CN102212880B - Elementary substance Bi nano-structured material and preparation method and application thereof - Google Patents
Elementary substance Bi nano-structured material and preparation method and application thereof Download PDFInfo
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- CN102212880B CN102212880B CN 201010141562 CN201010141562A CN102212880B CN 102212880 B CN102212880 B CN 102212880B CN 201010141562 CN201010141562 CN 201010141562 CN 201010141562 A CN201010141562 A CN 201010141562A CN 102212880 B CN102212880 B CN 102212880B
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Abstract
The invention discloses an elementary substance Bi nano-structured material and a preparation method and an application thereof. The elementary substance Bi nano-structured material is a flower-shaped nano particle comprising platy hexagonal phase elementary substances Bi which are used as structural units. The preparation method of the elementary substance Bi nano-structured material comprises the following steps of: dissolving a surfactant, hydrazine hydrate and a bismuth salt in water, and preparing into turbid liquid; and reacting the turbid liquid at the temperature of 80 to 120 DEG C for 18 to 30 hours, and centrifuging the turbid liquid to obtain the elementary substance Bi nano-structured material. The elementary substance Bi nano-structured material can be used for preparing Bi modified electrodes. The obtained Bi modified electrodes can be used for detecting heavy metal ions in an aqueous solution, and the detection limit can reach 1 x 10<-4> grams per liter.
Description
Technical field
The present invention relates to inorganic advanced material technical field, be specifically related to a kind of Bi simple substance nano structural material and preparation method thereof and application.
Background technology
Heavy metal element such as Cr, Cd, Pb and Hg, has become in the 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 environment protection or consumer's goods security monitorings, all seem particularly important.Heavy metal element detection method commonly used has comprised sulphur hydrazone development process and atomic absorption spectrometry, the sample-pretreating method that these two kinds of methods relate to is complicated, the testing process cost is higher, instrument also there is certain requirement, its widespread use is particularly used for the Site Detection of special requirement and has been subject to certain limitation.Stripping volt ampere analysis is being paid close attention in recent years widely as a kind of desirable electrochemical analysis method, is widely used in inorganics trace detection, organism even DNA detection.The key problem in technology of the 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, materials 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 of these novel electrodes is complicated, and it is unstable to detect circulation ratio, thereby can't really be used.
With metal Bi simple substance membrane modified glassy carbon electrode, and used as the working electrode of stripping volt ampere analysis method, can detect heavy metal ion.This type of electrode all shows higher sensitivity in wider work potential scope, and can not be subject to dissolving effect of oxygen, has high application prospect in the trace detection of heavy metal ion.The method for preparing the Bi modified electrode has a lot, usually all needs to experience a process of carrying out pre-treatment with the electrolytic solution that contains Bi.Can omit this pretreatment process and adopt the Bi nanoparticle that it is modified, can obtain again larger electrode activity surface, therefore receive more concern.Regrettably, this type of research, and is carried out as technical support widely in default of high-quality Bi nano structural material.Still remain systematic Study for the synthesis of the fast and effectively novel method of Bi nanostructure.
Summary of the invention
The purpose of this invention is to provide a kind of high-quality Bi simple substance nano structural material and preparation method thereof and application.
Bi simple substance nano structural material provided by the present invention is the nano particle with flower shape pattern that structural unit forms by sheet hexagonal crystal phase Bi simple substance.
Bi simple substance nano structural material of the present invention, wherein, described flower diameter is 1000～1500nm.
The preparation method of Bi simple substance nano structural material provided by the present invention comprises the steps:
With the water-soluble suspension liquid that is prepared into of tensio-active agent, hydrazine hydrate and bismuth salt;
Described suspension liquid was reacted 18～30 hours under 80～120 ℃ of conditions, centrifugally obtain described Bi simple substance nano structural material.
The preparation method of Bi simple substance nano structural material of the present invention, wherein, described Bi simple substance nano structural material is through washing and drying treatment.
The preparation method of Bi simple substance nano structural material of the present invention, wherein, the mass ratio of described water, described tensio-active agent, described hydrazine hydrate and described bismuth salt is 50: (0.2～0.4): (1～2.5): (0.3～0.4).
