CN102659188A - Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof - Google Patents
Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof Download PDFInfo
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- CN102659188A CN102659188A CN2012101587945A CN201210158794A CN102659188A CN 102659188 A CN102659188 A CN 102659188A CN 2012101587945 A CN2012101587945 A CN 2012101587945A CN 201210158794 A CN201210158794 A CN 201210158794A CN 102659188 A CN102659188 A CN 102659188A
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Abstract
The invention discloses a magnetic ferric oxide micrometer flower material with a multi-stage structure and a preparation method of the magnetic ferric oxide micrometer flower material. The magnetic ferric oxide micrometer flower material with the multi-stage structure has the shape of a flower which is arranged by nano-pieces with the thickness of 85-95nm in an interlaced way assembled by spherical particles with the particle sizes from 20nm to 30nm and has the multi-stage structure, and integrates the nano-grains, the nano-pieces and the micro flower. The preparation method comprises the following steps of: preparing a solution with the concentration of 0.05-0.6mol/L based on hexahydrated ferric trichloride as an iron source and ethylene glycol as solvent, adding a surface active agent, stirring to obtain clear solution, adding urea, reacting for 30-90min by an ethylene glycol auxiliary method at the temperature of 190-197 DEG C, centrifugally separating, cleaning and drying, and calcining for 1-5h at high temperature of 300-500 DEG C, so that the magnetic ferric oxide micrometer flower material can be obtained. The preparation method is simple in technology, low in cost, easy to produce on a large scale, and safe and reliable in production process; and the product is good in repeatability, regular in shape, concentrated in particle size distribution, and free from agglomeration.
Description
Technical field
The present invention relates to a kind of magnetic red oxide of iron material, be specifically related to a kind of magnetic ferric oxide micron floral material, the invention still further relates to this preparation methods with multilevel hierarchy.
Background technology
Nano particle makes it all show the new feature that is different from conventional solid and macroscopic particle at aspects such as light, electricity, magnetic, heat, mechanical property, chemical property, bio-physical properties owing to have quantum size effect, surface effects, macro quanta tunnel effect, enclosed pasture obstruction and dielectric confinement effect.And the performance of nano material depends on the microscopic appearance of nanoparticle to a great extent, and therefore, the nano material of synthetic various special appearances becomes the indispensable important component part in nano science field.
The oxide compound of the iron that red oxide of iron is a kind of cheapness, environmental protection, performance is the most stable has the characteristic of n-N-type semiconductorN, has a wide range of applications at aspects such as photochemical catalysis, lithium ion battery, gas sensor, magnetics materials.And the micro-flowers of multilevel hierarchy is collected rice particle, nanometer sheet and three kinds of structures of micro-flowers in one because of it, makes it in fields such as write head, nano-catalytic, biosensor, nanosecond medical sciences good prospects for application arranged.Yet do not see multilevel hierarchy alpha-acetol-red oxide of iron (α-Fe at present as yet
2O
3) pertinent literature and the patent report of micro-flowers.
Summary of the invention
The purpose of this invention is to provide a kind of magnetic ferric oxide micron floral material and preparation method thereof with multilevel hierarchy.
A kind of magnetic ferric oxide micron floral material with multilevel hierarchy; Be by particle diameter be thickness that the spheroidal particle of 20-30 nm is assembled into be the nanometer sheet of 85-95 nm be staggered form have the flower-shaped of multilevel hierarchy, collect a rice particle, nanometer sheet and three kinds of structures of micro-flowers in one.
The present invention realizes through following technical scheme:
A kind of preparation method with magnetic ferric oxide micron floral material of multilevel hierarchy may further comprise the steps:
(1) be source of iron with the Iron(III) chloride hexahydrate, terepthaloyl moietie is solvent, obtains the solution of concentration 0.05 ~ 0.6 mol/L, adds tensio-active agent again, stirs at normal temperatures and pressures, and Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtains settled solution;
(2) urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts terepthaloyl moietie auxiliary law reaction 30 ~ 90 min down at 190 ~ 197 ℃;
(4) reaction finishes the back spinning, and throw out is cleaned with absolute ethyl alcohol, and oven dry obtains the Powdered precursor of yellow-green colour then;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air or oxygen at 300 ~ 500 ℃ of following high-temperature calcination 1 ~ 5 h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
Further, the mol ratio of described tensio-active agent and Iron(III) chloride hexahydrate is 0.065:1 ~ 0.67:1.
