CN105499595A - Preparing method of foamed silver material carrying nano silver - Google Patents
Preparing method of foamed silver material carrying nano silver Download PDFInfo
- Publication number
- CN105499595A CN105499595A CN201410494581.9A CN201410494581A CN105499595A CN 105499595 A CN105499595 A CN 105499595A CN 201410494581 A CN201410494581 A CN 201410494581A CN 105499595 A CN105499595 A CN 105499595A
- Authority
- CN
- China
- Prior art keywords
- silver
- nano
- foam
- foamed
- foam silver
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Powder Metallurgy (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparing method of a foamed silver material carrying nano silver. The method mainly comprises the following several steps: first, selecting a certain size of foamed silver as a carrier, and uniformly dropping a certain concentration of silver nitrate solution on the foamed silver carrier; then, placing the foamed silver with silver nitrate attached in an oven to carry out dewatering treatment, after dewatering, carrying out 400-600 DEG C high-temperature treatment on the foamed silver material with silver nitrate attached to the surface in a furnace, and realizing the decomposition of the silver nitrate; and finally, carrying out 400-900 DEG C reduction treatment on the material at a reduction atmosphere, realizing the great combination of nano silver and foamed silver surfaces, and obtaining the foamed silver material carrying nano silver. The method can regulate the number, distribution density and corresponding particle size of nano silver on the surface of a foamed silver tiny structure through controlling the concentration of the silver nitrate solution and the later reduction sintering temperature. The preparing method of the foamed silver material carrying nano silver is simple in technology, simple to operate, stable in performance and suitable for massive production.
Description
Technical field
That the present invention relates to is a kind of preparation method of nano metal material, and what be specifically related to is matrix material using Foam silver as carrier, realizes a kind of preparation method of Nano Silver and Foam silver surface recombination.
Background technology
Foam (also claiming porous) metal material is development in recent years a kind of Multifunction material faster.Foam metal has three-dimensional netted through-hole structure, porosity is high, specific area is large, permeability is good, is all widely used in a lot of field.Foam silver is as the one in foam metal, except possessing general character structure and characteristics that above-mentioned foam metal has, it also has good adsorptivity, very strong capillary force and high thermal conductivity and conductance and good bactericidal effect etc., and thus Foam silver is with a wide range of applications in fields such as medical science, chemical industry, environmental protection, new forms of energy, electronics, biological detection.
Because silver is as the one of noble metal, it is as foaming structure and nano application just most valuable and effect, particularly Nano Silver has the special process based prediction model such as nanometer or quantum size effect, macro quanta tunnel effect and skin effect due to it, gets more and more people's extensive concerning.Nano Silver has metastable physical and chemical performance, as high surface, bigger serface, strong catalytic capability and high conductance, now many fields such as electric slurry, biology sensor, catalysis, low-temperature superconducting, nano-device and optical switch are widely used in.In addition, Nano Silver also has antibacterial, deodorizing and the ultraviolet function of absorption portion, thus can be applicable to pharmaceuticals industry (for aspects such as medical apparatus sterilizing, externally used antimicrobial medicine and agricultural plant bactericide), building materials field (for aspects such as coating, paint, floor, potteries), marine microorganism protection and cosmetics sterilization of keeping a public place clean (as mildy wash, water smoke spray and repair breast etc. aspect) etc. industry, as added a small amount of Nano Silver in chemical fibre, some performance of chemical fibre product can be changed, and give very strong sterilizing ability.