The preparation method of Bi simple substance nano structural material of the present invention wherein, reacts described suspension liquid 24～28 hours under 90～110 ℃ of conditions.
The preparation method of Bi simple substance nano structural material of the present invention, wherein, the washings of described carrying out washing treatment is ethanol.
The preparation method of Bi simple substance nano structural material of the present invention, wherein, described tensio-active agent is sodium polystyrene sulfonate.
The Bi simple substance nano structural material that the preparation method of Bi simple substance nano structural material of the present invention obtains is the nano structural material with flower pattern that forms take sheet hexagonal crystal phase Bi simple substance as structural unit, about the length of side 50nm of this structural unit, the diameter of flower is 1000～1500nm, such Bi simple substance nano structural material quality is high, be used for preparing the Bi modified electrode, the Bi modified electrode that obtains 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.
Embodiment
Embodiment 1, preparation Bi simple substance nano structural material
0.2g the tensio-active agent sodium polystyrene sulfonate is dissolved in the 50g water, stirs 0.8 hour at magnetic stirring apparatus, after the dissolving, adds the 2g hydrazine hydrate fully, stirs 0.5 hour, the 0.3g Trichlorobismuthine is disperseed wherein again, stirs 0.8 hour.Change gained white suspension liquid over to teflon lined stainless steel hydrothermal reaction kettle that capacity is 80mL, after the sealing, put into baking oven, 90 ℃ of heating 28 hours.After reaction finished, hydrothermal reaction kettle left standstill cooling under room temperature environment.Products therefrom changes centrifuge tube over to, is under 1000 rev/mins of conditions centrifugal 10 minutes at rotating speed; Discarding precipitation, change the upper strata suspension liquid over to centrifuge tube, is under 8000 rev/mins of conditions centrifugal 15 minutes at rotating speed, discards supernatant liquid.With excess ethyl alcohol ultrasonic cleaning 8 minutes, be 8000 rev/min conditions under centrifugal 10 minute at rotating speed with centrifugal products therefrom, discard supernatant liquid, repeated washing 1 time.Change the black solid product after the washing over to watch-glass, drying is 1 day under the normal temperature ventilation condition, obtains Bi simple substance nano structural material.
Bi simple substance nano structural material is through XRD, laser particle analyzer, SEM, and TEM and EDX characterize.
Characterization result such as Fig. 1 (S4800 5.0KV 8.3mm * 60.0kSE (U, LA10)) show shown in that Bi simple substance nano structural material is the nano structural material with flower pattern take sheet hexagonal crystal phase Bi simple substance as structural unit, about the length of side 50nm of this structural unit, the diameter of flower is 1000～1500nm.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 obtains can detect the heavy metal ion in the aqueous solution, and detection limit can reach 1 * 10
-4G/L.
Embodiment 2, preparation Bi simple substance nano structural material
0.3g the tensio-active agent sodium polystyrene sulfonate is dissolved in the 50g water, stirs 1 hour at magnetic stirring apparatus, after the dissolving, adds the 1g hydrazine hydrate fully, stirs 0.5 hour, the 0.35g Trichlorobismuthine is disperseed wherein again, stirs 1 hour.Change gained white suspension liquid over to teflon lined stainless steel hydrothermal reaction kettle that capacity is 80mL, after the sealing, put into baking oven, 100 ℃ of heating 26 hours.After reaction finished, hydrothermal reaction 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 liquid 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, be 10000 rev/min conditions under centrifugal 10 minute at rotating speed with centrifugal products therefrom, discard supernatant liquid, repeated washing 1 time.Change the black solid product after the washing over to watch-glass, drying is 1 day under the normal temperature ventilation condition, obtains Bi simple substance nano structural material.
Bi simple substance nano structural material is through XRD, laser particle analyzer, SEM, and TEM and EDX characterize.
Characterization result such as Fig. 2 (S4800 5.0KV 8.3mm * 60.0kSE (U, LA30)) show shown in that Bi simple substance nano structural material is the nano structural material with flower pattern take sheet hexagonal crystal phase Bi simple substance as structural unit, about the length of side 50nm of this structural unit, the diameter of flower is 1000～1500nm.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 obtains can detect the heavy metal ion in the aqueous solution, and detection limit can reach 1 * 10
-4G/L.
