CN105002552A - Iridium mesoscopic crystal synthesis method - Google Patents
Iridium mesoscopic crystal synthesis method Download PDFInfo
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- CN105002552A CN105002552A CN201410148004.4A CN201410148004A CN105002552A CN 105002552 A CN105002552 A CN 105002552A CN 201410148004 A CN201410148004 A CN 201410148004A CN 105002552 A CN105002552 A CN 105002552A
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Abstract
The present invention provides an iridium mesoscopic crystal synthesis method, which comprises: preparing an aqueous solution of chloroiridic acid, PEG-400 and 2,7-dihydroxynaphthalene, adjusting the pH value of the solution to achieve an alkaline state with a pH value adjusting agent, and placing the solution in an ultraviolet illumination environment to irradiate. According to the present invention, the dispersant concentration, the reducing agent concentration, the iridium source concentration and the ultraviolet illumination time importantly affect the morphology and the size of the iridium mesoscopic crystal, such that the iridium mesoscopic crystals with characteristics of different morphologies, different sizes and good dispersion can be prepared; and the method has characteristics of simpleness, green environmental protection and no requirement of consumption of a lot of energy sources, and can be used for industrial production.
Description
Technical field
The present invention relates to a kind of iridium Jie and see brilliant synthetic method, particularly relate to a kind of photochemical syntheses legal system that utilizes and see the method for crystalline substance for iridium Jie.
Background technology
Iridium is one of metal that erosion resistance is the strongest, be the metal uniquely still keeping excellent mechanical property in a kind of air more than 1600 DEG C, and it can present superconductor character at 0.14 below K.The features such as the high-melting-point of iridium, high stability, electric conductivity are high and corrosion-resistant make it have important use at a lot of special occasions.Such as, the high-temperature oxidation resistance of iridium and thermoelectricity capability make iridium/iridium rhodium thermocouple become only and can measure the Precious Metals Temperature-measurement Materials reaching 2100 DEG C of high temperature in an atmosphere; Iridium can be used as the container material of radioactive heat source; Anodic iridium oxide film is a kind of promising electric colour development material.Meanwhile, iridium nanocatalyst is also widely used in the fields such as aerospace, vehicle maintenance service and new forms of energy.
Size and pattern are the important factors affecting the mechanics of materials, electricity and optical property, therefore, make nanoparticle be assembled into the superstructure material of different size and pattern, it can be made more effectively to be applied in nanoelectronic, photoelectricity and sensor and manufacture field.The sight crystalline substance that is situated between is a kind of by the nano particle ordered crystal combined.And at present, also do not have a kind of preparation method of environmental protection effectively can control iridium combinations of nanoparticles and become iridium Jie of different size and pattern to see brilliant.
Summary of the invention
Main purpose of the present invention is to provide a kind of environmental protection, the simple iridium of preparation technology is situated between and sees brilliant synthetic method.
For realizing above-mentioned main purpose, the invention provides a kind of iridium Jie and see brilliant synthetic method, it comprises the following steps: the aqueous solution of preparation chloro-iridic acid, PEG-400 and 2,7 dihydroxy naphthalene, and by pH adjusting agent, the pH value of solution is adjusted to alkalescence; Solution is positioned in ultraviolet lighting environment and irradiates.
By concentration and the ultraviolet lighting time in the PEG-400 of control as dispersion agent, the 2,7 dihydroxy naphthalene as reductive agent, iridium source, the iridium that can synthesize different-shape and size is situated between and sees crystalline substance.Utilize PEG-400 as dispersion agent, iridium can be prevented to be situated between and see the raw reunion of trichite.Iridium is situated between and sees crystalline substance the used time is not placed in solution and stores, and takes out and depend on carrier when needing to use from solution.
Concrete, in solution, the mol ratio of iridium, 2,7 dihydroxy naphthalene and PEG-400 is 1:1 ~ 30:1 ~ 10, and in solution, the concentration of iridium is 1.2 × 10
-5~ 1.2mol/L.
More specifically, in solution, the mol ratio of iridium, 2,7 dihydroxy naphthalene and PEG-400 is 1:0.5 ~ 40:1 ~ 10.
Because the concentration of iridium ion, 2,7 dihydroxy naphthalene and PEG-400 seeing brilliant pattern and size by affecting iridium Jie, therefore configuring suitable reaction soln solubility and can obtain better pattern and size.
Concrete, PH conditioning agent is NaOH or KOH solution.
Concrete, the time that solution is placed under ultraviolet lighting environment is 0.01 ~ 620 hour.
