CN104525940A - Bismuth micron particle and manufacturing method thereof - Google Patents
Bismuth micron particle and manufacturing method thereof Download PDFInfo
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- CN104525940A CN104525940A CN201410852761.XA CN201410852761A CN104525940A CN 104525940 A CN104525940 A CN 104525940A CN 201410852761 A CN201410852761 A CN 201410852761A CN 104525940 A CN104525940 A CN 104525940A
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Abstract
The invention provides a bismuth micron particle. The particle is a bismuth elementary substance, the particle size of the particle is 1 micron to 3 microns, and the particle is spherical or polyhedral. The method for manufacturing the particle comprises the following steps that a bismuth source and template agents are added to glycol and stirred to be completely dissolved, then the pH value of a solution is adjusted to be larger than 10 while stirring is carried out, after solute is completely dissolved, the solution is transferred into a closed polytetrafluoroethylene lining high-pressure reaction still, a reaction is carried out for more than 10 h under the condition of 160 DEG C to 200 DEG C, a product is centrifuged or filtered after the reaction is finished, residual solute is removed through washing, and the bismuth micron particle can be obtained through drying and cooling. The positive colossal magnetoresistance of the bismuth micron particle is more than 700 percent at low temperature, the positive colossal magnetoresistance of the bismuth micron particle is more than 180 percent at indoor temperature, and the manufacturing method of the bismuth micron particle is simple.
Description
Technical field
The invention provides a kind of bismuth micron particles, under being specifically related to a kind of alkaline environment, prepare the method for high giant magnetic effect bismuth micron particles, belong to chemical, function micro-nano material technical field.
Background technology
Giant magnetoresistance effect refers to the phenomenon of the great variety of the material resistance caused by externally-applied magnetic field, can be used for the science technology information fields such as magnetic recording, magnetic head reading, magnetic information storage, giant magnetoresistance sensor, magneto-electronics.
Bismuth is a kind of semimetal, and the Fermi surface of its high anisotropy, low carrier concentration and its little carrier effective mass make it have unique electrical properties.Because bismuth has large Fermi's wavelength and long carrier mean free path, thus large quantity research concentrates on its Quantum Teleportation and size confinement effect.Minimum carrier effective mass and mean free path make bismuth have extraordinary giant magnetoresistance effect, the nano material that bismuth simple substance comprises film, block and various pattern has all been successfully synthesized and has studied, and its synthesis technique related to includes chemistry or physical vapour deposition (PVD), electrochemical deposition, solution reduction etc.Wherein the giant magnetic effect of bismuth simple substance micron monocrystal thin films is the most excellent, and the giant magnetoresistance of block, various pattern nano material is all difficult to reach more than 300%.The high bismuth micron particles of degree of crystallinity has longer carrier mean free path, thus has relative to block materials or the better giant magnetoresistance effect of nano material, and synthesizes bismuth simple substance under synthesizing bismuth micron particles and alkali condition and there is no bibliographical information.
Summary of the invention
The invention provides a kind of bismuth micron particles, solve the deficiency in background technology, the positive at low temperatures giant magnetoresistance of this bismuth micron particles is more than 700%, and under room temperature, positive giant magnetoresistance is more than 180%, and its preparation method is simple.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of bismuth micron particles, described particle is bismuth simple substance, its particle diameter is 1 ~ 3 μm, spherical in shape or the polyhedral of particle, prepared by employing following methods: add in ethylene glycol by bismuth source and template, be stirred to and dissolve completely, stir the pH value of solution to be adjusted to back and be greater than 10, after solute dissolves completely, solution is transferred in airtight polytetrafluoroethyllining lining autoclave, more than 10h is reacted under the condition of 160 ~ 200 DEG C, reaction terminate after by products therefrom centrifugal or filter after, after the residual solute of washing removing, Drying and cooling can obtain bismuth micron particles.
Described bismuth source is bismuth nitrate or bismuth acetate, and described template is CTAC, or the Dual Surfactants that CTAC and PVP mixes, and the mol ratio of described bismuth source and template is 0.5 ~ 3:1.
The ethylene glycol solution of KOH is adopted to regulate the pH value of solution to being greater than 10.
