CN1546382A - Method for synthesizing cadmium hydroxide single-crystal nanowire - Google Patents
Method for synthesizing cadmium hydroxide single-crystal nanowire Download PDFInfo
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- CN1546382A CN1546382A CNA2003101144187A CN200310114418A CN1546382A CN 1546382 A CN1546382 A CN 1546382A CN A2003101144187 A CNA2003101144187 A CN A2003101144187A CN 200310114418 A CN200310114418 A CN 200310114418A CN 1546382 A CN1546382 A CN 1546382A
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Abstract
The invention provides a process for preparing cadmium hydroxide single-crystal nanowires comprising the steps of, (1) dissolving soluble cadmium salt in deionized water, slowly charging alkali or ammonia solution till the pH is 10-14, stiring to produce white Cd(OH)2 deposition, (2) centrifugally scouring the white Al(OH)2 till pH is neutral, (3) redepersing the scoured white Cd(OH)2 deposition into deionized water, charging right amount of inorganic salt, (4) hot reaction 10-15 hours in air-tight container at 200-250 deg. C, thus obtaining cadmium hydroxide single crystal nanowires.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, relate to the production method of nano material, relate in particular to a kind of synthetic method of cadmium hydroxide monocrystal nanowire.
Background technology
Since carbon nanotube is found, one-dimensional nano structure material receives much attention because of its peculiar electricity, optics, magnetic and mechanical property and the potential application in nano-device structure thereof, thereby to explore preparation low-dimension nano material structurally ordered, excellent property be the focus of research always.Relevant technologies personnel are doing a lot of trials aspect the preparation of one dimension Nano structure, wherein template or tensio-active agent have obtained using widely.Yet, in reaction system, to introduce template or tensio-active agent and be unable to do without their preparation and selection, this makes that not only entire reaction course is complicated, in addition, is unfavorable for forming large-scale industrial production, and might reduces the purity of the finished product.Mainly concentrate on the preparation research of oxide compound [ZhengWei Pan, Zu Rong Dai, Zhang Lin Wang etc., science, 291,1947] and sulfide [Jian Yang etc., Angew.Chem.Int.Ed.2002,41,4697] for the compound of cadmium.At present as yet not relevant for cadmium hydroxide nano wire preparation method's report.
Summary of the invention
The purpose of this invention is to provide a kind of tensio-active agent or template do not used, simple for process, cost is low, helps forming the synthetic method of the cadmium hydroxide monocrystal nanowire of large-scale industrial production.
Purpose of the present invention can realize by following technical measures:
The synthetic method of this cadmium hydroxide monocrystal nanowire adopts following steps to carry out:
A, elder generation are dissolved in the solubility cadmium salt in the deionized water, and slowly adding alkali or ammonia soln to pH value again is 10～14, stir to generate white Cd (OH) down
2Precipitation; Then
B, with white Cd (OH)
2Precipitation centrifuge washing to pH value is neutral; Then
C, the white Cd (OH) after will washing
2Precipitation is dispersed in the deionized water again, adds an amount of inorganic salt; Then
D, put into encloses container in 200～250 ℃ of following hydro-thermal reactions 10～15 hours, the cadmium hydroxide monocrystal nanowire.
Purpose of the present invention also can realize by following technical measures:
Preferred Cadmium chloride fine powder of described solubility cadmium salt and cadmium nitrate; Preferred potassium hydroxide of described alkali and sodium hydroxide; Described inorganic salt can be selected any or several mixtures in Repone K, sodium-chlor, saltpetre, vitriolate of tartar, SODIUMNITRATE, the sodium sulfate for use as mineralizer.
