CN104625084A - Colorless nano-silver sol preparation and preservation method utilizing cryogenic technology - Google Patents
Colorless nano-silver sol preparation and preservation method utilizing cryogenic technology Download PDFInfo
- Publication number
- CN104625084A CN104625084A CN201410850968.3A CN201410850968A CN104625084A CN 104625084 A CN104625084 A CN 104625084A CN 201410850968 A CN201410850968 A CN 201410850968A CN 104625084 A CN104625084 A CN 104625084A
- Authority
- CN
- China
- Prior art keywords
- silver
- nano silver
- reducing agent
- colloidal sol
- sorbet
- 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.)
- Granted
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a colorless nano-silver sol preparation and preservation method utilizing a cryogenic technology. The method comprises the steps that 1, raw materials including silver are added into water, uniform mixing is conducted to obtain a water solution of the raw materials including the silver, and freezing and smashing are conducted to obtain an iced blend of the raw materials including the silver; 2, a reducing agent is added into water, uniform mixing is conducted to obtain a water solution including the reducing agent, and freezing and smashing are conducted to obtain an iced blend including the reducing agent; 3, the iced blend of the raw materials including the silver obtained in step 1 and the iced blend including the reducing agent obtained in step 2 are mixed and grinded to obtain ice crystals including nano-silver; 4, the ice crystals including nano-silver obtained in step 3 are preserved. The colorless nano-silver sol preparation and preservation method utilizing the cryogenic technology has the advantages that pyroreaction, a separation process, a protective agent and a dispersing agent are all omitted, and the obtained nano-silver is small in crystal nucleus, and high in activity, purity and safety.
Description
Technical field
The invention belongs to technical field of nano material, relate to cryogenic technique solid phase and prepare nano material, more specifically utilize cryogenic technique to prepare for a kind of and preserve the method for colourless nano silver colloidal sol.
Background technology
Particle diameter is accomplished nano level argent simple substance by Nano Silver exactly.It is reported that Nano Silver all has broad application prospects in fields such as anti-biotic material, effective catalyst, lubricant, light absorbing material, coating, sensor, electrocondution slurry, high performance electrode materials, become and there is the functional material theoretical research of property and the important topic of application and development.As added a small amount of Nano Silver in chemical fibre, some performance of chemical fibre product can be improved, and make it have very strong sterilizing ability; Adulterate appropriate Nano Silver in silicon oxide film, and the glass of this film of plating can be made to have certain Photoluminescence; Be coated with burn wound and cureless hemorrhoid with Nanometer silver dressing, can achieve good results.
At present, mainly there is following problem in the preparation of Nano Silver and store method:
1) preparation method of Nano Silver is based on methods such as support methods/template, sol-gel process, solid phase method, irradiation methods at present, and step is more, preparation technology is wayward, and preparation condition is harsh;
2) Nano Silver preparation method is shown in the process-intensive of bibliographical information at present, and the Nano Silver prepared varies in color, and the changes colour along with particle diameter presents glassy yellow, brown color, brownish red, aubergine, bluish violet and brown etc.Chinese patent 200410069105.9 discloses a kind of preparation method of nano silver colloid aqueous solution; the method adopts double injecting control technology; under the stirring of agitator; the Dual Implantations while of silver-colored ammonia spirit and the reducing agent aqueous solution is contained in the reaction system of the protective agent aqueous solution; generate nano silver particles; through ultrafiltration desalination, obtain the nano silver colloid aqueous solution of nanometer.200810143657.8 preparation methods disclosing a kind of Nano Silver, its principal character is reaction environment with high-pressure sterilizing pot, and utilize silver nitrate for silver-colored source, the polysaccharide materials such as soluble starch, as protective agent, prepare nano silver colloidal sol.201010215387.4 preparation methods disclosing a kind of nano silver colloidal sol, it comprises the following steps, and a) is dissolved in ultra-pure water by silver nitrate, obtains liquor argenti nitratis ophthalmicus; B) with liquor argenti nitratis ophthalmicus described in agitator rapid stirring; C) heat described liquor argenti nitratis ophthalmicus by oil bath, after being heated to uniform temperature, reduce the mixing speed of described agitator; D) continue to pass into liquor argenti nitratis ophthalmicus described in hydrogen reducing and obtain nano silver colloidal sol.201310574416.X disclose a kind of nano silver colloidal sol and preparation and purification method thereof; adopt silver salt, protective agent and cosolvent; take water as solvent; by silver salt solution, protective agent aqueous solution; add the reduction of a certain amount of reducing agent; obtain initial nano silver colloidal sol, this colloidal sol through adjust ph, precipitation, separation, washing, heavy molten after obtain the nano silver colloidal sol of required concentration.A kind of preparation method of nano silver colloidal sol of 201410344102.5 disclosure of the invention, mixes liquor argenti nitratis ophthalmicus or silver ammino solution with poly-D-lysine is water-soluble, stirring reaction 30-180min under the condition of 50-100 DEG C, obtains nano silver colloidal sol.
