The present invention relates to the method preparing silver powder.
Background technology
Most widely used a kind of Precious Metal in electronics industry containing silver electronic paste.As the silver powder of key component containing silver electronic paste, industrially substantially to be obtained by chemical reduction method at present.[publication number CN1227148A] discloses a kind of formates that utilizes for reducing agent and special nozzle mixed nitrate silvery are for the method for silver powder; [publication number CN101462164A] discloses a kind of method utilizing hydrazine hydrate and ascorbic acid reduction silver nitrate to prepare high tap density silver powder; [publication number CN1709618A] discloses a kind of method preparing nanometer, sub-micron and silver powder; [publication number CN101347841A] discloses a kind of preparation method utilizing tipping prepared sizes high tap density silver powder with controllable; [publication number CN101569937A] discloses a kind of method liquor argenti nitratis ophthalmicus and reducing agent being added hyper-dispersant solution simultaneously and prepare silver powder.[publication number CN1387968A] discloses a kind of method by regulating liquor argenti nitratis ophthalmicus pH value to prepare silver powder.These methods are prepared in the technical process of silver powder all must use chemical reducing agent, and this increases cost on the one hand, also brings environmental issue on the other hand.In addition, aforementioned production method can cause generating the by-product impurities such as nitrate anion in product, brings difficulty to separating-purifying, also can produce the discharge of a large amount of waste water.
[Chinese patent ZL201110008831.X] discloses one and utilizes in aqueous
60the method of the easy dispersible silver powder of ball-type narrow ditribution is prepared in the reduction of Co-gamma-ray irradiation, the method does not use chemical reducing agent, decrease the use of chemicals, favourable to environmental protection, but, a weak point existing for this patent is, preparation method still use silver nitrate the same as chemical method is " silver-colored source ", there is nitrate anion by-product impurities problem.
Document [radiation research and radiation process journal, 2004,02:69-72] reports a kind of method utilizing high energy electron beams reduction silver nitrate to prepare silver powder, and the method does not equally need to use chemical reducing agent yet, but there is nitrate anion by-product impurities problem.
Summary of the invention
The object of this invention is to provide a kind of method that radiation reduction prepares silver powder, to overcome the defect that prior art exists.
Method of the present invention, comprises the steps:
By " silver-colored source " 1-40% not containing nitrate anion, dispersant 0-1%, active particle agent for capturing 0.1-10%, weight concentration is ammoniacal liquor 0-1% and the deionized water 40-96% of 28%, is uniformly mixed, under inert gas atmosphere, be placed in radiation source, carry out radiation reduction reaction under agitation; Then from product, described silver powder is collected;
Described not containing " the silver-colored source " of nitrate anion be selected from include but not limited in citric acid three silver medal, silver oxalate, silver acetate, silver formate, silver carbonate, silver oxide, silver tartrate one or more, " silver-colored source " principal character is not containing nitrate anion;
Described dispersant be selected from PVP (PVP), gelatin, polyvinyl alcohol (PVA), lauryl sodium sulfate or PEO (PEO) etc. more than one;
Described active particle agent for capturing be selected from isopropyl alcohol, ethanol, methyl alcohol, acetone, formic acid ammonia, triethanolamine, triethylene tetramine or five ethene hexamines one or more;
Described radiation source be cobalt-60 (
60co) gamma-ray radiation source or electron accelerator;
Radiation dose rate is 1-600kGy/h, and absorbed dose of radiation is reduced to standard with " silver-colored source " 100%.
Silver powder after radiation reduction, without separation directly application, also can adopt the simple cleaning of deionized water (or organic solvent), concentrated or dry rear use.
Silver powder particle diameter controls by regulating the ratio of various raw material and the size of radiation dose rate, generally can be controlled between 10nm-3 μm;
Preferably, the percentage by weight of each raw material is:
The present invention's employing, not containing " the silver-colored source " of nitrate anion, prepares silver powder by nuclear radiation reduction technique, and the method is not only exempted to use chemical reducing agent, and not containing inorganic byproduct impurity in product, later separation is simple with purification.