The present invention is a raw material with the solubility cadmium salt, adopts the way that slowly adds potassium hydroxide, sodium hydroxide or ammonia soln, controls certain pH value, generates white Cd (OH) under agitation condition
2Precipitation is again with the white Cd (OH) of gained
2Precipitate with deionized water repeatedly wash to the pH value be about 7, then with inorganic salt as mineralizer, in closed reactor, under 200～250 ℃ of conditions, carry out hydro-thermal reaction, can obtain the cadmium hydroxide monocrystal nanowire.Nanowire diameter is 40～200 nanometers, reaches hundreds of microns.The nano wire of preparation can be used for preparing nano-oxide or sulfide as precursor through dehydration or sulfuration, through after the finishing, will play an important role in bioanalysis.This method is not used any organic reagent of tensio-active agent or template or other, technology is simple, working condition is controlled, raw material is cheap and easy to get, and is with low cost, can realize large-scale industrial production, synthetic cadmium hydroxide nano wire is a single crystal structure, because nano wire has specific physiques such as anisotropy, therefore, be expected to obtain to use widely simultaneously in fields such as magnetic, electricity, optics.
Embodiment:
Embodiment 1:
Take by weighing 0.001mol analytical pure Cadmium chloride fine powder and place beaker,, adjust the pH value to 14 of solution again with 5% potassium hydroxide solution, obtain white Cd (OH) with the 20ml deionized water dissolving
2Precipitation continues to stir 10 minutes.With the above-mentioned white Cd (OH) that obtains
2Precipitation centrifuge washing to pH value is 7, then with white Cd (OH)
2Precipitation is scattered in the 18ml water again, adds 0.3 gram Repone K as mineralizer.Above-mentioned solution is moved in the withstand voltage reactor of 20ml stainless steel, and reaction is 12 hours under 250 ℃ of conditions, is cooled to room temperature then, and product is with the B suction filtration, dry under 60 ℃ of conditions with deionized water wash, obtains white Cd (OH)
2Powder.Product is accredited as six side's phase cadmium hydroxides through X-ray powder diffraction; TEM Electronic Speculum testing product pattern: diameter is 40～200 nanometers, and length reaches hundreds of microns; Single nano-wire electron diffraction proof product is a monocrystalline.
Embodiment 2:
Take by weighing 0.001mol analytical pure Cadmium chloride fine powder and place beaker,, adjust the pH value to 14 of solution again with 5% potassium hydroxide solution, obtain white Cd (OH) with the 20ml deionized water dissolving
2Precipitation continues to stir 10 minutes.With the above-mentioned white Cd (OH) that obtains
2Precipitation centrifuge washing to pH value is 7, then with white Cd (OH)
2Precipitation is scattered in the 18ml water again, adds 0.3 gram SODIUMNITRATE as mineralizer.Above-mentioned solution is moved in the withstand voltage reactor of 20ml stainless steel, and reaction is 12 hours under 250 ℃ of conditions, is cooled to room temperature then, and product is with the B suction filtration, dry under 60 ℃ of conditions with deionized water wash, obtains white Cd (OH)
2Powder.Product detects through X-ray powder diffraction, TEM Electronic Speculum.
Embodiment 3:
Take by weighing 0.001mol analytical pure cadmium nitrate and place beaker,, adjust the pH value to 14 of solution again with 5% potassium hydroxide solution, obtain white Cd (OH) with the 20ml deionized water dissolving
2Precipitation continues to stir 10 minutes.With the above-mentioned white Cd (OH) that obtains
2Precipitation centrifuge washing to pH value is 7, then with white Cd (OH)
2Precipitation is scattered in the 18ml water again, adds 0.3 gram sodium sulfate as mineralizer.Above-mentioned solution is moved in the withstand voltage reactor of 20ml stainless steel, and reaction is 12 hours under 250 ℃ of conditions, is cooled to room temperature then, and product is with the B suction filtration, dry under 60 ℃ of conditions with deionized water wash, obtains white Cd (OH)
2Powder.Product detects through X-ray powder diffraction, TEM Electronic Speculum.