Above invention existence utilizes protective agent, protection gas, elevated temperature heating stage, and the Nano Silver size distribution obtained is wide, wayward, and unstable properties, preserves perishable problem.And the use of a large amount of protective agent and dispersant etc. brings problem inevitably to the application security of nano-class silver colloidal solution.The fields harsh to color requirements such as weaving year silver that are applied in color nano silver colloidal sol are restricted.
Be with the deficiencies, particularly coloured nano silver colloidal sol such as the general particle diameter of coloured nano silver colloidal sol is large, domain size distribution is wide to carry silver-colored field in weaving in prior art and be subject to significant limitation.
And water white transparency nano silver colloidal sol prepared by the present invention can overcome that above-mentioned particle diameter is large, domain size distribution is wide and be with coloured deficiency, have that particle diameter is little, narrow particle size distribution, an advantage such as colourless, a limitation of carrying the application of silver-colored field in weaving can be eliminated.
Summary of the invention
Technical problem to be solved by this invention is, in view of Nano Silver in prior art must add protective agent in preparation process, and dispersant, and also coloured Nano Silver also makes the use field of nano silver colloidal sol be restricted.The invention provides a kind of method utilizing cryogenic technique preparation and preserve colourless nano silver colloidal sol; described preparation method does not need protective agent, dispersant; also do not need separation process, and the colourless Nano Silver of preparation has that granularity is little, purity is high and the advantage such as easy preservation.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
Utilize cryogenic technique to prepare and preserve a method for colourless nano silver colloidal sol, comprising the following steps:
1) will be added to the water containing silver material, and mix, and obtain the aqueous solution containing silver material, freezing, pulverizing, obtains the Sorbet containing silver material;
2) reducing agent is added to the water, mixes, obtain the aqueous solution containing reducing agent, freezing, pulverize, obtain the Sorbet containing reducing agent;
3) step 1) obtain containing the Sorbet of silver material and step 2) Sorbet obtained containing reducing agent mixes, grinds, obtain Nano Silver ice crystal;
4) step 3 is preserved) the Nano Silver ice crystal that obtains.
Further, step 1) in, described is silver nitrate containing silver material, and in described silver nitrate aqueous solution, the molar concentration of silver nitrate is 0.1-0.5mol/L.
Further, step 2) in, the molar concentration of described reducing agent is 0.1-0.5mol/L.
Further, step 2) in, described reducing agent is one or more in ascorbic acid, hydrazine hydrate, hydrogen peroxide.
Further, step 1) and step 2) in, described cryogenic temperature is-4 DEG C to-24 DEG C, cooling time 8-24h; Described grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C to-18 DEG C.
Further, step 3) in, in described reaction, the mol ratio of silver material and reducing agent is 4:3-2:1.
Further, step 3) in, described milling time is 12-48h, and grind size is 0.1-0.3 μm, and temperature during grinding is-15 DEG C to-18 DEG C.
Further, step 4) in, described preservation condition is-4 DEG C to-24 DEG C, can preserve 3 years.
The invention has the beneficial effects as follows:
The method of preparation of the present invention and preservation Nano Silver is reacted at low temperatures; direct use is reacted at low temperatures containing silver material (liquor argenti nitratis ophthalmicus) and reducing agent; without the need to protective atmosphere; protective agent, dispersant is not needed yet; do not need follow-up separation process; time to be used directly with required compound material with the use of, preparation method is simple.
Because reaction carries out under low-temperature condition, the nanocrystal of reaction is little, does not need protective agent, dispersant, directly prepares colourless nano silver colloidal sol ice crystal, and the product be obtained by reacting adopts cryogenic technique to preserve, and stability is high, the holding time is long.