The mol ratio of described Iron(III) chloride hexahydrate and urea is 0.01 ~ 4:1.
Described tensio-active agent is Vinylpyrrolidone polymer, cetyl trimethylammonium bromide or tetrabutylammonium chloride.
Compared with prior art, the present invention has following advantage:
(1) preparation technology is simple, and required equipment is simple and easy;
(2) with respect to the complicated technology of template, present method production cost is low, and easy realization of large-scale production makes things convenient for practical application in industry;
(3) do not produce hazardous and noxious substances in the preparation process, safe reliability is high;
(4) product favorable reproducibility, the product pattern is regular, and centralized particle diameter does not have and reunites.
Description of drawings
Presoma sem (SEM) photo that Fig. 1 makes for embodiment 1;
The X-ray energy spectrum analysis of the presoma that Fig. 2 makes for embodiment 1;
Sem (SEM) photo of the multilevel hierarchy magnetic ferric oxide micron flower that Fig. 3 makes for embodiment 1;
Fig. 4 is the partial enlarged drawing of Fig. 3;
Fig. 5 is the partial enlarged drawing of Fig. 3;
Fig. 6 executes the multilevel hierarchy magnetic ferric oxide micron flower hysteresis graph at normal temperatures that example 1 makes.
Embodiment
Embodiment 1
A kind of preparation method with magnetic ferric oxide micron floral material of multilevel hierarchy may further comprise the steps:
(1) be source of iron with the 0.005mol Iron(III) chloride hexahydrate; 100ml terepthaloyl moietie is solvent, adds the tensio-active agent tetrabutylammonium chloride again, stirs at normal temperatures and pressures; Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtain the settled solution that iron trichloride concentration is 0.05 mol/L;
(2) 0.5mol urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts the terepthaloyl moietie auxiliary law to react 60 min down at 190 ℃;
(4) reaction finishes the back spinning, and the yellow-green precipitate thing that obtains is dried 12 h down at 60 ℃ then with absolute ethanol washing 3 times, can obtain α-Fe
2O
3Presoma;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air at 300 ~ 350 ℃ of following high-temperature calcination 3 h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
Ferric oxide micron floral material with multilevel hierarchy be by particle diameter be thickness that the spheroidal particle of 20-30 nm is assembled into be the nanometer sheet of 85-95 nm be staggered form have the flower-shaped of multilevel hierarchy, collect a rice particle, nanometer sheet and three kinds of structures of micro-flowers in one.
Fig. 1 is presoma sem (SEM) photo that step (4) makes, and as can be seen from the figure, adopting the presoma of present method preparation is flower-like structure.
Fig. 2 carries out the X-ray energy spectrum analysis to presoma, and the result shows that it is elementary composition for Fe, O and three kinds of elements of C.
Fig. 3 is sem (SEM) photo of the multilevel hierarchy magnetic ferric oxide micron flower of preparation, and as can be seen from the figure, the magnetic red oxide of iron that obtains after the calcining is the micro-flowers that is assembled into by nanometer sheet.
Fig. 4,5 is the partial enlarged drawing of Fig. 3, and the result shows that this nanometer sheet is to be assembled by the small-particle about 22 nm.
Fig. 6 is the multilevel hierarchy magnetic ferric oxide micron flower hysteresis curve at normal temperatures of preparation; Can find out that the ferric oxide micron flower of this structure is the soft magnetism characteristic, its saturation magnetization is 0.67 emu/g; Residual magnetization is 0.10 emu/g, and coercive force is 127 Oe.