Embodiment 3, preparation Bi simple substance nano structural material
0.4g the tensio-active agent sodium polystyrene sulfonate is dissolved in the 50g water, stirs 0.5 hour at magnetic stirring apparatus, after the dissolving, adds the 2.5g hydrazine hydrate fully, stirs 1 hour, the 0.4g Trichlorobismuthine is disperseed wherein again, stirs 0.5 hour.Change gained white suspension liquid over to teflon lined stainless steel hydrothermal reaction kettle that capacity is 80mL, after the sealing, put into baking oven, 110 ℃ of heating 24 hours.After reaction finished, hydrothermal reaction 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 liquid 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, be 10000 rev/min conditions under centrifugal 10 minute at rotating speed with centrifugal products therefrom, discard supernatant liquid, repeated washing 2 times.Change the black solid product after the washing over to watch-glass, drying is 1 day under the normal temperature ventilation condition, obtains Bi simple substance nano structural material.
Bi simple substance nano structural material is through XRD, laser particle analyzer, SEM, and TEM and EDX characterize.
Characterization result such as Fig. 3 (S4800 15.0KV 5.9mm * 30.0kSE (M, LA30)) show shown in that Bi simple substance nano structural material is the nano structural material with flower pattern take sheet hexagonal crystal phase Bi simple substance as structural unit, about the length of side 50nm of this structural unit, the diameter of flower is 1000～1500nm.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 obtains 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 engineering technical personnel 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 (7)
1. a Bi simple substance nano structural material is the nano particle with flower shape pattern that structural unit forms by sheet hexagonal crystal phase Bi simple substance.
2. Bi simple substance nano structural material according to claim 1, it is characterized in that: described flower diameter is 1000～1500nm.
3. the preparation method of claim 1 or 2 described Bi simple substance nano structural materials comprises the steps:
With the water-soluble suspension liquid that is prepared into of tensio-active agent, hydrazine hydrate and bismuth salt; The mass ratio of described water, described tensio-active agent, described hydrazine hydrate and described bismuth salt is 50:(0.2～0.4): (1～2.5): (0.3～0.4); Described tensio-active agent is sodium polystyrene sulfonate;
Described suspension liquid was reacted 18～30 hours under 80～120 ℃ of conditions, centrifugally obtain described Bi simple substance nano structural material.
4. preparation method according to claim 3 is characterized in that: the washing of described Bi simple substance nano structural material process and drying treatment.
5. preparation method according to claim 3 is characterized in that: described suspension liquid was reacted 24～28 hours under 90～110 ℃ of conditions.
6. preparation method according to claim 4, it is characterized in that: the washings of described carrying out washing treatment is ethanol.
7. claim 1 or the 2 described Bi simple substance nano structural materials application in preparation Bi modified electrode.
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| 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 |
| 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 |
| CN103774217B (en) * | 2012-10-26 | 2016-08-24 | 北京师范大学 | A kind of preparation method of micron order bismuth single crystal flower |
| CN104525940A (en) * | 2014-12-31 | 2015-04-22 | 中国地质大学（武汉） | Bismuth micron particle and manufacturing method thereof |
| CN105251474B (en) * | 2015-10-09 | 2017-07-25 | 重庆文理学院 | One kind is used for light-catalysed bismuth nanospheres and preparation method |
| CN106099076B (en) * | 2016-08-22 | 2018-09-21 | 北京化工大学 | A kind of flower-shaped nitrogen-doped carbon cladding bismuth structural composite material and its preparation method and application |
| CN108421987A (en) * | 2018-03-16 | 2018-08-21 | 南京工业大学 | A kind of preparation method of sheet bismuth with elementary |
| CN113274499B (en) * | 2021-06-25 | 2022-06-24 | 中国药科大学 | Bionic bismuth nanoflower and preparation method and application thereof |
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Non-Patent Citations (2)
| Title |
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| A facile water-based process for preparation of stabilized Bi nanoparticles;Yi Wang et al;《 Materials Research Bulletin》;20080408;第44卷;220-223 * |
| Yi Wang et al.A facile water-based process for preparation of stabilized Bi nanoparticles.《 Materials Research Bulletin》.2008,第44卷 |
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