Detailed description of the invention
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Utilize cryogenic technique to prepare and preserve a method for colourless nano silver colloidal sol, comprising the following steps:
1) silver nitrate is added to the water, mix, obtain silver nitrate aqueous solution (in silver nitrate aqueous solution, the molar concentration of silver nitrate is 0.1-0.5mol/L), freezing 8-24h under-4 DEG C to-24 DEG C conditions, be placed on afterwards in the Sorbet machine with low temperature chuck and pulverize, grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C to-18 DEG C, obtains the Sorbet containing silver material;
2) one or more of ascorbic acid, hydrogen peroxide or hydrazine hydrate are added to the water, mix, obtain the aqueous solution (wherein the molar concentration of reducing agent is 0.1-0.5mol/L) containing reducing agent, freezing 8-24h under-4 DEG C to-24 DEG C conditions, be placed on afterwards in the Sorbet machine with low temperature chuck and pulverize under-15 DEG C to-18 DEG C conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing reducing agent;
3) step 1) obtain containing the Sorbet of silver material and step 2) Sorbet obtained containing reducing agent is placed in freezing agitating ball mill simultaneously and mixes, temperature during mixing is-15 DEG C to-18 DEG C, 12-48h is ground under-15 DEG C to-18 DEG C conditions, granularity after grinding is 0.1-0.3 μm, obtains colourless Nano Silver ice crystal;
4) by step 3) in colourless Nano Silver ice crystal take out and be placed on-4 DEG C to-24 DEG C preservations.
Embodiment 1
1) 8.5g silver nitrate silver is added in 100mL water, mix, obtain the silver nitrate aqueous solution of 0.5mol/L, under-4 DEG C of conditions after cooling time 8h, be placed in the Sorbet machine with low temperature chuck and pulverize under-15 DEG C to-18 DEG C conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing silver material;
2) 4.5g ascorbic acid is added in 250mL water, mix, obtain 0.1mol/L aqueous ascorbic acid,-4 DEG C of freezing 8h, be placed in the Sorbet machine with low temperature chuck and pulverize under-15 DEG C to-18 DEG C conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing ascorbic acid;
3) step 1) obtain containing the Sorbet of silver material and step 2) Sorbet obtained containing ascorbic acid is placed in freezing agitating ball mill simultaneously and mixes, temperature during mixing is-15 DEG C to-18 DEG C, 12h is ground under-15 DEG C to-18 DEG C conditions, granularity after grinding is 0.1-0.3 μm, obtains colourless Nano Silver ice crystal 359.3g;
4) by step 3) in colourless Nano Silver ice crystal take out and be placed on-4 DEG C of preservations.
Embodiment 2
1) 8.5g silver nitrate is added in 500mL water, mix, obtain 0.1mol/L silver nitrate aqueous solution, freezing 24h under-15 DEG C of conditions, be placed in the Sorbet machine with low temperature chuck and pulverize, grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C to-18 DEG C, obtains the Sorbet containing silver material;
2) the hydrazine hydrate 2.2mL of mass fraction 85% is got, be diluted with water 75mL, obtain the aqueous solution of hydrazine hydrate (wherein, the molar concentration 0.5mol/L of hydrazine hydrate), freezing 24h under-15 DEG C of conditions, be placed in the Sorbet machine with low temperature chuck and pulverize under-15 DEG C to-18 DEG C conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing hydrazine hydrate;
3) step 1) obtain containing the Sorbet of silver material and step 2) Sorbet obtained containing hydrazine hydrate is placed in freezing agitating ball mill simultaneously and mixes, temperature during mixing is-15 DEG C to-18 DEG C, 48h is ground under-15 DEG C to-18 DEG C conditions, granularity after grinding is 0.1-0.3 μm, obtains colourless Nano Silver ice crystal 577.5g;
4) by step 3) in colourless Nano Silver ice crystal take out and be placed on-15 DEG C of preservations.
