CN101045551A - Chemical method for preparing nano metal iodine compound film - Google Patents
Chemical method for preparing nano metal iodine compound film Download PDFInfo
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- CN101045551A CN101045551A CN 200610146056 CN200610146056A CN101045551A CN 101045551 A CN101045551 A CN 101045551A CN 200610146056 CN200610146056 CN 200610146056 CN 200610146056 A CN200610146056 A CN 200610146056A CN 101045551 A CN101045551 A CN 101045551A
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Abstract
A chemical process for preparing the nano-class metallic iodide film features that its substrate may be a metallic one made of Pb, Cu, Ag, or Cd, or a semiconductor material with a plated metallic film, layer, or a glass plate with a plated Ag layer, and the reactant iodine may be the organic solution of ethanol, propanol, n-hexane, propanetriol, etc, or the monomer iodine. The iodine and organic solvent take part in reaction in teflon reactor at 60-160 deg.C for 6-24 hr.
Description
Technical field:
The invention belongs to material chemistry technical field, relate in particular to a kind of chemical process for preparing nano metal iodine compound film.
Background technology:
Although preparation, purification and the application prospect about metal iodide (lead iodide, iodate chromium, cuprous iodide, Silver iodide etc.) has a large amount of bibliographical informations in the world at present, but the preparation method of new efficient quick is actually rare, and the report of domestic this respect still less.Usually, the crystal of metal iodide can still because reaction has related to other metal ion or tensio-active agent, will take impurity such as sodium, oxygen, sulphur in the final product to inevitably simply by the wet chemistry reaction acquisition of salt compounded of iodine and metal-salt.In recent years, some special preparation method such as gel methods, vapour deposition process, preparation PbI such as spraying pyrolytic decomposition
2The crystalline technology also develops rapidly.But the common technological process of these methods is comparatively complicated, needs extra preparation process in early stage sometimes, and introduces new impurity easily in purification process; Preparation work many times need be carried out in a vacuum, and the iodide crystal melts in a vacuum and the decomposing phenomenon when distilling is difficult to avoid.Especially it should be noted that the danger that when adopting airtight ampoule, has blast as reaction vessel.Therefore, seek efficient quick more and practical preparation metal iodide crystalline method not only also has very high industrial application value in the scientific research field while of crucial importance.
Summary of the invention:
Problem to be solved by this invention is: the method for preparing metal iodine compound film at present exists that product is impure, complex process, conditional request is harsh and easily cause product to decompose, exist the problems such as potential safety hazard of blasting.
The technical scheme that the present invention takes the technical problem that will solve is to realize like this;
This technology by a step chemical reaction directly in the metal base materials such as semi-conductor, glass of metallic film (or the plated) in-situ preparing of coming up iodine compound film, the product impure phenomenon of having avoided the wet chemistry prepared in reaction to be caused; Thereby this technology places reactant the airtight polytetrafluoroethylcontainer container that has stainless steel outer sleeve react to have overcome method complex process such as gel method, vapor deposition method, spraying pyrolytic decomposition under lower temperature shortcoming has also been eliminated the hidden peril of explosion because of using ampoule to exist simultaneously; This technology does not require vacuum environment, so avoided iodide to decompose because of easily distilling in a vacuum.
Embodiment:
(1) preparation work: with the top grade pure metal sheet of buying (or materials such as semi-conductor, glass), be cut into the rectangle of (or cutting into) 0.5 * 2.5cm, put into the beaker that fills deionized water, stand-by with being soaked in the dehydrated alcohol behind the ultrasonic cleaner washing 0.5h.
Can directly do substrate for tinsel uses.
Semiconductor material then can plate layer of metal film earlier by methods such as plating, ion sputtering, vapour deposition, silver mirror reaction, remakes metal base and uses.
Other material silver metal film for example on glass then can pass through silver mirror reaction, makes to plate on the sheet glass to remake behind the argent directly to do substrate and use.Polytetrafluoroethylcontainer container is used tap water, distilled water, absolute ethanol washing successively, and dry back is stand-by.
Iodine is mixed with certain density solution with dehydrated alcohol (or other organic solvents).
(2) reactions steps: get and put into container after the tinsel that a slice the handled material such as semi-conductor, glass of metallic film (or plated) dries up with the cold wind of hair dryer, add 15mL iodine solution (or the iodine of weighing certain mass, then at the organic molten meter that adds 15mL), cover the polytetrafluoroethylcontainer container lid, polytetrafluoroethylcontainer container is put into stainless steel outer sleeve, put into loft drier after tightening the stainless steel outer sleeve loam cake, (60-160, temperature rise rate are 1-2 ℃/min) following reaction some time (6-24h) in certain temperature.
