CN102211183A - Bismuth (Bi) nanostructured material as well as preparation method and application thereof - Google Patents
Bismuth (Bi) nanostructured material as well as preparation method and application thereof Download PDFInfo
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- CN102211183A CN102211183A CN2010101418539A CN201010141853A CN102211183A CN 102211183 A CN102211183 A CN 102211183A CN 2010101418539 A CN2010101418539 A CN 2010101418539A CN 201010141853 A CN201010141853 A CN 201010141853A CN 102211183 A CN102211183 A CN 102211183A
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Abstract
The invention discloses a Bismuth Bi nanostructured material as well as a preparation method and application thereof. The Bi nanostructured material is a hexagonal crystalline phase Bi elemental nanoparticle in a globular shape; the grain size of the particle is 50-100nm. The preparation method of the Bi nanostructured material comprises the following steps: dissolving a surface active agent, a hydrazine hydrate and a bismuth salt in water to obtain a turbid liquid; enabling the turbid liquid to react for 2-10 hours at 120-180 DEG C, and performing centrifugation to obtain the Bi nanostructured material. The Bi nanostructured material can be used for preparing a Bi modified electrode, wherein the obtained Bi modified electrode can be used for detecting heavy metal ions in a water solution; and the detection limit can be 1x10<-4>g/L.
Description
Technical field
The present invention relates to Bi nano structural material and preparation method thereof and application.
Background technology
Heavy metal element as Cr, Cd, Pb and Hg, has become in the current society to one of the most serious adverse factor of human health threat.Set up fast, reliably, method accurately, the heavy metal ion in all kinds of media is detected, no matter be at aspects such as environmental protection or consumer goods security monitorings, all seem particularly important.Heavy metal element detection method commonly used has comprised sulphur hydrazone development process and atomic absorption spectrography (AAS), the sample-pretreating method complexity that these two kinds of methods relate to, the testing process cost is higher, instrument also there is certain requirement, its extensive use particularly detects application at the scene of special requirement and has been subjected to certain limitation.The stripping volt-ampere analysis is subjected to paying close attention to widely in recent years as a kind of desirable electrochemical analysis method, is widely used in inorganic matter trace detection, organic matter even DNA and detects.The key problem in technology of this method is the selection of working electrode.It is working electrode that conventional process is often selected the Hg material, yet, consider the environment friendly problem, this type of material may produce Hg or Hg in analytic process
2+Refuse causes serious harm to analysis operation person and even environment.Some novel electrodes are seen in bibliographical information in succession in recent years, and regrettably, the preparation process complexity of these novel electrodes detects the reappearance instability, thereby can't really be used.
With metal Bi simple substance membrane modified glassy carbon electrode, and, can detect heavy metal ion used as the working electrode of stripping volt-ampere analysis.This type of electrode all shows higher sensitivity in the work potential scope of broad, and can not be subjected to the influence of dissolved oxygen, has high application prospect in the trace detection of heavy metal ion.The method for preparing the Bi modified electrode has a lot, all needs to experience a process of carrying out pre-treatment with the electrolyte that contains Bi usually.And adopt the Bi nano particle that it is modified this pre-treatment process of can omitting, and can obtain bigger electrode activity surface again, therefore be subjected to more concern.Regrettably, this type of research, and is carried out as technical support widely in default of high-quality Bi nano structural material.The new method fast and effectively that is used for synthetic Bi nanostructured still remains systematic Study.
Summary of the invention
The purpose of this invention is to provide a kind of high-quality Bi nano structural material and preparation method thereof and application.
Bi nano structural material provided by the present invention is a hexagonal crystal phase Bi simple substance nano particle, has spherical pattern.
Bi nano structural material of the present invention, wherein, described nano particle diameter is 50～100nm.
Bi nano structural material preparation method provided by the present invention comprises the steps:
With the water-soluble suspension that is prepared into of surfactant, hydrazine hydrate and bismuth salt;
Described suspension was reacted 2～10 hours under 120～180 ℃ of conditions, centrifugally obtain described spherical pattern Bi simple substance nano structural material.
Bi nano structural material preparation method of the present invention, wherein, described Bi simple substance nano structural material is through washing and dry the processing.
Bi nano structural material preparation method of the present invention, wherein, the mass ratio of described surfactant, described hydrazine hydrate and described bismuth salt is 50: (0.2～0.4): (1～2.5): (0.3～0.4).
Bi nano structural material preparation method of the present invention wherein, reacts described suspension 4～8 hours under 140～160 ℃ of conditions.
Bi nano structural material preparation method of the present invention, wherein, the cleaning solution of described carrying out washing treatment is an ethanol.
Bi nano structural material preparation method of the present invention, wherein, described surfactant is a kayexalate.
Bi nano structural material of the present invention is a hexagonal crystal phase Bi simple substance nano particle, has spherical pattern, nano particle diameter is 50～100nm, such Bi nano structural material quality height, be used for preparing the Bi modified electrode, the Bi modified electrode that is obtained can detect the heavy metal ion in the aqueous solution, and detection limit can reach 1 * 10
-4G/L.
Description of drawings
Fig. 1 is the SEM photo of the synthetic Bi nano structural material of embodiment 1.