Embodiment 3
1) 8.5g silver nitrate is added in 125mL water, mix, obtain silver nitrate aqueous solution (wherein, the molar concentration 0.4mol/L of silver nitrate), freezing 10h under-24 DEG C of conditions, be placed on afterwards in the Sorbet machine with low temperature chuck and pulverize under-15 DEG C to-18 DEG C conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing silver material;
2) get the hydrogen peroxide 2.5mL of 30%, be diluted with water 125mL, obtain 0.2mol/L hydrogen peroxide solution,-24 DEG C of freezing 10h, be placed on afterwards in the Sorbet machine with low temperature chuck and pulverize under 15 DEG C to-18 DEG C of conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing hydrogen peroxide;
3) step 1) obtain containing the Sorbet of silver material and step 2) Sorbet obtained containing hydrogen peroxide is placed in freezing agitating ball mill simultaneously and mixes, temperature during mixing is-15 DEG C to-18 DEG C, 24h is ground under-15 DEG C to-18 DEG C conditions, granularity after grinding is 0.1-0.3 μm, obtains colourless Nano Silver ice crystal 255.5g;
4) by step 3) in colourless Nano Silver ice crystal take out and be placed on-24 DEG C of preservations.
Embodiment 4
1) 8.5g silver nitrate is added in 100mL water, mix, obtain the silver nitrate aqueous solution of 0.5mol/L, under-24 DEG C of conditions after cooling time 8h, be placed in the Sorbet machine with low temperature chuck and pulverize under-15 DEG C to-18 DEG C conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing silver material;
2) 2.25g ascorbic acid is added in 125mL water, mix, obtain 0.1mol/L aqueous ascorbic acid; Get the hydrogen peroxide 2.0mL of 30%, be diluted with water 102.5mL, obtain 0.2mol/L hydrogen peroxide solution; By 0.1mol/L aqueous ascorbic acid obtained above with obtain 0.2mol/L hydrogen peroxide solution and mix, freezing 8h under being placed in-24 DEG C of conditions, be placed in the Sorbet machine with low temperature chuck and pulverize under-15 DEG C to-18 DEG C conditions, grinding particle size is 1-3 μm, obtains the Sorbet containing ascorbic acid and hydrogen peroxide;
3) step 1) obtain containing the Sorbet of silver material and step 2) Sorbet obtained containing ascorbic acid and hydrogen peroxide is placed in freezing agitating ball mill simultaneously and mixes, temperature during mixing is-15 DEG C to-18 DEG C, 12h is ground under-15 DEG C to-18 DEG C conditions, granularity after grinding is 0.1-0.3 μm, obtains colourless Nano Silver ice crystal 334.5g;
4) by step 3) in colourless Nano Silver ice crystal take out and be placed on-24 DEG C of preservations.
Embodiment 5
The nano silver colloidal sol prepared in currently available technology is general all with color.Such as: the prior art (research of glycol method synthesizing stable nano silver colloidal sol, chemistry world, 5th phase 257-259 in 2009) color of nano silver colloidal sol for preparing, present brown color, milky, brown, rufous, khaki, lark, orange etc.; The nano silver colloidal sol that prior art (taking electro-conductive glass as the research of electrode ultrasonic electrolysis synthesis of nano silver sol, chemistry world, calendar year 2001 the 6th phase 323-326) prepares is rufous, green, celadon, brown, yellow green etc.And be water white transparency nano silver colloidal sol by the nano silver colloidal sol prepared by the present invention.
Embodiment 6
Coloured nano silver colloidal sol that the colourless nano silver colloidal sol stability of cryogenic technique synthesis is prepared than prior art is better, existing coloured nano silver colloidal sol shelf-life mostly is 2 years most, the general shelf-life is 6-12 month, easily there is the phenomenon of layering, sedimentation in the change by external environment, thus lose the stability of colloidal sol, and the colourless nano silver colloidal sol that the present invention utilizes cryogenic technique to synthesize, shelf-life is at least 3 years, through the nano silver colloidal sol ice crystal that 3 years preserve, compositely with other raw material after thawing the effect of brand-new for nano silver colloidal sol can be reached.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included in this, within bright protection domain.
Claims (8)
1. utilize cryogenic technique to prepare and preserve a method for colourless nano silver colloidal sol, it is characterized in that, comprise the following steps:
1) will be added to the water containing silver material, and mix, and obtain the aqueous solution containing silver material, freezing, pulverizing, obtains the Sorbet containing silver material;
2) reducing agent is added to the water, mixes, obtain the aqueous solution containing reducing agent, freezing, pulverize, obtain the Sorbet containing reducing agent;
3) step 1) obtain containing the Sorbet of silver material and step 2) Sorbet obtained containing reducing agent mixes, grinds, obtain Nano Silver ice crystal;
4) step 3 is preserved) the Nano Silver ice crystal that obtains.
