CN1443706A - Preparation method of nano tricopper diselenide - Google Patents
Preparation method of nano tricopper diselenide Download PDFInfo
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- CN1443706A CN1443706A CN 03116457 CN03116457A CN1443706A CN 1443706 A CN1443706 A CN 1443706A CN 03116457 CN03116457 CN 03116457 CN 03116457 A CN03116457 A CN 03116457A CN 1443706 A CN1443706 A CN 1443706A
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Abstract
The preparation method of nano tricopper diselenide includes the following steps: preparing coordination compound of cupric ion and triethanolamine-triethanolaminocopper complex cation aqueous solution and aqueous solution of sodium selenosulfate, then mixing said two aqueous solutions in quartz conical flask, introducing nitrogen gas and discharging air completely, using high-voltage mercury vapour lamp to make irradiation, and using cooling water to retain and make the temp. of reaction system be room temp., irradiating for 4-8 hr, then can obtain nano tricopped diselenide with tetragonal structure and average grain size of 40-50 nm.
Description
Technical field:
The present invention relates to a kind of preparation method of nanometer lithium selenide-copper, be specifically related to adopt photochemical method to prepare the nanometer lithium selenide-copper.
Background technology:
Nanometer powder has the physics of many uniquenesses, the great attention that chemical property causes people because of its dimensional effect.The nanometer lithium selenide-copper be because of being widely used in solar cell, field such as superionic conductor(s) and become one of research focus of academia.Preparation method about the nanometer lithium selenide-copper reports more in recent years.These methods mainly concentrate on uses sonochemical method, the microwave-assisted heating method, hydrothermal method and solvent-thermal method prepare the nanometer lithium selenide-copper, in these methods, ultrasonic radiation, microwave radiation and hydrothermal method, the High Temperature High Pressure in the solvent-thermal method provides required negative divalence plasma selenium for generating the nanometer lithium selenide-copper, though above method technology is simple, but ubiquity product and is reunited more serious, apparatus expensive, cost height, shortcoming such as danger is bigger.
Summary of the invention:
The objective of the invention is at the deficiencies in the prior art, provide a kind of simple to operate, the preparation method of the nanometer lithium selenide-copper that cost is low has more practicality.
For realizing such purpose, in the technical scheme of the present invention, the method that adopts the high voltage mercury lamp irradiation trolamine to close the mixed aqueous solution of copper complex cation and sodium thiosulfate makes the nanometer lithium selenide-copper.Preparation bivalent cupric ion and trolamine title complex---trolamine closes the copper complex cation aqueous solution, and behind the aqueous solution of sodium thiosulfate, these two kinds of aqueous solution that obtain are mixed in quartz conical flask, feed and use high voltage mercury lamp irradiation after nitrogen drains air, and to keep reaction system with water coolant be room temperature, can obtain the nanometer lithium selenide-copper after irradiation 4-8 hour.
Preparation method of the present invention comprises following concrete steps:
1. trolamine closes the preparation of the copper complex cation aqueous solution: trolamine is dissolved in the aqueous solution that contains bivalent cupric ion and obtain bivalent cupric ion and trolamine title complex---trolamine closes the copper complex cation aqueous solution.The mol ratio of trolamine and bivalent cupric ion is 1～1.5: 1.
The said aqueous solution that contains bivalent cupric ion of the present invention is generally cupric nitrate, anhydrous cupric sulfate, contains the aqueous solution of copper sulfate, the anhydrous cupric chloride of crystal water, the cupric chloride that contains crystal water, cupric bromide, venus crystals.
2. the preparation of the aqueous solution of sodium thiosulfate: sodium sulfite aqueous solution and selenium powder backflow were made in 3～5 hours.The mol ratio of sodium sulfite aqueous solution and selenium powder is 2～4: 1
3. the nanometer lithium selenide-copper is synthetic: the aqueous solution that prepared trolamine is closed the copper complex cation aqueous solution and sodium thiosulfate is with 1～1.2: 1 mol ratio is mixed in quartz conical flask, feed nitrogen and after draining air, used high voltage mercury lamp irradiation 4-8 hour in 10-30 minute, and to keep reaction system with water coolant be room temperature, reaction finishes the back centrifugation, repeatedly washing, vacuum-drying can obtain the nanometer lithium selenide-copper.
The present invention is owing to adopted the title complex trolamine to close the copper complex cation as reactant, and cupric ion discharges from title complex lentamente and participates in reaction in reaction process, so the nanometer lithium selenide-copper that obtains disperses, has avoided serious reunion.The present invention utilizes SO
3 2-Absorb the characteristic that ultraviolet ray discharges electronics, adopted the high voltage mercury lamp irradiation reaction solution to produce required electronics in the reaction process, and then generate the nanometer lithium selenide-copper, so just avoided using expensive ultrasonic generator, microwave generator and dangerous bigger autoclave.In addition, adopt the simple to operate and easy control of way of high voltage mercury lamp irradiation.
The inventive method is simple to operate, cost is low, and the nanometer lithium selenide-copper product of preparation is a tetragonal, and median size is 40-50nm.
Description of drawings:
Fig. 1 is the x-ray diffraction pattern of the embodiment of the invention 1 resulting nanometer lithium selenide-copper.
Fig. 2 is the transmission electron microscope photo of the embodiment of the invention 1 resulting nanometer lithium selenide-copper.
Embodiment:
Below by specific embodiment technical scheme of the present invention is further described.The following examples do not limit the scope of the invention.
Embodiment 1:
1. in the quartz conical flask of a 50mL, the 0.2g cupric nitrate is dissolved in the 26mL deionized water, by 1: 1 mol ratio add trolamine obtain bivalent cupric ion and trolamine title complex---trolamine closes the copper complex cation aqueous solution.