Because impact is situated between and sees brilliant pattern by the ultraviolet lighting time, therefore control reaction soln be placed on ultraviolet irradiation condition under time, Jie that can obtain different-shape sees crystalline substance.
Concrete, it is 20 ~ 7000 that iridium Jie sees brilliant length, and the width that iridium Jie sees crystalline substance is 2 ~ 200nm.
Concrete, iridium is situated between, and sight is brilliant to be made up of iridium nanoparticle, and the particle diameter of iridium nanoparticle is 0.5 ~ 20nm.
In such scheme, brilliant pattern is seen and size has material impact because the concentration in dispersion agent, reductive agent, iridium source and ultraviolet lighting time are situated between to iridium, therefore can prepare that pattern is different, size is different, the iridium of favorable dispersity be situated between see brilliant, and method is simple, environmental protection, without the need to the at substantial energy, can be applicable to suitability for industrialized production.Raw material involved in the present invention and equipment all can buied on the market.Iridium Jie prepared by the present invention sees crystalline substance and is expected to apply to the fields such as precision scientific instrument, nano electron device, photoelectronics, sensor, aerospace, new forms of energy and chemical industry chemistry.
Accompanying drawing explanation
Fig. 1 is the TEM figure that the embodiment of the present invention 1 needle-like iridium Jie sees brilliant different amplification;
Fig. 2 is the TEM figure that the embodiment of the present invention 2 dendroid iridium Jie sees brilliant different amplification;
Fig. 3 is that the embodiment of the present invention 3 corynebacterium iridium Jie sees brilliant TEM figure;
Fig. 4 is that the embodiment of the present invention 3 different size needle-like iridium Jie sees brilliant TEM figure.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described further, but the invention is not restricted to the following stated scope.
Embodiment 1: the needle-like iridium of the present embodiment is situated between and sees the concrete steps of brilliant preparation method:
First, measuring 0.5 ml polyoxyethylene glycol (PEG-400) with 4ml volumetric molar concentration is 1.5 × 10
-2the chloro-iridic acid Homogeneous phase mixing of mol/L.Then, in mixing solutions, the 2,7 dihydroxy naphthalene that 0.6 ml volumetric molar concentration is 1.0 mol/L is added.Finally, pH value is adjusted to 9.0 (alkalescence) by the NaOH solution that takes a morsel.Final mixed solution is transferred on ultraviolet lighting platform, adopt wavelength to be the ultraviolet source irradiation 0.5 hour of 200nm.It is 0.2 ~ 30 μm that needle-like iridium Jie of final synthesis sees brilliant length, and diameter is 10 ~ 200nm, takes out and can obtain needle-like iridium Jie sight crystalline substance, see Fig. 1 from solution.
Embodiment 2:
First, measuring 0.5 ml polyoxyethylene glycol (PEG-400) with 4ml volumetric molar concentration is 1.5 × 10
-2the chloro-iridic acid Homogeneous phase mixing of mol/L.Then, in mixing solutions, the 2,7 dihydroxy naphthalene that 0.6 ml volumetric molar concentration is 1.0 mol/L is added.Finally, pH value is adjusted to 9.0 (alkalescence) by the NaOH solution that takes a morsel.Final mixed solution is transferred on ultraviolet lighting platform, adopt wavelength to be the ultraviolet source irradiation 20 hours of 200nm.It is 0.2 ~ 2 μm that dendroid iridium Jie of final synthesis sees brilliant length, and diameter is 10 ~ 200nm, takes out and can obtain dendroid iridium Jie sight crystalline substance, see Fig. 2 from solution.
Embodiment 3:
First, measuring 0.5 ml polyoxyethylene glycol (PEG-400) with 4ml volumetric molar concentration is 1.5 × 10
-2the chloro-iridic acid Homogeneous phase mixing of mol/L.Then, in mixing solutions, the 2,7 dihydroxy naphthalene that 3 ml volumetric molar concentrations are 1.0 mol/L is added.Finally, pH value is adjusted to 9.0 (alkalescence) by the NaOH solution that takes a morsel.Final mixed solution is transferred on ultraviolet lighting platform, adopt wavelength to be the ultraviolet source irradiation 0.5 hour of 200nm.It is 20 ~ 600nm that corynebacterium iridium Jie of final synthesis sees brilliant length, and diameter is 10 ~ 100nm, takes out and can obtain corynebacterium iridium Jie sight crystalline substance, see Fig. 3 from solution.