Good effect of the present invention is: compared with existing silver powder technology of preparing, the silver powder product impurity content of this method gained is low, directly can apply without separation, or concentrated after slightly doing cleaning (or drying) just can apply, there is clean environment firendly, advantage that cost is low.Larger impetus is had to the development of electronic device and product.
Detailed description of the invention
Embodiment 1
Raw material: (percentage by weight)
Silver source 9%, dispersant 0.5%, active particle agent for capturing 1.5%, weight concentration is ammoniacal liquor 0.1% and the deionized water 88.9% of 28%;
Silver source is citric acid three silver medal, and dispersant is PVP, and active particle agent for capturing is isopropyl alcohol;
Citric acid three silver medal is joined in the water containing dispersant PVP, active particle agent for capturing, ammoniacal liquor, dispersed with stirring; Logical nitrogen deoxygenation puts into Co-60 source irradiation after 5 minutes, close rate is 100kGy/h; React 24 hours under room temperature, products therefrom is dry after washed with de-ionized water.
Embodiment 2
Raw material: (percentage by weight)
Silver source 10%, dispersant 0.2%, active particle agent for capturing 1.1%, weight concentration is ammoniacal liquor 0.3% and the deionized water 88.5% of 28%;
Silver source is silver acetate, and dispersant is gelatin, and active particle agent for capturing is ethanol,
Silver acetate is joined in the deionized water containing dispersant gelatin, active particle agent for capturing, ammoniacal liquor, dispersed with stirring; Logical nitrogen deoxygenation puts into Co-60 source irradiation after 5 minutes, close rate is 100kGy/h; React 24 hours under room temperature, products therefrom through 60 DEG C of decompression distillation removing moisture content, when to be concentrated into silver content be 60%.
Embodiment 3
Raw material: (percentage by weight)
Silver source 15%, dispersant 0.1%, active particle agent for capturing 10%, deionized water 74.9%;
Silver source is silver acetate and silver oxide, and weight ratio is 1:1; Dispersant is gelatin; Active particle agent for capturing is ethanol and triethanolamine, and weight ratio is 1:1;
Silver-colored source is joined in the deionized water containing dispersant gelatin, active particle agent for capturing, dispersed with stirring; Logical nitrogen deoxygenation puts into Co-60 source irradiation after 5 minutes, close rate is 100kGy/h; React 24 hours under room temperature, products therefrom through 60 DEG C of decompression distillation removing moisture content, when to be concentrated into silver content be 60%.
Embodiment 4
Raw material: (percentage by weight)
Silver source 15%, dispersant 0.1%, active particle agent for capturing 6%, deionized water 78.9%;
Silver source is silver carbonate; Dispersant is gelatin; Active particle agent for capturing is ethanol and triethanolamine, and weight ratio is 1:1;
Silver-colored source is joined in the deionized water containing dispersant gelatin, active particle agent for capturing, dispersed with stirring; Logical nitrogen deoxygenation puts into Co-60 source irradiation after 5 minutes, close rate is 100kGy/h; React 24 hours under room temperature, products therefrom through 60 DEG C of decompression distillation removing moisture content, when to be concentrated into silver content be 60%.
Claims (7)
1. radiation reduction prepares the method for silver powder, it is characterized in that, comprise the steps: the ammoniacal liquor 0-1% and the deionized water 40-96% that containing silver-colored source 1-40%, the dispersant 0-1% of nitrate anion, active particle agent for capturing 0.1-10%, weight concentration will not be 28%, be uniformly mixed, under inert gas atmosphere, be placed in radiation source, carry out radiation reduction reaction under agitation, then from product, collect described silver powder.