Fig. 2 is the SEM photo of the synthetic Bi nano structural material of embodiment 2.
Fig. 3 is the SEM photo of the synthetic Bi nano structural material of embodiment 3.
The specific embodiment
Embodiment 1, preparation Bi simple substance nano structural material
0.21g the surfactant kayexalate is dissolved in the 50g water, stirs 0.8 hour on magnetic stirring apparatus, after the dissolving, adds the 2g hydrazine hydrate fully, stirs 0.5 hour, the 0.3g bismuth nitrate is disperseed wherein again, stirs 0.8 hour.Change gained white suspension over to teflon lined stainless steel hydrothermal reaction kettle that capacity is 80mL, after the sealing, put into baking oven, 140 ℃ of heating 8 hours.After reaction finished, hydrothermal reaction kettle left standstill cooling under room temperature environment.Products therefrom changes centrifuge tube over to, is under 2000 rev/mins of conditions centrifugal 10 minutes at rotating speed; Discarding precipitation, change the upper strata suspension over to centrifuge tube, is under 9000 rev/mins of conditions centrifugal 15 minutes at rotating speed, discards supernatant liquid.With excess ethyl alcohol ultrasonic cleaning 8 minutes, is 9000 rev/min conditions under centrifugal 10 minute at rotating speed with centrifugal products therefrom, discards supernatant liquid, repeated washing 1 time.Change the black solid product after the washing over to surface plate, drying is 1 day under the normal temperature ventilation condition, obtains the Bi nano structural material.
The Bi nano structural material is through XRD, laser particle analyzer, SEM, and TEM and EDX characterize.
(show shown in S4800 15.0KV 8.6mm * 22.0kSE (M, LA10)) that the Bi nano structural material is a hexagonal crystal phase Bi simple substance nano particle, have spherical pattern, particle diameter is about 90nm for characterization result such as Fig. 1.
Bi simple substance nano structural material of the present invention can be used to prepare the Bi modified electrode, and the Bi modified electrode that is obtained can detect the heavy metal ion in the aqueous solution, and detection limit can reach 1 * 10
-4G/L.
Embodiment 2, preparation Bi nano structural material
0.30g the surfactant kayexalate is dissolved in the 50g water, stirs 1 hour on magnetic stirring apparatus, after the dissolving, adds the 1.5g hydrazine hydrate fully, stirs 0.5 hour, the 0.35g bismuth nitrate is disperseed wherein again, stirs 1 hour.Change gained white suspension over to teflon lined stainless steel hydrothermal reaction kettle that capacity is 80mL, after the sealing, put into baking oven, 150 ℃ of heating 6 hours.After reaction finished, water heating kettle left standstill cooling under room temperature environment.Products therefrom changes centrifuge tube over to, is under 1500 rev/mins of conditions centrifugal 12 minutes at rotating speed; Discarding precipitation, change the upper strata suspension over to centrifuge tube, is under 10000 rev/mins of conditions centrifugal 15 minutes at rotating speed, discards supernatant liquid.With excess ethyl alcohol ultrasonic cleaning 10 minutes, is 10000 rev/min conditions under centrifugal 10 minute at rotating speed with centrifugal products therefrom, discards supernatant liquid, repeated washing 1 time.Change the black solid product after the washing over to surface plate, drying is 1 day under the normal temperature ventilation condition, obtains the Bi nano structural material.
The Bi nano structural material is through XRD, laser particle analyzer, SEM, and TEM and EDX characterize.
(show shown in S4800 15.0KV 8.6mm * 22.0kSE (M, LA10)) that the Bi nano structural material is a hexagonal crystal phase Bi simple substance nano particle, have spherical pattern, particle diameter is about 80nm for characterization result such as Fig. 2.
Bi simple substance nano structural material of the present invention can be used to prepare the Bi modified electrode, and the Bi modified electrode that is obtained can detect the heavy metal ion in the aqueous solution, and detection limit can reach 1 * 10
-4G/L.
Embodiment 3, preparation Bi nano structural material
0.4g the surfactant kayexalate is dissolved in the 50g water, stirs 0.8 hour on magnetic stirring apparatus, after the dissolving, adds the 2g hydrazine hydrate fully, stirs 1 hour, the 0.4g bismuth nitrate is disperseed wherein again, stirs 0.5 hour.Change gained white suspension over to teflon lined stainless steel hydrothermal reaction kettle that capacity is 80mL, after the sealing, put into baking oven, 160 ℃ of heating 4 hours.After reaction finished, water heating kettle left standstill cooling under room temperature environment.Products therefrom changes centrifuge tube over to, is under 1000 rev/mins of conditions centrifugal 15 minutes at rotating speed; Discarding precipitation, change the upper strata suspension over to centrifuge tube, is under 10000 rev/mins of conditions centrifugal 15 minutes at rotating speed, discards supernatant liquid.With excess ethyl alcohol ultrasonic cleaning 10 minutes, is 10000 rev/min conditions under centrifugal 10 minute at rotating speed with centrifugal products therefrom, discards supernatant liquid, repeated washing 2 times.Change the black solid product after the washing over to surface plate, drying is 1 day under the normal temperature ventilation condition, obtains the Bi nano structural material.