2. a kind ofly according to claim 1 utilize cryogenic technique to prepare and preserve the method for colourless nano silver colloidal sol, it is characterized in that, step 1) in, described is silver nitrate containing silver material; In described silver nitrate aqueous solution, the molar concentration of silver nitrate is 0.1-0.5mol/L.
3. a kind ofly according to claim 1 utilize cryogenic technique to prepare and preserve the method for colourless nano silver colloidal sol, it is characterized in that, step 2) in, be describedly 0.1-0.5mol/L containing the molar concentration of reducing agent in the aqueous solution of reducing agent.
4. a kind ofly according to claim 1 utilize cryogenic technique to prepare and preserve the method for colourless nano silver colloidal sol, it is characterized in that, step 2) in, described reducing agent is one or more in hydrogen peroxide, ascorbic acid or hydrazine hydrate.
5. a kind ofly according to claim 1 utilize cryogenic technique to prepare and preserve the method for colourless nano silver colloidal sol, it is characterized in that, in the described molal quantity containing silver in the Sorbet of silver material and described reducing agent Sorbet, the mole ratio of reducing agent is 4:3 to 2:1.
6. a kind of method utilizing cryogenic technique preparation and preserve colourless nano silver colloidal sol according to any one of claim 1 to 5, is characterized in that, step 1) and step 2) in, described cryogenic temperature is-4 DEG C to-24 DEG C, cooling time 8-24h; Described grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C to-18 DEG C.
7. a kind of method utilizing cryogenic technique preparation and preserve colourless nano silver colloidal sol according to any one of claim 1 to 5, it is characterized in that, step 3) in, described milling time is 12-48h, grind size is 0.1-0.3 μm, and temperature during grinding is-15 DEG C to-18 DEG C.
8. a kind of method utilizing cryogenic technique preparation and preserve colourless nano silver colloidal sol according to any one of claim 1 to 5, is characterized in that, step 4) in, described preservation condition is-4 DEG C to-24 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410850968.3A CN104625084B (en) | 2014-12-31 | 2014-12-31 | A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410850968.3A CN104625084B (en) | 2014-12-31 | 2014-12-31 | A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104625084A true CN104625084A (en) | 2015-05-20 |
| CN104625084B CN104625084B (en) | 2016-08-24 |
Family
ID=53204580
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410850968.3A Active CN104625084B (en) | 2014-12-31 | 2014-12-31 | A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104625084B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113770370A (en) * | 2021-08-18 | 2021-12-10 | 清华大学 | Silver powder and preparation method thereof, silver paste and photovoltaic cell |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101384388A (en) * | 2006-03-10 | 2009-03-11 | 三井金属矿业株式会社 | Process for production of ultrafine silver particles and ultrafine silver particles produced by the process |
| RU2451578C1 (en) * | 2010-11-30 | 2012-05-27 | Общество с ограниченной ответственностью Научно Производственный Центр "Квадра" | Method of producing biocide inorganic zinc oxide-based composite nanoparticles |
| CN102699341A (en) * | 2012-04-26 | 2012-10-03 | 蔡雄辉 | Wet-chemical preparation method for silver micro/nanowires |
| CN103302307A (en) * | 2013-06-25 | 2013-09-18 | 通化师范学院 | Preparation method of silver nano particles and method for facilitating germination of cucumber seeds and growth and development of seedlings with silver nano particles |
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
| KR20140038845A (en) * | 2012-09-21 | 2014-03-31 | 제주대학교 산학협력단 | Method for preparing linear metal nanoparticles |
-
2014
- 2014-12-31 CN CN201410850968.3A patent/CN104625084B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101384388A (en) * | 2006-03-10 | 2009-03-11 | 三井金属矿业株式会社 | Process for production of ultrafine silver particles and ultrafine silver particles produced by the process |
| RU2451578C1 (en) * | 2010-11-30 | 2012-05-27 | Общество с ограниченной ответственностью Научно Производственный Центр "Квадра" | Method of producing biocide inorganic zinc oxide-based composite nanoparticles |
