CN1308102A - Nanometer level silver oxide and its production process - Google Patents
Nanometer level silver oxide and its production process Download PDFInfo
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- CN1308102A CN1308102A CN 01108083 CN01108083A CN1308102A CN 1308102 A CN1308102 A CN 1308102A CN 01108083 CN01108083 CN 01108083 CN 01108083 A CN01108083 A CN 01108083A CN 1308102 A CN1308102 A CN 1308102A
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Abstract
The present invention relates to a nanometer-level silver oxide, its mean grain size is 80-100 nm, and the difference of maximum grain size and minium grain size is less than or equal to 5nm. Its production process includes the following steps: dissolving silvers nitrate by adding water, progressively adding concentrated ammonia water under the condition of stirring to obtain silver ammonia solution; then adding water and dissolving solid sodium hydroxide and protecting agent, and stirring them to obtain an alkali solution, then progressively adding the silver ammonia solution into the alkaline solution under the condition of stirring, fully stirring them, centrifugation to obtain silver oxide, washing and vacuum dryign so as to obtain the invented nanometer-level silver oxide with good stability and dispersity and uniform grain distribution. Its protecting agent can be polyvinyl-pyrrolidone (PVP) or polyvinyl alcohol.
Description
The present invention relates to nanometer level silver oxide and production technique thereof.
Silver suboxide (Ag
2O) be widely used in electronic devices and components, button cell, sanitas, scavenging agent, glass colorant and industries such as abrasive, chemical catalyst.Have 30% silver to be used for silver suboxide (or Silver Nitrate) production in the industrial silver, wherein the silver suboxide that consumed of electronic devices and components industry accounts for 90% of silver suboxide ultimate production.At present, silver nitrate solution and sodium hydroxide solution reaction are mainly adopted in state's internal oxidized Ag production, obtain the silver suboxide post precipitation, obtain the silver suboxide finished product through washing, separation and drying.The key technical indexes of product comprises not hypostasis content of silver suboxide content, clarity test and nitric acid insolubles, free alkali, nitrate, hydrochloric acid, weight loss on drying etc.
The main problem that exists has:
1. existing product does not have the definiteness mark to granularity, and granularity is difficult to reach the needs of different industries.In the Electronic Components Manufacturing with silver, silver suboxide generally is used for making the silver suboxide slurry, by the levigate back of ball milling method and other mixing of materials (needing approximately about 7 days), again by being screen-printed on the device substrate.The size of silver oxide particle degree directly has influence on the quality of prepared silver suboxide slurry and the expense of silk-screen, and then has influence on device quality.The desired silver oxide particle degree of this industry is the smaller the better.The domestic and foreign current production technique is difficult to accomplish.Require granularity the smaller the better equally at used silver suboxides of industry such as chemical catalyst, medical sanitas and glass colorants.
2. though the purity of homemade silver suboxide can reach GB, because on the current technology, product particle is too big, wraps up impurity easily, it is very big to obtain high-purity or ultrapure silver suboxide difficulty.
The purpose of this invention is to provide nanometer level silver oxide of a kind of stable, good dispersity, even particle size distribution and preparation method thereof.
Technological thought of the present invention: when silver nitrate solution directly reacts with sodium hydroxide solution, the Ag in the solution
+Concentration is excessive, and the speed of growth of silver suboxide particulate in reaction system of generation is too fast, is easy between the particle simultaneously reunite, and causes the silver suboxide product particle that obtains excessive.If Ag in the time of reducing reaction
+Concentration, the formation speed that makes silver suboxide is accelerated and the speed of growth slows down, and is protected immediately after silver oxide particle generates simultaneously, stops the generation of agglomeration, then can obtain the minimum silver oxide particle product of granularity.
Therefore technical scheme of the present invention is as follows:
A kind of nanometer level silver oxide, its median size≤100nm, and its maximum particle diameter and minimum grain size poor≤5nm.
A kind of nanometer level silver oxide production technique, it is that Silver Nitrate is made into the aqueous solution, adds strong aqua and obtains silver ammino solution, joins gradually to be added with in advance in protectant sodium hydroxide solution, the superfine silver oxide precipitation promptly generates.Obtain the superfine silver oxide that median size is 80-100nm through filtration, washing and drying.
Above-mentioned protective material can be a polyvinylpyrrolidone, or polyvinyl alcohol.