Compared with prior art, the preparation method of bismuth micron particles provided by the present invention is simple, has prepared bismuth with elementary crystal micron particles under alkali condition.Its pattern is comparatively homogeneous, and be spherical or polyhedron, particle diameter is 1 ~ 3 μm.The positive at low temperatures giant magnetoresistance of preparation-obtained bismuth micron particles reaches 700%, giant magnetoresistance about 180% under room temperature.
Accompanying drawing explanation
The SEM photo of the bismuth micron particles that Fig. 1 provides for the embodiment of the present invention;
The XRD figure of the bismuth micron particles that Fig. 2 provides for the embodiment of the present invention;
Fig. 3 is target product magnetic field intensity-MR curves (T=10K, 300K).
Detailed description of the invention
Below in conjunction with accompanying drawing, detailed specific description is done to the present invention, but protection scope of the present invention is not limited to following examples.
Embodiment 1
Bismuth micron particles prepared in the present embodiment adopts following methods to obtain: 3mmol bismuth nitrate and 3mmolCTAC are joined in 60mL ethylene glycol, dissolving is stirred under 500r/min, then drip the ethylene glycol solution of the KOH of 1mol/L wherein, be greater than 10 to pH.Obtain settled solution, after continuing to stir 1h, solution is transferred in airtight polytetrafluoroethyllining lining autoclave, and be placed in 180 DEG C of convection oven and react 12h, naturally take out after cooling, by products therefrom suction filtration, use deionized water to be washed till neutrality, use ethanol to wash away template.Finally the product filtered is obtained target product in 60 DEG C of vacuum drying 12h.
As shown in Figure 1, as can be seen from Fig. 1, the particle diameter of described bismuth micron particles is 1 ~ 3 μm to the Flied emission surface sweeping electromicroscopic photograph of the bismuth micron particles that the present embodiment provides, the spherical in shape or polyhedral of particle.The XRD figure of the bismuth micron particles prepared by the present embodiment as shown in Figure 2.Magnetic field intensity-MR curves the figure of the bismuth micron particles prepared by the present embodiment as shown in Figure 3, as can be seen from Fig. 3, described bismuth micron particles positive giant magnetoresistance under low temperature (10K) is more than 700%, and under room temperature (300K), positive giant magnetoresistance is more than 180%.
Embodiment 2
Bismuth micron particles prepared in the present embodiment adopts following methods to obtain: 3mmol bismuth acetate and 2.5mmolCTAC are joined in 60mL ethylene glycol, dissolving is stirred under 500r/min, then drip the ethylene glycol solution of the KOH of 1mol/L wherein, be greater than 10 to pH.Obtain settled solution, after continuing to stir 1h, solution is transferred in airtight polytetrafluoroethyllining lining autoclave, and be placed in 160 DEG C of convection oven and react 12h, naturally take out after cooling, by products therefrom suction filtration, use deionized water to be washed till neutrality, use ethanol to wash away template.Finally the product filtered is obtained target product in 60 DEG C of vacuum drying 12h.
Embodiment 3
Bismuth micron particles prepared in the present embodiment adopts following methods to obtain: 3mmol bismuth nitrate and 1mmolCTAC are joined in 60mL ethylene glycol, dissolving is stirred under 500r/min, then drip the ethylene glycol solution of the KOH of 1mol/L wherein, be greater than 10 to pH.Obtain settled solution, after continuing to stir 1h, solution is transferred in airtight polytetrafluoroethyllining lining autoclave, and be placed in 160 DEG C of convection oven and react 12h, naturally take out after cooling, by products therefrom suction filtration, use deionized water to be washed till neutrality, use ethanol to wash away template.Finally the product filtered is obtained target product in 60 DEG C of vacuum drying 12h.
Embodiment 4
Bismuth micron particles prepared in the present embodiment adopts following methods to obtain: 3mmol bismuth nitrate and 3mmolCTAC are joined in 35mL ethylene glycol, dissolving is stirred under 500r/min, then drip the ethylene glycol solution of the KOH of 1mol/L wherein, be greater than 10 to pH.Obtain settled solution, after continuing to stir 1h, solution is transferred in airtight polytetrafluoroethyllining lining autoclave, and be placed in 180 DEG C of convection oven and react 24h, naturally take out after cooling, by products therefrom suction filtration, use deionized water to be washed till neutrality, use ethanol to wash away template.Finally the product filtered is obtained target product in 60 DEG C of vacuum drying 12h.