Silver is made particle diameter from structure or size is little of nano level argent by Nano Silver exactly in theory, and according to the usual definition of nano material, the particle diameter of Nano Silver should be less than or equal to 100nm.We know, when the particle diameter of material is less, its surface area is larger, just because of the high specific area that the particle diameter that Nano Silver is minimum is formed, just make the performances such as the bactericidal effect of Nano Silver and catalytic efficiency be far superior to the block materials of silver or the Foam silver material that obtained by micron-scale silver powder, thus the size controlling nano-Ag particles cause close important.Except containing Nano Silver paste, Nano Silver needs to load on carrier usually, and the nano effect that the kind of carrier material and structure produce it is directly related.Conventional kind of carrier, as metal, pottery, carbon or string, as selected the structure of carrier to be the foaming structure of through hole, will improve the characteristics such as the specific area of Nano Silver greatly.Nano Silver size is relevant with corresponding preparation technology with the control of quantity, because under nano-scale, Nano Silver easily occurs reunite and grow up, thus lose its nano effect, therefore how to realize the good combination of Nano Silver and carrier and effectively to control the size of Nano Silver by corresponding preparation technology most important to subsequent applications.In addition, the application operating mode of Nano Silver is relevant with the material of the matrix material selected, and relates to the bond strength of Nano Silver and carrier interface and the durability of the follow-up use of Nano Silver and regenerative nature, we have proposed the present invention for this reason.
Summary of the invention
The object of the invention is to utilize the specific area of Foam silver own very large, overcome above-mentioned Nano Silver and be difficult to realize deficiency that good interface is combined and application operating mode to the requirement of carrier medium itself between carrier, can guarantee on the basis of Nano Silver and carrier Foam silver surface good combination, the nano effect of abundant displaying Nano Silver and corresponding Foam silver and the common bactericidal action etc. of Nano Silver, meet some application operating mode to the restriction of material and requirement.For this reason, the present invention proposes that a kind of technique is simple, easy to operate, the preparation method of the Foam silver loaded with nano ag material of excellent performance, Foam silver loaded with nano ag material prepared by the method have that huge specific area, controlled porosity are high, Nano Silver domain size distribution and the feature such as size is controlled.When Foam silver loaded with nano ag material is used for the environmental protection such as sterilization and medical application, not only Nano Silver plays bactericidal effect, the Foam silver of its carrier own can play certain bactericidal action and strong capillary action too, and both materials of the same race, not because of other any side effects that the difference of material is brought, achieve the three-dimensional through hole foaming structure of material of the same race and the integration of nanostructured.
Technical scheme of the present invention is as follows:
Foam silver loaded with nano ag material of the present invention is prepared by the following method, and this preparation method specifically comprises the following steps:
(1) first select the Foam silver of a certain specification as carrier, choose the different porosities of Jiangsu Ge Ye new material Science and Technology Ltd. and the Foam silver of thickness, its porosity ranges 40 ~ 95%, thickness can choose according to application requirement at 0.05 ~ 3mm;
(2) prepare the silver nitrate aqueous solution of desired concn, the concentration of solution is chosen as 0.001 ~ 3M, by theory calculate, adds concentration and the quantity of liquor argenti nitratis ophthalmicus needed for calculating, and adopts dropper to be evenly added drop-wise on Foam silver carrier by corresponding liquor argenti nitratis ophthalmicus;
(3) Foam silver then surface being had silver nitrate is placed in baking oven and carries out processed, and the temperature that baking oven is arranged is 80 ~ 100 DEG C, and dewatering time is chosen according to thickness etc., is generally 0.3 ~ 1 hour;
(4), after dehydration, the Foam silver material of adsorption silver nitrate is carried out pyrolytic process in oxidation furnace or chamber type electric resistance furnace, and resolution process temperature is arranged on 400 ~ 600 DEG C usually, and the resolution process time is chosen as 0.3 ~ 2 hour;
(5) last, above-mentioned material is carried out reduction sintering processes in reducing atmosphere, realizes the good combination on Nano Silver and Foam silver surface, can obtain Foam silver loaded with nano ag material like this, the atmosphere temperature of wherein said reduction treatment is chosen as 400 ~ 900
oc, reducing atmosphere is H
2and N
2mist or pure hydrogen, wherein the percent by volume of hydrogen is: 10 ~ 100%.