Concrete way is:
Silver Nitrate 50-100 part (quality, down together) is dissolved in 300 parts of water, under agitation adds strong aqua 100-400 part gradually, be made into silver ammino solution.In addition solid sodium hydroxide 20-40 part and 0.2-1.0 part protective material are added 500 parts in water, stirring and dissolving, proportionaling alkali-forming solution.Protective material can be polyvinylpyrrolidone or polyvinyl alcohol.Above-mentioned silver ammino solution is under agitation joined in the above-mentioned alkaline solution gradually, fully stir 4-8 hour again after, centrifuging goes out silver suboxide, washes with water 3 times, uses washing with alcohol again 3 times, is lower than 80 ℃ of following vacuum-dryings in temperature, promptly gets nanometer level silver oxide.The nanometer level silver oxide particle diameter of the inventive method preparation is 80-100nm, stability, good dispersity, even particle size distribution.
Adopt production technique of the present invention, the silver suboxide median size that obtains is below the 100nm, and the poor≤5nm of maximum particle diameter and minimum grain size owing to adopted protective material, therefore has good stability and dispersiveness.
Embodiment 1
Silver Nitrate 50Kg is dissolved in the 300L water, under agitation adds strong aqua 100L gradually, be made into silver ammino solution.In addition solid sodium hydroxide 40Kg and 0.2Kg protective material (polyvinylpyrrolidone is called for short PVP, and molecular weight is 30000) are added water 500L, stirring and dissolving, proportionaling alkali-forming solution.Silver ammino solution is under agitation joined in the alkaline solution gradually, fully stir 4h again after, centrifuging goes out silver suboxide, washes with water 3 times, uses washing with alcohol again 3 times, is 80 ℃ of vacuum-dryings in temperature, promptly gets nanometer level silver oxide.The nanometer level silver oxide median size that present embodiment is produced is 88nm, the poor≤5nm of maximum particle diameter and minimum grain size.
Embodiment 2
Silver Nitrate 100Kg is dissolved in the 300L water, under agitation adds strong aqua 100L gradually, be made into silver ammino solution.In addition solid sodium hydroxide 25Kg and 1.0Kg protective material (polyvinylpyrrolidone, molecular weight are 30000) are added water 500L, stirring and dissolving, proportionaling alkali-forming solution.Silver ammino solution is under agitation joined in the alkaline solution gradually, fully stir 8h again after, centrifuging goes out silver suboxide, washes with water 3 times, uses washing with alcohol again 3 times, is 80 ℃ of vacuum-dryings in temperature, promptly gets nanometer level silver oxide.The nanometer level silver oxide median size that present embodiment is produced is 100nm, the poor≤5nm of maximum particle diameter and minimum grain size.
Embodiment 3
Silver Nitrate 100Kg is dissolved in the 300L water, under agitation adds strong aqua 400L gradually, be made into silver ammino solution.In addition solid sodium hydroxide 40Kg and 1.0Kg protective material (polyvinylpyrrolidone, molecular weight are 30000) are added water 500L, stirring and dissolving, proportionaling alkali-forming solution.Silver ammino solution is under agitation joined in the alkaline solution gradually, fully stir 8h again after, centrifuging goes out silver suboxide, washes with water 3 times, uses washing with alcohol again 3 times, is 80 ℃ of vacuum-dryings in temperature, promptly gets nanometer level silver oxide.The nanometer level silver oxide median size that present embodiment is produced is 82nm, the poor≤5nm of maximum particle diameter and minimum grain size.
Embodiment 4
Silver Nitrate 50Kg is dissolved in the 300L water, under agitation adds strong aqua 400L gradually, be made into silver ammino solution.In addition solid sodium hydroxide 40Kg and 1.0Kg protective material (polyvinylpyrrolidone, molecular weight are 30000) are added water 500L, stirring and dissolving, proportionaling alkali-forming solution.Silver ammino solution is under agitation joined in the alkaline solution gradually, fully stir 8h again after, centrifuging goes out silver suboxide, washes with water 3 times, uses washing with alcohol again 3 times, is 80 ℃ of vacuum-dryings in temperature, promptly gets nanometer level silver oxide.The nanometer level silver oxide median size that present embodiment is produced is 80nm, the poor≤5nm of maximum particle diameter and minimum grain size.
Embodiment 5
Silver Nitrate 50Kg is dissolved in the 300L water, under agitation adds strong aqua 100L gradually, be made into silver ammino solution.In addition solid sodium hydroxide 15Kg and 0.2Kg protective material (polyvinyl alcohol, being called for short the PVA molecular weight is 40000) are added water 500L, stirring and dissolving, proportionaling alkali-forming solution.Silver ammino solution is under agitation joined in the alkaline solution gradually, fully stir 8h again after, centrifuging goes out silver suboxide, washes with water 3 times, uses washing with alcohol again 3 times, is 80 ℃ of vacuum-dryings in temperature, promptly gets nanometer level silver oxide.The nanometer level silver oxide median size that present embodiment is produced is 92nm, the poor≤5nm of maximum particle diameter and minimum grain size.
Claims (3)
1. a nanometer level silver oxide is characterized in that its median size is smaller or equal to 100nm.
