CN1093023C - Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film - Google Patents
Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film Download PDFInfo
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- CN1093023C CN1093023C CN97100952A CN97100952A CN1093023C CN 1093023 C CN1093023 C CN 1093023C CN 97100952 A CN97100952 A CN 97100952A CN 97100952 A CN97100952 A CN 97100952A CN 1093023 C CN1093023 C CN 1093023C
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Abstract
The present invention relates to a preparation method of metal, metal oxides or metal films, which comprises: soluble metal salt containing certain compositions and a buffer solution system of isopropyl alcohol are placed under an ultraviolet light source; the irradiation of solution absorption is controlled within 40 to 3000 J/ml, which can prepare metal or metal oxide ultrafine powder of uniform granularity, and the size of the ultrafine powder is 10 to 100 nm, or a metal film of uniform film thickness is prepared on a substrate. The equipment of the present invention is simple, and can be operated under normal temperature and pressure. The present invention has the advantage of simple technology, and is suitable for the preparation of nickel, cobalt, copper, silver, gold, platinum group metal and the metal suboxide ultrafine powder thereof.
Description
The present invention relates to the preparation method and the ultraviolet rays irradiation applied technical field of metal oxide superfine powder.
Metal, metal oxide ultrafine particulate and powder thereof or metallic film become the important object of chemistry and investigation of materials owing to the widespread use in catalysis, photodissociation, fine chemistry industry, electronics and magneticsubstance and other functional materials.Typical preparation method such as Britain's " progress in materials science " (Progress inMaterials) 1991,35 volumes, the vacuum or the reactant gas evaporation-condensation method of page 1 report, but this vapor phase process preparation owned by France, equipment is comparatively complicated; Chinese patent application number 95100344.5 and 96101060.6 gamma-ray irradiation method preparations that propose; though can directly from aqueous environment, make metal super-fine microparticle or metallic film respectively; the optional equipment that yet the cobalt source must be arranged and have relatively high expectations; at the high levels of radioactivity environment strict safeguard procedures must be arranged; operate cumbersome; be difficult to generally promote, do not relate to the preparation of metal oxide superfine powder simultaneously again.Therefore the preparation method who seeks the simple more metal oxide superfine powder of technology and equipment is still very necessary.
The objective of the invention is to propose the method that a kind of solution that adopts ultraviolet rays irradiation metal ion directly prepares the Red copper oxide ultrafine powder, to overcome existing preparation method's above-mentioned shortcoming.
The preparation method of this Red copper oxide ultrafine powder is characterized in that adopting ultraviolet rays irradiation to contain the aqueous solution of soluble copper salt, contains following material in this solution:
Neutralized verdigris or copper sulfate 0.001-1 mol
Virahol 0.08-0.8 mol
Acetic acid 0.004-0.17 mol
Sodium-acetate 0.006-0.15 mol
Sodium lauryl sulphate (SLS) or sodium laurylsulfonate (SDS) 0.288-3 mg/ml
Control this solution and accept the irradiation energy of ultraviolet rays irradiation absorption between 40-210J/ml.
Owing to contain the aqueous solution of metal ion when being subjected to ultraviolet rays irradiation, can produce the hydrated electron of strong reductant effect, it can be with the metal ion gradual deoxidizing, by the suitable buffered soln environment of control acetic acid-sodium-acetate and the suitable dosage of ultraviolet rays irradiation, thereby promptly may command reduction of metal ion degree obtains metal super-fine microparticle or film or metal oxide superfine powder; The hydrated electron that produces in view of irradiation is evenly distributed in solution, so adopt the present invention can make particle evenly isolated nucleation in solution; Additive helps to make particle to be protected when generating, thereby plays the effect of modified outcome particle; When containing multiple metal ion in the solution, but also single stage method is synthesized the metal/metal oxide composite ultrafine powder.
Compare with existing preparation metal oxide ultrafine particulate and powder method thereof, the equipment that the present invention uses is simple, can operate at normal temperatures and pressures, and is simple for process, and can be by regulator solution concentration and irradiation time control ultrafine particle size.The superfine powder that is obtained through X-ray diffraction slow sweep and electron microscopic analysis as can be known, size of particles is between 10-100nm.
Because the precious metal reduction potential is far above copper, so the inventive method is also applicable to the preparation of precious metal metal suboxide ultrafine powder.