| CN102699341A (en) * | 2012-04-26 | 2012-10-03 | 蔡雄辉 | Wet-chemical preparation method for silver micro/nanowires |
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
| KR20140038845A (en) * | 2012-09-21 | 2014-03-31 | 제주대학교 산학협력단 | Method for preparing linear metal nanoparticles |
| CN103302307A (en) * | 2013-06-25 | 2013-09-18 | 通化师范学院 | Preparation method of silver nano particles and method for facilitating germination of cucumber seeds and growth and development of seedlings with silver nano particles |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113770370A (en) * | 2021-08-18 | 2021-12-10 | 清华大学 | Silver powder and preparation method thereof, silver paste and photovoltaic cell |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104625084B (en) | 2016-08-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Huignard et al. | Synthesis and luminescence properties of colloidal YVO4: Eu phosphors | |
| Yang et al. | Size and shape controllable synthesis and luminescent properties of BaGdF5: Ce3+/Ln3+ (Ln= Sm, Dy, Eu, Tb) nano/submicrocrystals by a facile hydrothermal process | |
| CN102079975B (en) | Coprecipitation preparation method of rare earth doped yttrium aluminum garnet fluorescent powder | |
| CN103496724B (en) | The preparation method of a kind of nano alumina sol and gel | |
| Liu et al. | Microwave synthesis and luminescent properties of YVO4: Ln3+ (Ln= Eu, Dy and Sm) phosphors with different morphologies | |
| Wang et al. | Controlled hydrothermal growth and tunable luminescence properties of β-NaYF4: Yb3+/Er3+ microcrystals | |
| CN102757081B (en) | Synthesis method of cerium oxide hydrosol dispersed by PVA (Polyvinyl Alcohol) | |
| CN108585048A (en) | A kind of preparation method of the caesium doping tungsten bronze nano-powder with near-infrared shielding properties | |
| CN108862362B (en) | Preparation method of micron-sized cerium oxide powder | |
| He et al. | Luminescence properties of Eu3+/CDs/PVA composite applied in light conversion film | |
| CN108585014A (en) | A series of micro-/ nano rare earth materials and preparation method thereof | |
| Fu et al. | Comparative study of synthesis and characterization of monodispersed SiO2@ Y2O3: Eu3+ and SiO2@ Y2O3: Eu3+@ SiO2 core–shell structure phosphor particles | |
| Li et al. | Tunable magnetic and fluorescent properties of Tb3Ga5O12 nanoparticles doped with Er3+, Yb3+, and Sc3+ | |
| Liu et al. | Synthesis and photophysical properties of crystalline [EuW10O36] 9--based polyoxometalates with lanthanide ions as counter cations | |
| Qian et al. | Preparation and luminescence properties of Eu3+ incorporated in CaCO3 nanocrystals with multiple sites | |
| Li et al. | Room-temperature fluorination of layered rare-earth hydroxide nanosheets leading to fluoride nanocrystals and elucidation of down-/up-conversion photoluminescence | |
| CN104625084B (en) | A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol | |
| Wang et al. | Effects of different organic additives on the formation of YVO4: Eu3+ microspheres under hydrothermal conditions | |
| CN107032401B (en) | Sodium bismuth molybdate nano material and preparation method thereof | |
| Wenyuan et al. | Sonochemical synthesis and photoluminescence properties of rare-earth phosphate core/shell nanorods | |
| Li et al. | Structure, properties and application of Eu3+ doped bismuth molybdate red-emitting phosphor synthesized by sol-gel method | |
| CN105948135B (en) | A kind of monodisperse porous magnetic sub-micro ball and preparation method thereof | |
| CN101712455B (en) | Method for directly chemically synthesizing rare-earth vanadium-doped yttrium phosphate nanocrystalline material | |
| Cui et al. | Synthesis of Tb3+ doped SrMoO4/SiO2 nanophosphor and its sensing properties for inorganic ions and tyrosine | |
| Yang et al. | EDTA-mediated morphology and tunable optical properties of Eu 3+-doped NaY (MoO 4) 2 phosphor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A method of preparing and preserving colorless nano silver sol by low temperature technology Effective date of registration: 20221111 Granted publication date: 20160824 Pledgee: Yantai Fushan huiran Private Capital Management Co.,Ltd. Pledgor: YANTAI JIALONG NANO INDUSTRY CO.,LTD. Registration number: Y2022980021675 |