Embodiment 4:
First, measuring 0.5 ml polyoxyethylene glycol (PEG-400) with 4ml volumetric molar concentration is 1.5 × 10
-2the chloro-iridic acid Homogeneous phase mixing of mol/L.Then, in mixing solutions, the 2,7 dihydroxy naphthalene that 0.6 ml volumetric molar concentration is 1.0 mol/L is added.Finally, pH value is adjusted to 8.0 (alkalescence) by the NaOH solution that takes a morsel.Final mixed solution is transferred on ultraviolet lighting platform, adopt wavelength to be the ultraviolet source irradiation 0.2 hour of 200nm.It is 150 ~ 600 that needle-like iridium Jie of final synthesis sees brilliant length, and diameter is 10 ~ 100nm, takes out and can obtain needle-like iridium Jie sight crystalline substance, see Fig. 4 from solution.
Claims (6)
1. iridium Jie sees a brilliant synthetic method, comprises the steps:
The aqueous solution of preparation chloro-iridic acid, PEG-400 and 2,7 dihydroxy naphthalene, and by pH adjusting agent, the pH value of described solution is adjusted to alkalescence;
Be positioned in ultraviolet lighting environment by described solution and irradiate, the wavelength of described UV-light is 130 ~ 400nm.
2. iridium Jie as claimed in claim 1 sees brilliant synthetic method, it is characterized in that:
In described solution, the mol ratio of iridium, 2,7 dihydroxy naphthalene and PEG-400 is 1:0.01 ~ 300:1 ~ 10, and in described solution, the concentration of iridium is 1.2 × 10
-5~ 1.2mol/L.
3. iridium Jie as claimed in claim 1 sees brilliant synthetic method, it is characterized in that:
Described PH conditioning agent is NaOH or KOH solution.
4. iridium Jie as claimed in claim 1 sees brilliant synthetic method, it is characterized in that:
The time that described solution is placed under ultraviolet lighting environment is 0.01 ~ 620 hour.
5. the iridium according to any one of claim 1-4 is situated between and sees brilliant synthetic method, it is characterized in that:
Described iridium Jie sight is brilliant extending longitudinally along it, and the length that described iridium Jie sees crystalline substance is 20 ~ 7000nm, and the diameter that described iridium Jie sees crystalline substance is 2 ~ 200nm.
6. the iridium according to any one of claim 1-4 is situated between and sees brilliant synthetic method, it is characterized in that:
Described iridium is situated between, and sight is brilliant to be made up of iridium nanoparticle, and the particle diameter of described iridium nanoparticle is 0.5 ~ 20nm.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786669A (en) * | 2010-03-26 | 2010-07-28 | 北京理工大学 | Alpha-ferric oxide mesoscopic crystal preparation method |
| CN102275977A (en) * | 2011-07-19 | 2011-12-14 | 西安交通大学 | Preparation method of zinc oxide mesoscopic crystal with adjustable aspect ratio |
| CN103056387A (en) * | 2013-01-22 | 2013-04-24 | 昆明理工大学 | Preparation method for iridium nanowires |
| CN103265060A (en) * | 2013-05-23 | 2013-08-28 | 中山大学 | Preparation method of monodisperse hexagonal-phase sodium yttrium fluoride mesoscopic crystal particles |
| CN103466718A (en) * | 2013-09-06 | 2013-12-25 | 浙江大学 | Method for preparing spindle iron oxide mesoscopic crystal |
| CN103482708A (en) * | 2013-09-06 | 2014-01-01 | 浙江大学 | Method of preparing monodisperse iron oxide quasi-cubic mesoscopic crystal with adjustable grain size |
-
2014
- 2014-04-15 CN CN201410148004.4A patent/CN105002552A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786669A (en) * | 2010-03-26 | 2010-07-28 | 北京理工大学 | Alpha-ferric oxide mesoscopic crystal preparation method |
| CN102275977A (en) * | 2011-07-19 | 2011-12-14 | 西安交通大学 | Preparation method of zinc oxide mesoscopic crystal with adjustable aspect ratio |
| CN103056387A (en) * | 2013-01-22 | 2013-04-24 | 昆明理工大学 | Preparation method for iridium nanowires |
| CN103265060A (en) * | 2013-05-23 | 2013-08-28 | 中山大学 | Preparation method of monodisperse hexagonal-phase sodium yttrium fluoride mesoscopic crystal particles |
| CN103466718A (en) * | 2013-09-06 | 2013-12-25 | 浙江大学 | Method for preparing spindle iron oxide mesoscopic crystal |
| CN103482708A (en) * | 2013-09-06 | 2014-01-01 | 浙江大学 | Method of preparing monodisperse iron oxide quasi-cubic mesoscopic crystal with adjustable grain size |
Non-Patent Citations (1)
| Title |
|---|
| 杨伦权: "Ir纳米粒子的形貌控制及其催化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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