(3) aftertreatment: after reaction finishes, close containers such as loft drier power supply be cooled to room temperature after (or take out from loft drier reaction vessel put into the indoor room temperature that naturally cools to), turn on the loam cake of stainless steel outer sleeve, gently eject polytetrafluoroethylcontainer container from its bottom with have gentle hands, carefully open loam cake, discard liquids with decantation, with after the yellow solid in the absolute ethanol washing container three times with the uncovered loft drier of putting into of polytetrafluoroethylcontainer container in 50 ℃ of dry 4-5h, carefully change over to then in the sample bottle, in lucifuge, exsiccant environment, preserve.
Beneficial effect: the present invention directly adopts iodine and metal reaction original position to prepare iodine compound film, does not have Use any additive and surfactant, belong to single step reaction, need not purify the crystal formation perfection. If promote Then because reduced the purifying technique only this item that can greatly reduce cost considerable economy effect is just arranged to industrial production Benefit.
Claims (8)
1. chemical process for preparing nano metal iodine compound film, it is characterized in that by metal base (0.1 * 50 * 250mm) and the organic solution (15mL) of iodine under 60-160 ℃ of temperature, direct reaction 6-24h in the tetrafluoroethylene reactor is at metallic surface in-situ preparing metal iodide material.
2. according to the described a kind of chemical process for preparing nano metal iodine compound film of claim 1., it is characterized in that: described metal base refers to tinsels such as lead, copper, silver, cadmium, or metal such as one deck lead that plates on semi-conductor, glass material, copper, silver, cadmium.
3. according to the described a kind of chemical process for preparing nano metal iodine compound film of claim 2., it is characterized in that: one deck lead, copper, silver, the cadmium metal that plates on materials such as semi-conductor, glass is meant that semiconductor material adopts methods such as plating, ion sputtering, vapour deposition, silver mirror reaction to plate layer of metal film earlier, and glass material plates the layer of metal silverskin by silver mirror reaction.
4. according to the described a kind of chemical process for preparing nano metal iodine compound film of claim 1., it is characterized in that: the organic solution of iodine matter iodine comprises organic solutions such as the ethanol of iodine, acetone, normal hexane, interior triol, quadrol, diethylamine, propyl alcohol.
5. according to the described a kind of chemical process for preparing nano metal iodine compound film of claim 1., it is characterized in that: temperature rise rate is 1-2 ℃/min.
6. according to the described a kind of chemical process for preparing nano metal iodine compound film of claim 1., it is characterized in that: metal and iodine solution react under 60-160 ℃ of temperature, its temperature operation can be earlier reactor to be put into loft drier, open the loft drier power supply again, temperature progressively rises to appointment numerical value from room temperature; Put into reactor after also can earlier loft drier being warming up to appointment numerical value.
7. according to the described a kind of chemical process for preparing nano metal iodine compound film of claim 1., it is characterized in that: reaction finishes, can slowly be cooled to room temperature by reactor in loft drier by powered-down, also can be reactor to be taken out be put in that spontaneous combustion is cooled to room temperature in the air from loft drier.
8. according to the described a kind of chemical process for preparing nano metal iodine compound film of claim 1., it is characterized in that: product colour is faint yellow, yellow, orange-yellow, golden yellow.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610146056 CN101045551A (en) | 2006-11-07 | 2006-11-07 | Chemical method for preparing nano metal iodine compound film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610146056 CN101045551A (en) | 2006-11-07 | 2006-11-07 | Chemical method for preparing nano metal iodine compound film |
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| CN101045551A true CN101045551A (en) | 2007-10-03 |
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| CN 200610146056 Pending CN101045551A (en) | 2006-11-07 | 2006-11-07 | Chemical method for preparing nano metal iodine compound film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645456A (en) * | 2016-03-30 | 2016-06-08 | 淮北师范大学 | Preparation method of CuI nano-powder |
| CN111362808A (en) * | 2018-12-26 | 2020-07-03 | 东泰高科装备科技有限公司 | Preparation method of perovskite thin film and solar cell |
| CN115806307A (en) * | 2022-12-06 | 2023-03-17 | 淮阴工学院 | Preparation method of sphere-like silver bromide nanoparticles with regular shape |
-
2006
- 2006-11-07 CN CN 200610146056 patent/CN101045551A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645456A (en) * | 2016-03-30 | 2016-06-08 | 淮北师范大学 | Preparation method of CuI nano-powder |
| CN111362808A (en) * | 2018-12-26 | 2020-07-03 | 东泰高科装备科技有限公司 | Preparation method of perovskite thin film and solar cell |
| CN115806307A (en) * | 2022-12-06 | 2023-03-17 | 淮阴工学院 | Preparation method of sphere-like silver bromide nanoparticles with regular shape |
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