Below be several embodiment of the inventive method:
Embodiment 1:
Be dissolved in 9mg neutralized verdigris, 6mg acetic acid, 12.3mg sodium-acetate and 14.4mg sodium lauryl sulphate (SLS) in the distilled water together, add the 3ml Virahol again, last adding distil water is mixed with the aqueous solution of 50ml containing metal cupric ion, be transferred to thickness of pipe 1.5mm, be of a size of in the silica tube of Φ 45mm * 150mm, mouth of pipe covered, and solution is placed predominant wavelength is the uniform light field district internal irradiation of the commercially available column low pressure mercury lamp stage casing range distance fluorescent tube axis 3-9cm of 254nm, electric power 30W, and irradiation promptly produced bright red Cu in 0.5 hour
2The O ultrafine particle filters and collects Cu
2O superfine powder product.Product is measured through TEM and X-ray diffraction slow sweep, size of particles between 10-35nm, median size 20nm.By being that 20mW calculates by the average irradiation energy specific absorption of irradiating soln per unit volume, the irradiation energy of solution absorption is 40J/ml.
Embodiment 2:
79.8mg copper sulfate, 12mg acetic acid, 24.6mg sodium-acetate and 144mg sodium lauryl sulphate (SLS) are dissolved in the distilled water together, add the 3ml Virahol again, last adding distil water is mixed with the aqueous solution of 50 milliliters of containing metal cupric ions.All the other steps are identical with embodiment 1, and irradiation promptly produced bright red Cu in 1 hour
2The O ultrafine particle filters and collects Cu
2O superfine powder product.Size of particles between 15-40nm, median size 25nm.The irradiation energy of irradiating soln absorption is 70J/ml as can be known as calculated.
Embodiment 3:
8g copper sulfate, 500mg acetic acid, 600mg sodium-acetate and 150mg sodium laurylsulfonate (SES) are dissolved in the distilled water together, and last adding distil water is mixed with the aqueous solution of 50ml containing metal cupric ion.All the other steps are identical with embodiment 1, and irradiation promptly produced bright red Cu in 3 hours
2The O ultrafine particle filters and collects Cu
2O superfine powder product.Size of particles between 50-100nm, median size 80nm.The irradiation energy of irradiating soln absorption is 210J/ml as can be known as calculated.
Claims (1)
1. the preparation method of a Red copper oxide ultrafine powder is characterized in that adopting ultraviolet rays irradiation to contain the aqueous solution of soluble copper salt, contains following material in this solution:
Neutralized verdigris or copper sulfate 0.001-1 mol
Virahol 0.08-0.8 mol
Acetic acid 0.004-0.17 mol
Sodium-acetate 0.006-0.15 mol
Sodium lauryl sulphate (SLS) or sodium laurylsulfonate (SDS) 0.288-3 mg/ml
Control this solution and accept the irradiation energy of ultraviolet rays irradiation absorption between 40-210J/ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97100952A CN1093023C (en) | 1997-02-03 | 1997-02-03 | Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97100952A CN1093023C (en) | 1997-02-03 | 1997-02-03 | Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1190042A CN1190042A (en) | 1998-08-12 |
| CN1093023C true CN1093023C (en) | 2002-10-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97100952A Expired - Fee Related CN1093023C (en) | 1997-02-03 | 1997-02-03 | Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film |
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| CN (1) | CN1093023C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322952C (en) * | 2004-09-24 | 2007-06-27 | 昆明贵金属研究所 | Indirecting light chemical preparation for gold nanometer material |
| CN100503744C (en) * | 2006-04-07 | 2009-06-24 | 中国科学院上海应用物理研究所 | Method for preparing nano silver grain, and prepared nano silver grain |
| CN101612671B (en) * | 2009-07-13 | 2011-04-27 | 浙江大学 | Method for preparing nanometer copper powder by using <60>Co-gamma rays in aqueous solution |
| CN105080544B (en) * | 2014-05-22 | 2017-11-03 | 天津大学 | The method that laser liquid phase ablation synthesizes cuprous oxide carbon mano-tube composite |
| CN105364082B (en) * | 2014-08-18 | 2018-01-19 | 上海理凯材料科技有限公司 | The method that radiation reduction prepares silver powder |
| CN105268987B (en) * | 2015-04-14 | 2018-05-18 | 华东理工大学 | A kind of method that liquid phase ultraviolet irradiation prepares mesoporous platinum |
| CN106086878A (en) * | 2016-06-22 | 2016-11-09 | 深圳市开天源自动化工程有限公司 | Utilize the method that ultraviolet forms antibacterial film on plastic carrier surface |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03215608A (en) * | 1990-01-19 | 1991-09-20 | Tanaka Kikinzoku Kogyo Kk | Manufacture of noble super fine particles |
| CN1127177A (en) * | 1995-01-16 | 1996-07-24 | 中国科学技术大学 | Ionization radiation chemistry redox preparation method for nm metal powder |
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1997
- 1997-02-03 CN CN97100952A patent/CN1093023C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03215608A (en) * | 1990-01-19 | 1991-09-20 | Tanaka Kikinzoku Kogyo Kk | Manufacture of noble super fine particles |
| CN1127177A (en) * | 1995-01-16 | 1996-07-24 | 中国科学技术大学 | Ionization radiation chemistry redox preparation method for nm metal powder |
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| CN1190042A (en) | 1998-08-12 |
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