According to above-mentioned preparation method, can prepare that specific area is very large, nano-Ag particles is evenly distributed and the Foam silver loaded with nano ag material that particle size is close and controlled, Foam silver loaded with nano ag material prepared by the present invention has the following advantages: in (1) Foam silver loaded with nano ag material, the particle size of Nano Silver effectively can control by decomposing and reducing sintering temperature; (2) the micron particles surface conjunction of nano-Ag particles and Foam silver is good, and bond strength can be improved according to reduction sintering temperature and the selection of time; (3) the method according to technological parameters such as the concentration of liquor argenti nitratis ophthalmicus, addition, decomposition temperature, reduction sintering temperatures, can regulate and control distribution density and the particle size of Foam silver nano surface silver; (4) the method technique is simple, easy to operate, suitability for mass industrialized production.Thus can need according to application the design carrying out Foam silver loaded with nano ag material, in conjunction with the selection of Foam silver carrier porosity, realize the quantity of Nano Silver and effective control of size, guarantee the effect of required Foam silver loaded with nano ag material.
accompanying drawing illustrates:
Fig. 1 is the ESEM micro-structural tissue that example 1 adopts Foam silver loading nano silvery of the present invention
Fig. 2 is the ESEM micro-structural tissue that example 2 adopts Foam silver loading nano silvery of the present invention
detailed description of the invention:
Embodiment 1:
Preferred dimension specification is 100mm × 100mm, thickness is 0.3mm, porosity is the Foam silver prepared of Jiangsu Ge Ye new material Co., Ltd of 80%, dripping 1.5ml concentration is the liquor argenti nitratis ophthalmicus of 0.25M, because Foam silver has good adsorptivity, now liquor argenti nitratis ophthalmicus will be diffused into the whole surface of Foam silver quickly and evenly, and the solution added is adsorbed in Foam silver completely, then the baking oven interior dehydration 0.5h of 80 DEG C of temperature is placed in, transfer them to after completing in chamber type electric resistance furnace, be heated to the decomposition reaction that 500 DEG C are carried out silver nitrate, its decomposition reaction temperature retention time elects 2h as, again it is placed in after cooling in the reduction furnace of hydrogen nitrogen mixed gas atmosphere, reduction treatment temperature is 800 DEG C, temperature retention time is 0.5h.First pass into nitrogen and carry out prepurging, and heat under nitrogen protection, wherein hydrogen nitrogen mixed gas passes at 500 DEG C, wherein H
2and N
2mol ratio be the mist of 1:5, namely density of hydrogen is 20%, and reducing atmosphere remains to always and cools to room temperature with the furnace, can obtain the Foam silver loaded with nano ag material with loose structure like this.Utilize the material of field emission scanning electron microscope to above-mentioned Foam silver loading nano silvery to carry out observation analysis, its micro-structural as shown in Figure 1.
Embodiment 2:
Preferred dimension specification is 100mm × 100mm, thickness is 0.5mm, porosity is the Foam silver prepared of Jiangsu Ge Ye new material Co., Ltd of 75%, dripping 2ml concentration is the liquor argenti nitratis ophthalmicus of 0.75M, this Foam silver material has good adsorptivity, now liquor argenti nitratis ophthalmicus can be observed and will be diffused into the whole surface of Foam silver quickly and evenly, and the solution added is adsorbed in Foam silver completely, then the baking oven interior dehydration 0.5h of 80 DEG C of temperature is placed in, transfer them to after completing in chamber type electric resistance furnace, be heated to the decomposition reaction that 500 DEG C are carried out silver nitrate, its decomposition reaction temperature retention time elects 2h as, again it is placed in after cooling in the reduction furnace of hydrogen nitrogen mixed gas atmosphere, reduction treatment temperature is 800 DEG C, temperature retention time is 0.5h.First pass into nitrogen and carry out prepurging, and heat under nitrogen protection, wherein hydrogen nitrogen mixed gas passes at 500 DEG C, wherein H
2and N
2mol ratio be the mist of 1:5, namely density of hydrogen is 20%, and reducing atmosphere remains to always and cools to room temperature with the furnace, can obtain the Foam silver loaded with nano ag material with loose structure like this.Utilize the material of field emission scanning electron microscope to above-mentioned Foam silver loading nano silvery to carry out observation analysis, its micro-structural as shown in Figure 2, can observe the particle surface that a large amount of nano-Ag particles is attached to Foam silver.