(1) be source of iron with the 0.01mol Iron(III) chloride hexahydrate; 100ml terepthaloyl moietie is solvent; Add tensio-active agent tetrabutylammonium chloride 0.00065mol again; Stir at normal temperatures and pressures, Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtain the settled solution that iron trichloride concentration is 0.1 mol/L;
(2) 0.1mol urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts the terepthaloyl moietie auxiliary law to react 70 min down at 192 ℃;
(4) reaction finishes the back spinning, and the yellow-green precipitate thing that obtains is dried 12 h down at 65 ℃ then with absolute ethanol washing 3 times, can obtain α-Fe
2O
3Presoma;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air at 340 ~ 390 ℃ of following high-temperature calcination 5h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
Embodiment 3
(1) be source of iron with the 0.06mol Iron(III) chloride hexahydrate; 100ml terepthaloyl moietie is solvent; Add the tensio-active agent cetyl trimethylammonium bromide again; Stir at normal temperatures and pressures, Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtain the settled solution that iron trichloride concentration is 0.6 mol/L;
(2) 0.03mol urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts the terepthaloyl moietie auxiliary law to react 30 min down at 197 ℃;
(4) reaction finishes the back spinning, and the yellow-green precipitate thing that obtains is dried 13 h down at 55 ℃ then with absolute ethanol washing 4 times, can obtain α-Fe
2O
3Presoma;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air at 380 ~ 460 ℃ of following high-temperature calcination 4 h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
Embodiment 4
(1) be source of iron with the 0.03mol Iron(III) chloride hexahydrate; 100ml terepthaloyl moietie is solvent; Add the tensio-active agent cetyl trimethylammonium bromide again; Stir at normal temperatures and pressures, Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtain the settled solution that iron trichloride concentration is 0.03mol/L;
(2) 0.01mol urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts the terepthaloyl moietie auxiliary law to react 90 min down at 195 ℃;
(4) reaction finishes the back spinning, and the yellow-green precipitate thing that obtains is dried 11 h down at 58 ℃ then with absolute ethanol washing 2 times, can obtain α-Fe
2O
3Presoma;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air at 450 ~ 5000 ℃ of following high-temperature calcination 1 h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
Embodiment 5
(1) be source of iron with the 0.008mol Iron(III) chloride hexahydrate; 100ml terepthaloyl moietie is solvent, adds the tensio-active agent Vinylpyrrolidone polymer again, stirs at normal temperatures and pressures; Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtain the settled solution that iron trichloride concentration is 0.08 mol/L;
(2) 0.002mol urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts the terepthaloyl moietie auxiliary law to react 80 min down at 196 ℃;
(4) reaction finishes the back spinning, and the yellow-green precipitate thing that obtains is dried 12 h down at 60 ℃ then with absolute ethanol washing 3 times, can obtain α-Fe
2O
3Presoma;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air at 420 ~ 480 ℃ of following high-temperature calcination 3 h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
(1) be source of iron with the 0.01mol Iron(III) chloride hexahydrate; 100ml terepthaloyl moietie is solvent; Add tensio-active agent tetrabutylammonium chloride 0.0067mol again; Stir at normal temperatures and pressures, Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtain the settled solution that iron trichloride concentration is 0.1 mol/L;
(2) 0.1mol urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts the terepthaloyl moietie auxiliary law to react 70 min down at 192 ℃;
(4) reaction finishes the back spinning, and the yellow-green precipitate thing that obtains is dried 12 h down at 65 ℃ then with absolute ethanol washing 3 times, can obtain α-Fe
2O
3Presoma;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air at 340 ~ 390 ℃ of following high-temperature calcination 5h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
Claims (5)
1. magnetic ferric oxide micron floral material with multilevel hierarchy; It is characterized in that be by particle diameter be thickness that the spheroidal particle of 20-30 nm is assembled into be the nanometer sheet of 85-95 nm be staggered form have the flower-shaped of multilevel hierarchy, collect a rice particle, nanometer sheet and three kinds of structures of micro-flowers in one.