Embodiment 4:
Take by weighing 0.001mol analytical pure cadmium nitrate and place beaker,, adjust the pH value to 10 of solution again with the ammonia soln of 5M, obtain white Cd (OH) with the 20ml deionized water dissolving
2Precipitation continues to stir 10 minutes.With the above-mentioned white Cd (OH) that obtains
2Precipitation centrifuge washing to pH value is 7, then with white Cd (OH)
2Precipitation is scattered in the 18ml water again, adds 0.3 gram Repone K as mineralizer.Above-mentioned solution is moved in the withstand voltage reactor of 20ml stainless steel, and reaction is 12 hours under 250 ℃ of conditions, is cooled to room temperature then, and product is with the B suction filtration, dry under 60 ℃ of conditions with deionized water wash, obtains white Cd (OH)
2Powder.Product detects through X-ray powder diffraction, TEM Electronic Speculum.
Description of drawings:
Fig. 1 is the cadmium hydroxide nano wire X-ray powder diffraction figure of the embodiment of the invention 1 preparation;
Fig. 2 is cadmium hydroxide nano wire transmission electron microscope (TEM) photo of the embodiment of the invention 1 preparation;
Fig. 3 is cadmium hydroxide nano wire scanning electron microscope (SEM) photo of the embodiment of the invention 1 preparation;
Fig. 4 is the cadmium hydroxide nano wire electron diffraction pattern of the embodiment of the invention 1 preparation;
Fig. 5 is the high explanation of the cadmium hydroxide nano wire photo of the embodiment of the invention 1 preparation;
Fig. 6 is cadmium hydroxide nano wire transmission electron microscope (TEM) photo of the embodiment of the invention 2 preparations;
Fig. 7 is cadmium hydroxide nano wire transmission electron microscope (TEM) photo of the embodiment of the invention 3 preparations;
Fig. 8 is cadmium hydroxide nano wire transmission electron microscope (TEM) photo of the embodiment of the invention 4 preparations.
Claims (4)
1, the synthetic method of cadmium hydroxide monocrystal nanowire is characterized in that this method carries out as follows:
A, elder generation are dissolved in the solubility cadmium salt in the deionized water, and slowly adding alkali or ammonia soln to pH value again is 10～14, stir to generate white Cd (OH) down
2Precipitation; Then
B, with white Cd (OH)
2Precipitation centrifuge washing to pH value is neutral; Then
C, the white Cd (OH) after will washing
2Precipitation is dispersed in the deionized water again, adds an amount of inorganic salt, then
D, put into encloses container in 200～250 ℃ of following hydro-thermal reactions 10～15 hours, the cadmium hydroxide monocrystal nanowire.
2,, it is characterized in that preferred Cadmium chloride fine powder of described solubility cadmium salt and cadmium nitrate according to the synthetic method of the described cadmium hydroxide monocrystal nanowire of claim 1.
3,, it is characterized in that preferred potassium hydroxide of described alkali and sodium hydroxide according to the synthetic method of the described cadmium hydroxide monocrystal nanowire of claim 1.
4,, it is characterized in that described inorganic salt can select any or several mixtures in Repone K, sodium-chlor, saltpetre, vitriolate of tartar, SODIUMNITRATE, the sodium sulfate for use as mineralizer according to the synthetic method of the described cadmium hydroxide monocrystal nanowire of claim 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2003101144187A CN1297483C (en) | 2003-12-10 | 2003-12-10 | Method for synthesizing cadmium hydroxide single-crystal nanowire |
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| CNB2003101144187A CN1297483C (en) | 2003-12-10 | 2003-12-10 | Method for synthesizing cadmium hydroxide single-crystal nanowire |
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| CN1546382A true CN1546382A (en) | 2004-11-17 |