2. method according to claim 1, is characterized in that, the percentage by weight of each raw material is:
3. method according to claim 1 and 2, is characterized in that, described does not include but not limited to one or more in citric acid three silver medal, silver oxalate, silver acetate, silver formate, silver carbonate, silver oxide, silver tartrate containing the silver-colored source of nitrate anion.
4. method according to claim 1 and 2, it is characterized in that, described dispersant be selected from PVP (PVP), gelatin, polyvinyl alcohol (PVA), lauryl sodium sulfate or PEO (PEO) etc. more than one.
5. method according to claim 1 and 2, is characterized in that, described active particle agent for capturing be selected from isopropyl alcohol, ethanol, methyl alcohol, acetone, formic acid ammonia, triethanolamine, triethylene tetramine or five ethene hexamines one or more.
6. method according to claim 1 and 2, is characterized in that, described radiation source be cobalt-60 (
60co) gamma-ray radiation source or electron accelerator.
7. method according to claim 6, is characterized in that, radiation dose rate is 1-600kGy/h, and absorbed dose of radiation is reduced to standard with silver-colored source 100%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410406488.8A CN105364082B (en) | 2014-08-18 | 2014-08-18 | The method that radiation reduction prepares silver powder |
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| CN201410406488.8A CN105364082B (en) | 2014-08-18 | 2014-08-18 | The method that radiation reduction prepares silver powder |
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| CN105364082A true CN105364082A (en) | 2016-03-02 |
| CN105364082B CN105364082B (en) | 2018-01-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114007783A (en) * | 2019-06-20 | 2022-02-01 | 南非大学 | Nanofluid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190042A (en) * | 1997-02-03 | 1998-08-12 | 中国科学技术大学 | Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film |
| CN101612670A (en) * | 2009-07-13 | 2009-12-30 | 浙江省技术物理应用研究所 | A kind ofly in the aqueous solution, use 60The Co-gamma-rays prepares the method for nano-silver powder |
| JP2010018839A (en) * | 2008-07-10 | 2010-01-28 | Osaka Prefecture Univ | Metal nanoparticle production device and metal nanoparticle production method |
| CN102069193A (en) * | 2011-01-17 | 2011-05-25 | 华东理工大学 | Method for preparing granularity-controllable narrow-distribution spherical easily-dispersible silver powder through radiation reduction |
| CN102773494A (en) * | 2011-05-13 | 2012-11-14 | 华东理工大学 | Method for preparing silver-coated copper powder through radiation reduction |
| RU2510310C1 (en) * | 2012-11-29 | 2014-03-27 | Общество с ограниченной ответственностью "Суперматериал" | Method for obtaining silver nanoparticles in polymer matrixes at laser irradiation |
-
2014
- 2014-08-18 CN CN201410406488.8A patent/CN105364082B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190042A (en) * | 1997-02-03 | 1998-08-12 | 中国科学技术大学 | Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film |
| JP2010018839A (en) * | 2008-07-10 | 2010-01-28 | Osaka Prefecture Univ | Metal nanoparticle production device and metal nanoparticle production method |
| CN101612670A (en) * | 2009-07-13 | 2009-12-30 | 浙江省技术物理应用研究所 | A kind ofly in the aqueous solution, use 60The Co-gamma-rays prepares the method for nano-silver powder |
| CN102069193A (en) * | 2011-01-17 | 2011-05-25 | 华东理工大学 | Method for preparing granularity-controllable narrow-distribution spherical easily-dispersible silver powder through radiation reduction |
| CN102773494A (en) * | 2011-05-13 | 2012-11-14 | 华东理工大学 | Method for preparing silver-coated copper powder through radiation reduction |
| RU2510310C1 (en) * | 2012-11-29 | 2014-03-27 | Общество с ограниченной ответственностью "Суперматериал" | Method for obtaining silver nanoparticles in polymer matrixes at laser irradiation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114007783A (en) * | 2019-06-20 | 2022-02-01 | 南非大学 | Nanofluid |
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