2. the production technique of a nanometer level silver oxide according to claim 1; it is characterized in that Silver Nitrate is mixed with the aqueous solution; add ammoniacal liquor and obtain silver ammino solution; join gradually and be added with in advance in protectant sodium hydroxide solution; the superfine silver oxide precipitation promptly generates; after filtration, washing and dry, obtain the superfine silver oxide that median size is 80-100nm.
3. production technique according to claim 1 is characterized in that protective material is polyvinylpyrrolidone or polyvinyl alcohol.
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| CNB011080833A CN1169883C (en) | 2001-02-07 | 2001-02-07 | Nanometer level silver oxide and its production process |
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| CNB011080833A CN1169883C (en) | 2001-02-07 | 2001-02-07 | Nanometer level silver oxide and its production process |
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| CN1169883C CN1169883C (en) | 2004-10-06 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006005521A1 (en) * | 2004-07-13 | 2006-01-19 | L'oreal | Aqueous photoprotective composition comprising hydrophilic metal oxide nanopigments and a vinylpyrrolidone homopolymer; uses |
| CN100500573C (en) * | 2007-04-04 | 2009-06-17 | 厦门大学 | Shape and size controllable preparation method of micro-nano silver oxide |
| US7745509B2 (en) * | 2003-12-05 | 2010-06-29 | 3M Innovative Properties Company | Polymer compositions with bioactive agent, medical articles, and methods |
| CN102259905A (en) * | 2010-05-26 | 2011-11-30 | 昆明其化新材料科技有限公司 | Preparation method of superfine silver oxide |
| CN101698500B (en) * | 2009-11-03 | 2011-12-28 | 宁波晶鑫电子材料有限公司 | Method for preparing micron-sized silver oxide powder with porous structure |
| CN107051432A (en) * | 2017-04-21 | 2017-08-18 | 滨州学院 | A kind of preparation method of photochemical catalyst and the equipment suitable for the preparation method |
| CN113576989A (en) * | 2021-08-02 | 2021-11-02 | 辽宁工程技术大学 | Zeolite-loaded aloe vera gel for treating acne and preparation method thereof |
| CN114121339A (en) * | 2022-01-28 | 2022-03-01 | 西安宏星电子浆料科技股份有限公司 | Conductive silver adhesive composition with low contact resistivity with TCO transparent conductive film layer |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7285576B2 (en) | 2003-03-12 | 2007-10-23 | 3M Innovative Properties Co. | Absorbent polymer compositions, medical articles, and methods |
-
2001
- 2001-02-07 CN CNB011080833A patent/CN1169883C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7745509B2 (en) * | 2003-12-05 | 2010-06-29 | 3M Innovative Properties Company | Polymer compositions with bioactive agent, medical articles, and methods |
| WO2006005521A1 (en) * | 2004-07-13 | 2006-01-19 | L'oreal | Aqueous photoprotective composition comprising hydrophilic metal oxide nanopigments and a vinylpyrrolidone homopolymer; uses |
| FR2873028A1 (en) * | 2004-07-13 | 2006-01-20 | Oreal | Photo-protective composition for use e.g. in manufacture of products for cosmetic treatment of e.g. skin, comprises aqueous phase(s), hydrophilic metal oxide nanopigments, and vinyl pyrrolidone homopolymer(s) in physiological medium |
| CN100500573C (en) * | 2007-04-04 | 2009-06-17 | 厦门大学 | Shape and size controllable preparation method of micro-nano silver oxide |
| CN101698500B (en) * | 2009-11-03 | 2011-12-28 | 宁波晶鑫电子材料有限公司 | Method for preparing micron-sized silver oxide powder with porous structure |
| CN102259905A (en) * | 2010-05-26 | 2011-11-30 | 昆明其化新材料科技有限公司 | Preparation method of superfine silver oxide |
| CN107051432A (en) * | 2017-04-21 | 2017-08-18 | 滨州学院 | A kind of preparation method of photochemical catalyst and the equipment suitable for the preparation method |
| CN113576989A (en) * | 2021-08-02 | 2021-11-02 | 辽宁工程技术大学 | Zeolite-loaded aloe vera gel for treating acne and preparation method thereof |
| CN114121339A (en) * | 2022-01-28 | 2022-03-01 | 西安宏星电子浆料科技股份有限公司 | Conductive silver adhesive composition with low contact resistivity with TCO transparent conductive film layer |
| CN114121339B (en) * | 2022-01-28 | 2022-05-31 | 西安宏星电子浆料科技股份有限公司 | Conductive silver adhesive composition with low contact resistivity with TCO transparent conductive film layer |
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| Publication number | Publication date |
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| CN1169883C (en) | 2004-10-06 |
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