The Bi nano structural material is through XRD, laser particle analyzer, SEM, and TEM and EDX characterize.
(show shown in S4800 15.0KV 8.6mm * 22.0kSE (M, LA10)) that the Bi nano structural material is a hexagonal crystal phase Bi simple substance nano particle, have spherical pattern, particle diameter is about 60nm for characterization result such as Fig. 3.
Bi simple substance nano structural material of the present invention can be used to prepare the Bi modified electrode, and the Bi modified electrode that is obtained can detect the heavy metal ion in the aqueous solution, and detection limit can reach 1 * 10
-4G/L.
Above embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineers and technicians in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (9)
1. a Bi nano structural material is a hexagonal crystal phase Bi simple substance nano particle, has spherical pattern.
2. Bi nano structural material according to claim 1 is characterized in that: described nano particle diameter is 50～100nm.
3. the preparation method of claim 1 or 2 described Bi nano structural materials comprises the steps:
With the water-soluble suspension that is prepared into of surfactant, hydrazine hydrate and bismuth salt;
Described suspension was reacted 2～10 hours under 120～180 ℃ of conditions, centrifugally obtain described Bi nano structural material.
4. preparation method according to claim 3 is characterized in that: described Bi nano structural material is through washing and dry the processing.
5. according to claim 3 or 4 described preparation methods, it is characterized in that: the mass ratio of described water, described surfactant, described hydrazine hydrate and described bismuth salt is 50: (0.2～0.4): (1～2.5): (0.3～0.4).
6. preparation method according to claim 3 is characterized in that: described suspension was reacted 4～8 hours under 140～160 ℃ of conditions.
7. preparation method according to claim 5 is characterized in that: the cleaning solution of described carrying out washing treatment is an ethanol.
8. preparation method according to claim 3 is characterized in that: described surfactant is a kayexalate.
9. claim 1 or the 2 described Bi nano structural materials application in preparation Bi modified electrode.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121107A (en) * | 2011-11-21 | 2013-05-29 | 中国检验检疫科学研究院 | Bismuth (Bi) simple substance nanometer structure material and preparation method and application thereof |
| CN103121108A (en) * | 2011-11-21 | 2013-05-29 | 中国检验检疫科学研究院 | Bi elementary substance nanostructured materials and preparation method and application thereof |
| CN103436958A (en) * | 2013-08-29 | 2013-12-11 | 陕西师范大学 | Preparation method of bismuth nanocrystalline |
| CN104525940A (en) * | 2014-12-31 | 2015-04-22 | 中国地质大学（武汉） | Bismuth micron particle and manufacturing method thereof |
| CN104668578A (en) * | 2015-02-05 | 2015-06-03 | 北京理工大学 | Preparation method for bismuth nanometer particles |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101569934A (en) * | 2009-05-27 | 2009-11-04 | 河南大学 | Method for preparing metal bismuth nanoparticle |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101569934A (en) * | 2009-05-27 | 2009-11-04 | 河南大学 | Method for preparing metal bismuth nanoparticle |
Non-Patent Citations (3)
| Title |
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| JUNWEI WANG ET AL.,: "Synthesis and Characterization of Bismuth Single-Crystalline Nanowires and Nanospheres", 《INORGANIC CHEMISTRY》, vol. 43, no. 23, 31 December 2004 (2004-12-31), pages 7552 - 7556 * |
| 史运泽: "纳米金属制备及其性能研究", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》, no. 6, 15 June 2007 (2007-06-15) * |
| 杨江海等: "直流电弧等离子法制备铋纳米粉体", 《中国有色金属学报》, vol. 19, no. 2, 28 February 2009 (2009-02-28), pages 334 - 338 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121107A (en) * | 2011-11-21 | 2013-05-29 | 中国检验检疫科学研究院 | Bismuth (Bi) simple substance nanometer structure material and preparation method and application thereof |
| CN103121108A (en) * | 2011-11-21 | 2013-05-29 | 中国检验检疫科学研究院 | Bi elementary substance nanostructured materials and preparation method and application thereof |
| CN103121107B (en) * | 2011-11-21 | 2015-04-22 | 中国检验检疫科学研究院 | Bismuth (Bi) simple substance nanometer structure material and preparation method and application thereof |
| CN103121108B (en) * | 2011-11-21 | 2015-04-22 | 中国检验检疫科学研究院 | Bi elementary substance nanostructured materials and preparation method and application thereof |
| CN103436958A (en) * | 2013-08-29 | 2013-12-11 | 陕西师范大学 | Preparation method of bismuth nanocrystalline |
| CN103436958B (en) * | 2013-08-29 | 2015-02-25 | 陕西师范大学 | Preparation method of bismuth nanocrystalline |
| CN104525940A (en) * | 2014-12-31 | 2015-04-22 | 中国地质大学（武汉） | Bismuth micron particle and manufacturing method thereof |
| CN104668578A (en) * | 2015-02-05 | 2015-06-03 | 北京理工大学 | Preparation method for bismuth nanometer particles |
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Application publication date: 20111012 |