Claims (6)
1. a preparation method for Foam silver loaded with nano ag material, is characterized in that comprising the following steps:
(1) first select the Foam silver of a certain specification as carrier, certain density liquor argenti nitratis ophthalmicus is evenly added drop-wise on Foam silver carrier;
(2) then the Foam silver with silver nitrate is placed in baking oven and carries out processed;
(3) after dehydration, the Foam silver material of absorption silver nitrate is carried out pyrolytic process in a furnace;
(4) finally by the material after resolution process, in reducing atmosphere, carry out reduction treatment, obtain Foam silver loaded with nano ag material.
2. the preparation method of Foam silver loaded with nano ag material according to claim 1, is characterized in that the concentration of the liquor argenti nitratis ophthalmicus described in step 1 is 0.001 ~ 3M.
3. the preparation method of Foam silver loaded with nano ag material according to claim 1, is characterized in that the baking oven dehydration 0.3 ~ 1 hour being placed in 80 ~ 100 DEG C in step 2 with the Foam silver of silver nitrate.
4. the preparation method of Foam silver loaded with nano ag material according to claim 1, it is characterized in that the Foam silver material adsorbing silver nitrate in step 3 is under 400 ~ 600 DEG C of conditions, insulation is 0.3 ~ 2 hour, so that silver nitrate realizes decomposition reaction.
5. the preparation method of Foam silver loaded with nano ag material according to claim 1, is characterized in that the atmosphere temperature of the reduction treatment of step 4 is chosen as 400 ~ 900
oc, namely obtains Foam silver loaded with nano ag material.
6. the preparation method of Foam silver loaded with nano ag material according to claim 1, is characterized in that the reducing atmosphere described in step 4 is hydrogen-nitrogen mixture gas or pure hydrogen, wherein H
2concentration be 10% ~ 100%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410494581.9A CN105499595A (en) | 2014-09-25 | 2014-09-25 | Preparing method of foamed silver material carrying nano silver |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410494581.9A CN105499595A (en) | 2014-09-25 | 2014-09-25 | Preparing method of foamed silver material carrying nano silver |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105499595A true CN105499595A (en) | 2016-04-20 |
Family
ID=55708107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410494581.9A Pending CN105499595A (en) | 2014-09-25 | 2014-09-25 | Preparing method of foamed silver material carrying nano silver |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105499595A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106319579A (en) * | 2016-08-25 | 2017-01-11 | 山东清大银光金属海绵新材料有限责任公司 | Method for preparing disinfection electrode material with copper sponge-based silver thin film loaded with nano particles |
| CN111349918A (en) * | 2020-03-09 | 2020-06-30 | 广东四维新材料有限公司 | Manufacturing method and process application of foamed silver |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007016258A (en) * | 2005-07-05 | 2007-01-25 | Mitsui Mining & Smelting Co Ltd | High crystal silver powder, and method for producing the high crystal silver powder |
| CN101054218A (en) * | 2007-05-30 | 2007-10-17 | 山东大学 | Nano silver composite antibacterial material using porous ceramics as carrier and preparation method thereof |
| CN102218296A (en) * | 2011-04-24 | 2011-10-19 | 大连理工大学 | Method for preparing carbon nanofiber-supported carbon foam and method for applying nanofiber-supported carbon foam to adsorption of greasy dirt |
| CN103801705A (en) * | 2014-02-11 | 2014-05-21 | 常州大学 | Method for loading nanocrystalline metal oxide or nanocrystalline metal materials by porous carbon |
| CN103862031A (en) * | 2014-02-20 | 2014-06-18 | 天津大学 | Composite nano metal materials prepared in combination with ordered porous support or rough surface and method thereof |
-
2014
- 2014-09-25 CN CN201410494581.9A patent/CN105499595A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007016258A (en) * | 2005-07-05 | 2007-01-25 | Mitsui Mining & Smelting Co Ltd | High crystal silver powder, and method for producing the high crystal silver powder |
| CN101054218A (en) * | 2007-05-30 | 2007-10-17 | 山东大学 | Nano silver composite antibacterial material using porous ceramics as carrier and preparation method thereof |