2. the sodium sulphite anhydrous 99.3 with 0.06mol is dissolved in the deionized water of 100mL, adds the selenium powder of 0.02mol again, refluxes to make the sodium thiosulfate aqueous solution of 0.2M in 5 hours.
3. measure the 4mL step 2. in the sodium thiosulfate aqueous solution of preparation join the 1. prepared trolamine of step and close the copper complex cation aqueous solution, fed nitrogen 15 minutes, the high voltage mercury lamp 20cm that then Erlenmeyer flask is placed 250W is irradiation 4 hours at a distance, keeps reaction system to be in room temperature state with water coolant.After the products therefrom centrifugation, use deionized water wash 3 times, drying at room temperature is 24 hours in the vacuum, obtains the nanometer lithium selenide-copper.
X-ray diffraction spectrogram such as Fig. 1 of resultant nanometer lithium selenide-copper, prepared as seen from Figure 1 nanometer lithium selenide-copper is a tetragonal structure, transmission electron microscope photo such as Fig. 2, prepared as seen from Figure 2 nanometer lithium selenide-copper grain size is 40-50nm.
Embodiment 2:
1. in the quartz conical flask of a 50mL, the 0.2g anhydrous cupric sulfate is dissolved in the 26mL deionized water, by 1: 1.2 mol ratio add trolamine obtain bivalent cupric ion and trolamine title complex---trolamine closes the copper complex cation aqueous solution.
2. the sodium sulphite anhydrous 99.3 with 0.05mol is dissolved in the deionized water of 100mL, adds the selenium powder of 0.02mol again, refluxes to make the sodium thiosulfate aqueous solution of 0.2M in 5 hours.
3. measure the 3mL step 2. in the sodium thiosulfate aqueous solution of preparation join the 1. prepared trolamine of step and close the copper complex cation aqueous solution, fed nitrogen 20 minutes, the high voltage mercury lamp 20cm that then Erlenmeyer flask is placed 250W is irradiation 4 hours at a distance, keeps reaction system to be in room temperature state with water coolant.After the products therefrom centrifugation, use deionized water wash 3 times, drying at room temperature is 30 hours in the vacuum, obtains the nanometer lithium selenide-copper.
Embodiment 3:
1. in the quartz conical flask of a 50mL, the 0.2g cupric chloride is dissolved in the 26mL deionized water, by 1: 1.5 mol ratio add trolamine obtain bivalent cupric ion and trolamine title complex---trolamine closes the copper complex cation aqueous solution.
2. the sodium sulphite anhydrous 99.3 with 0.06mol is dissolved in the deionized water of 100mL, adds the selenium powder of 0.02mol again, refluxes to make the sodium thiosulfate aqueous solution of 0.2M in 4 hours.
3. measure the 4mL step 2. in the sodium thiosulfate aqueous solution of preparation join the 1. prepared trolamine of step and close the copper complex cation aqueous solution, fed nitrogen 30 minutes, the high voltage mercury lamp 20cm that then Erlenmeyer flask is placed 250W is irradiation 8 hours at a distance, keeps reaction system to be in room temperature state with water coolant.After the products therefrom centrifugation, use deionized water wash 3 times, drying at room temperature is 24 hours in the vacuum, obtains the nanometer lithium selenide-copper.
Claims (2)
1, a kind of preparation method of nanometer lithium selenide-copper is characterized in that comprising the steps:
1) trolamine closes the preparation of the copper complex cation aqueous solution: trolamine is dissolved in the aqueous solution that contains bivalent cupric ion and obtain bivalent cupric ion and trolamine title complex---trolamine closes the copper complex cation aqueous solution, the mol ratio of trolamine and bivalent cupric ion is 1～1.5: 1;
2) preparation of the aqueous solution of sodium thiosulfate: sodium sulfite aqueous solution and selenium powder backflow were made in 3～5 hours, and the mol ratio of sodium sulfite aqueous solution and selenium powder is 2～4: 1;
3) the nanometer lithium selenide-copper is synthetic: the aqueous solution that prepared trolamine is closed the copper complex cation aqueous solution and sodium thiosulfate is with 1～1.2: 1 mol ratio is mixed in quartz conical flask, feed nitrogen and after draining air, used high voltage mercury lamp irradiation 4-8 hour in 10-30 minute, and to keep reaction system with water coolant be room temperature, reaction finishes the back centrifugation, and washing, dry back obtain the nanometer lithium selenide-copper.
2, the preparation method of nanometer lithium selenide-copper as claimed in claim 1 is characterized in that the said aqueous solution that contains bivalent cupric ion is cupric nitrate, anhydrous cupric sulfate, contains the aqueous solution of copper sulfate, the anhydrous cupric chloride of crystal water, the cupric chloride that contains crystal water, cupric bromide, venus crystals.
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| CNB031164579A CN1194886C (en) | 2003-04-17 | 2003-04-17 | Preparation method of nano tricopper diselenide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100548311C (en) * | 2007-06-13 | 2009-10-14 | 中国科学技术大学 | Application and the fast preparation method of sodium thiosulfate in preparation clinical selenium-complementing and treatment cancer drug |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101871117B (en) * | 2010-06-30 | 2011-11-23 | 湖南大学 | CuxSe/TiO2 nanotube array of p-type semiconductor nano material and preparation method thereof |
| CN102936004B (en) * | 2012-10-25 | 2014-05-28 | 江苏大学 | Preparation method for preparing cobalt diselenide-ethylenediamine micron-grade flowers through hydrothermal method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100548311C (en) * | 2007-06-13 | 2009-10-14 | 中国科学技术大学 | Application and the fast preparation method of sodium thiosulfate in preparation clinical selenium-complementing and treatment cancer drug |
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