| CN1297483C CN1297483C (en) | 2007-01-31 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891240A (en) * | 2010-07-14 | 2010-11-24 | 南京大学 | Preparation method of CdO porous nanometer material |
| CN102181283A (en) * | 2011-04-14 | 2011-09-14 | 中国科学院化学研究所 | CdS/Cd(OH)2 composite nano wire and preparation method thereof |
| CN102432061A (en) * | 2011-09-29 | 2012-05-02 | 新疆大学 | Method for preparing Cd(OH)2 and CdO hexagonal nanoplates in simple solvent system |
| CN102502786A (en) * | 2011-10-20 | 2012-06-20 | 哈尔滨工程大学 | Method for preparing cadmium hydroxide nanowires |
| CN102557105A (en) * | 2011-12-31 | 2012-07-11 | 中国科学院过程工程研究所 | Monodisperse cerium oxide nanoparticle and preparation method thereof |
| CN103482684A (en) * | 2013-09-23 | 2014-01-01 | 哈尔滨工程大学 | Preparation method for cadmium hydroxide nano-array capable of adsorbing and extracting DNA |
| CN106853984A (en) * | 2017-02-27 | 2017-06-16 | 曲阜师范大学 | A kind of preparation method of the nano oxygen cadmium of special appearance |
| WO2021109853A1 (en) * | 2019-12-03 | 2021-06-10 | 中国科学院深圳先进技术研究院 | Cadmium hydride porous material, preparation method for same, and negative electrode and battery comprising same |
| CN114702059A (en) * | 2021-12-30 | 2022-07-05 | 南京大学 | Binary hydroxide nanotube with composite structure and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB720842A (en) * | 1952-03-29 | 1954-12-29 | Gen Electric | Improvements relating to the preparation of cadmium selenide |
| SU1567263A1 (en) * | 1988-10-10 | 1990-05-30 | Институт общей и неорганической химии АН БССР | Method of producing sorbent based on cadmium hydroxide |
-
2003
- 2003-12-10 CN CNB2003101144187A patent/CN1297483C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891240A (en) * | 2010-07-14 | 2010-11-24 | 南京大学 | Preparation method of CdO porous nanometer material |
| CN101891240B (en) * | 2010-07-14 | 2012-02-29 | 南京大学 | Preparation method of CdO porous nanometer material |
| CN102181283A (en) * | 2011-04-14 | 2011-09-14 | 中国科学院化学研究所 | CdS/Cd(OH)2 composite nano wire and preparation method thereof |
| CN102181283B (en) * | 2011-04-14 | 2013-09-18 | 中国科学院化学研究所 | CdS/Cd(OH)2 composite nano wire and preparation method thereof |
| CN102432061A (en) * | 2011-09-29 | 2012-05-02 | 新疆大学 | Method for preparing Cd(OH)2 and CdO hexagonal nanoplates in simple solvent system |
| CN102502786B (en) * | 2011-10-20 | 2013-07-31 | 哈尔滨工程大学 | Method for preparing cadmium hydroxide nanowires |
| CN102502786A (en) * | 2011-10-20 | 2012-06-20 | 哈尔滨工程大学 | Method for preparing cadmium hydroxide nanowires |
| CN102557105A (en) * | 2011-12-31 | 2012-07-11 | 中国科学院过程工程研究所 | Monodisperse cerium oxide nanoparticle and preparation method thereof |
| CN102557105B (en) * | 2011-12-31 | 2014-06-04 | 中国科学院过程工程研究所 | Monodisperse cerium oxide nanoparticle and preparation method thereof |
| CN103482684A (en) * | 2013-09-23 | 2014-01-01 | 哈尔滨工程大学 | Preparation method for cadmium hydroxide nano-array capable of adsorbing and extracting DNA |
| CN106853984A (en) * | 2017-02-27 | 2017-06-16 | 曲阜师范大学 | A kind of preparation method of the nano oxygen cadmium of special appearance |
| CN106853984B (en) * | 2017-02-27 | 2018-09-18 | 曲阜师范大学 | A kind of preparation method of the nano oxygen cadmium of special appearance |
| WO2021109853A1 (en) * | 2019-12-03 | 2021-06-10 | 中国科学院深圳先进技术研究院 | Cadmium hydride porous material, preparation method for same, and negative electrode and battery comprising same |
| CN114702059A (en) * | 2021-12-30 | 2022-07-05 | 南京大学 | Binary hydroxide nanotube with composite structure and preparation method thereof |
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|---|---|
| CN1297483C (en) | 2007-01-31 |
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