Embodiment 5
Bismuth micron particles prepared in the present embodiment adopts following methods to obtain: 3mmol bismuth nitrate and 3mmolCTAC and 1gPVP are joined in 60mL ethylene glycol, dissolving is stirred under 500r/min, then drip the ethylene glycol solution of the KOH of 1mol/L wherein, be greater than 10 to pH.Obtain settled solution, after continuing to stir 1h, solution is transferred in airtight polytetrafluoroethyllining lining autoclave, and be placed in 180 DEG C of convection oven and react 24h, naturally take out after cooling, products therefrom is used centrifuge separating, washing, rotating speed is 1500 ~ 4000r/min, centrifugation time is 5min, uses deionized water to be washed till neutrality, uses ethanol to wash away template.Finally the product filtered is obtained target product in 60 DEG C of vacuum drying 12h.
Claims (4)
1. a bismuth micron particles, it is characterized in that: described particle is bismuth simple substance, its particle diameter is 1 ~ 3 μm, spherical in shape or the polyhedral of particle, prepared by employing following methods: add in ethylene glycol by bismuth source and template, be stirred to and dissolve completely, while stirring the pH value of solution is adjusted to subsequently and is greater than 10, after solute dissolves completely, solution is transferred in airtight polytetrafluoroethyllining lining autoclave, more than 10h is reacted under the condition of 160 ~ 200 DEG C, reaction terminate after by products therefrom centrifugal or filter after, after the residual solute of washing removing, Drying and cooling can obtain bismuth micron particles.
2. bismuth micron particles according to claim 1, it is characterized in that: described bismuth source is bismuth nitrate or bismuth acetate, described template is CTAC, or the Dual Surfactants that CTAC and PVP mixes, and the mol ratio of described bismuth source and template is 0.5 ~ 3:1.
3. bismuth micron particles according to claim 1, is characterized in that: adopt the ethylene glycol solution of KOH to regulate the pH value of solution to being greater than 10.
4. bismuth micron particles according to claim 1, is characterized in that: the positive at low temperatures giant magnetoresistance of described bismuth micron particles is more than 700%, and under room temperature, positive giant magnetoresistance is more than 180%.
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| CN104874811A (en) * | 2015-05-22 | 2015-09-02 | 武汉工程大学 | Preparing method of simple substance bismuth/bismuth compound nanocomposite with oxygen vacancies |
| CN105798321A (en) * | 2016-01-29 | 2016-07-27 | 宁波工程学院 | Half-metallic bismuth nanoribbon, half-metallic bismuth nanospheres and preparation method of half-metallic bismuth nanoribbon and half-metallic bismuth nanospheres |
| CN105903474A (en) * | 2016-05-12 | 2016-08-31 | 江苏华夏制漆科技有限公司 | Preparation method of magnetic Fe3O4@ elemental bismuth sphere photocatalyst |
| CN107469804A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | A kind of titania-based composite photocatalyst material of nano particle bismuth load 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 |
| CN108436101A (en) * | 2018-04-27 | 2018-08-24 | 同济大学 | A kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres |
| CN112337498A (en) * | 2020-11-17 | 2021-02-09 | 石家庄铁道大学 | Bismuth/graphite phase carbon nitride/bismuth oxybromide composite photocatalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104874811A (en) * | 2015-05-22 | 2015-09-02 | 武汉工程大学 | Preparing method of simple substance bismuth/bismuth compound nanocomposite with oxygen vacancies |
| CN105798321A (en) * | 2016-01-29 | 2016-07-27 | 宁波工程学院 | Half-metallic bismuth nanoribbon, half-metallic bismuth nanospheres and preparation method of half-metallic bismuth nanoribbon and half-metallic bismuth nanospheres |
| CN105903474A (en) * | 2016-05-12 | 2016-08-31 | 江苏华夏制漆科技有限公司 | Preparation method of magnetic Fe3O4@ elemental bismuth sphere photocatalyst |
| CN107469804A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | A kind of titania-based composite photocatalyst material of nano particle bismuth load 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 |
| CN108436101A (en) * | 2018-04-27 | 2018-08-24 | 同济大学 | A kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres |
| CN112337498A (en) * | 2020-11-17 | 2021-02-09 | 石家庄铁道大学 | Bismuth/graphite phase carbon nitride/bismuth oxybromide composite photocatalyst and preparation method and application thereof |
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Application publication date: 20150422 |