| CN102218296A (en) * | 2011-04-24 | 2011-10-19 | 大连理工大学 | Method for preparing carbon nanofiber-supported carbon foam and method for applying nanofiber-supported carbon foam to adsorption of greasy dirt |
| CN103801705A (en) * | 2014-02-11 | 2014-05-21 | 常州大学 | Method for loading nanocrystalline metal oxide or nanocrystalline metal materials by porous carbon |
| CN103862031A (en) * | 2014-02-20 | 2014-06-18 | 天津大学 | Composite nano metal materials prepared in combination with ordered porous support or rough surface and method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106319579A (en) * | 2016-08-25 | 2017-01-11 | 山东清大银光金属海绵新材料有限责任公司 | Method for preparing disinfection electrode material with copper sponge-based silver thin film loaded with nano particles |
| CN106319579B (en) * | 2016-08-25 | 2018-04-13 | 山东清大银光金属海绵新材料有限责任公司 | The preparation method of the copper-based Ag films load nano particle sterilization electrode material of sponge |
| CN111349918A (en) * | 2020-03-09 | 2020-06-30 | 广东四维新材料有限公司 | Manufacturing method and process application of foamed silver |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107447231B (en) | One kind two cobaltous telluride electro-catalysis analysis O compoiste material and its preparation method and application | |
| CN105951123B (en) | A kind of preparation method of NiCoP nano wires electro catalytic electrode | |
| CN104630822B (en) | Foam transition-metal solid/gas-state phosphated self-support hydrogen evolution electrode and preparation method thereof | |
| KR101801789B1 (en) | Porous carbon materials and methods of manufacturing the same | |
| CN106048650B (en) | The preparation method of 3D porous electrodes and its application in electrochemistry evolving hydrogen reaction | |
| CN100537422C (en) | Method for preparing hollow micrometre carbon ball with structured size | |
| CN107051568A (en) | One kind analysis oxygen Fe two cobaltous selenide@N CT composite catalysts of doping and its preparation method and application | |
| CN110148760B (en) | Porous carbon-carbon nanotube composite material and preparation method and application thereof | |
| CN106975426B (en) | High stability Catalytic Layer and preparation method thereof in micro passage reaction | |
| Ye et al. | Hierarchically structured carbon materials derived from lotus leaves as efficient electrocatalyst for microbial energy harvesting | |
| CN107159268B (en) | Hollow molybdenum disulfide/molybdenum trioxide flower-shaped heterostructure nano material, preparation method and application | |
| CN107630227A (en) | A kind of method that three-D nano-porous copper mesh elctro-catalyst is prepared based on metal net | |
| KR20170072065A (en) | Nitrogen-doped graphene aggregate and method of preparing the same | |
| Peng et al. | Construction of ZnO nanosheet arrays within BiVO4 particles on a conductive magnetically driven cilia film with enhanced visible photocatalytic activity | |
| Amer et al. | Enriched active surface structure in nanosized tungsten-cobalt oxides electrocatalysts for efficient oxygen redox reactions | |
| KR20160074291A (en) | Hydrogen sensor based on platinum/palladium-graphene hybrid and method of fabricating the same | |
| CN105161730B (en) | Air cathode and microbiological fuel cell | |
| Kong et al. | Hydrothermal synthesis of nanoporous NiO rods self-supported on Ni foam as efficient electrocatalysts for hydrogen evolution reaction | |
| Jiang et al. | Dimension conversion: from a 1D metal–organic gel into a 3D metal–organic porous network with high-efficiency multiple enzyme-like activities for cascade reactions | |
| Ren et al. | Mesoporous microcapsules with noble metal or noble metal oxide shells and their application in electrocatalysis | |
| CN105499595A (en) | Preparing method of foamed silver material carrying nano silver | |
| CN109876869A (en) | Titanium diboride surface cladding functional film material of core-shell structure and the preparation method and application thereof | |
| CN103539090B (en) | High orientation arrayed carbon nitride nanorod array and preparation method thereof | |
| Zhang et al. | Facile fabrication of large scale microtubes with a natural template—Kapok fiber | |
| Kim et al. | Fabrication of iridium oxide nanoparticles supported on activated carbon powder by flashlight irradiation for oxygen evolutions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160420 |
|
| WD01 | Invention patent application deemed withdrawn after publication |