2. the described preparation method with magnetic ferric oxide micron floral material of multilevel hierarchy of claim 1 is characterized in that may further comprise the steps:
(1) be source of iron with the Iron(III) chloride hexahydrate, terepthaloyl moietie is solvent, obtains the solution of concentration 0.05 ~ 0.6 mol/L, adds tensio-active agent again, stirs at normal temperatures and pressures, and Iron(III) chloride hexahydrate and tensio-active agent are dissolved fully, obtains settled solution;
(2) urea is added in the settled solution that step (1) disposed, stir, thorough mixing obtains the reddish-brown settled solution;
(3) the above-mentioned solution with step (2) preparation adopts terepthaloyl moietie auxiliary law reaction 30 ~ 90 min down at 190 ~ 197 ℃;
(4) reaction finishes the back spinning, and throw out is cleaned with absolute ethyl alcohol, and oven dry obtains the Powdered precursor of yellow-green colour then;
(5) precursor is placed the vacuum atmosphere box-type furnace, bubbling air or oxygen at 300 ~ 500 ℃ of following high-temperature calcination 1 ~ 5 h, can obtain having the ferric oxide micron floral material of multilevel hierarchy.
3. the preparation method with magnetic ferric oxide micron floral material of multilevel hierarchy according to claim 2, the mol ratio that it is characterized in that tensio-active agent and Iron(III) chloride hexahydrate is 0.065:1 ~ 0.67:1.
4. according to claim 2 or 3 described a kind of preparing methods with magnetic ferric oxide micron floral material of multilevel hierarchy, the mol ratio that it is characterized in that described Iron(III) chloride hexahydrate and urea is 0.01 ~ 4:1.
5. according to claim 2 or 3 described a kind of preparing methods, it is characterized in that described tensio-active agent is Vinylpyrrolidone polymer, cetyl trimethylammonium bromide or tetrabutylammonium chloride with magnetic ferric oxide micron floral material of multilevel hierarchy.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105762354A (en) * | 2016-05-17 | 2016-07-13 | 安徽师范大学 | Flower-like ferric oxide nanometer material, preparation method thereof, lithium ion battery negative pole and lithium ion battery |
| CN106093137A (en) * | 2016-06-20 | 2016-11-09 | 吉林大学 | A kind of based on α Fe2o3acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof |
| CN106946294A (en) * | 2017-04-11 | 2017-07-14 | 深圳市佩成科技有限责任公司 | Hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation |
| CN106966436A (en) * | 2017-04-11 | 2017-07-21 | 深圳市佩成科技有限责任公司 | Hollow structure Fe is carried out based on microwave synthesis2O3The method of preparation |
| CN106966435A (en) * | 2017-04-11 | 2017-07-21 | 深圳市佩成科技有限责任公司 | Hollow structure Fe is carried out based on oil bath synthesis2O3The method of preparation |
| CN107706413A (en) * | 2017-11-08 | 2018-02-16 | 苏州宇量电池有限公司 | A kind of leaf Cyclic dart type iron oxide cathode material of nanometer three and preparation method thereof |
| CN107946590A (en) * | 2017-11-09 | 2018-04-20 | 湖南友能高新技术有限公司 | A kind of pomegranate type structure di-iron trioxide and preparation method thereof and the application as lithium-ion negative pole active material |
| CN107973348A (en) * | 2017-11-28 | 2018-05-01 | 合肥学院 | A kind of spherical di-iron trioxide of micro-meter scale and preparation method thereof |
| CN108213454A (en) * | 2018-03-28 | 2018-06-29 | 燕山大学 | A kind of preparation method of the flower-shaped fe submicron particles of nano particle assembling |
| CN110801804A (en) * | 2019-12-09 | 2020-02-18 | 安徽建筑大学 | Metal oxide nano adsorption material with micro-nano hierarchical structure and preparation method thereof |
| CN110903490A (en) * | 2019-12-13 | 2020-03-24 | 湖南文理学院 | Novel metal organic compound semiconductor micro-nano material and preparation method and application thereof |
| CN114853082A (en) * | 2022-05-08 | 2022-08-05 | 西南石油大学 | Preparation method of spherical ferric oxide negative electrode material of lithium ion battery |
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| CN105762354B (en) * | 2016-05-17 | 2018-04-13 | 安徽师范大学 | A kind of flower-shaped ferric oxide nano-material and preparation method thereof, negative electrode of lithium ion battery and lithium ion battery |
| CN105762354A (en) * | 2016-05-17 | 2016-07-13 | 安徽师范大学 | Flower-like ferric oxide nanometer material, preparation method thereof, lithium ion battery negative pole and lithium ion battery |
| CN106093137A (en) * | 2016-06-20 | 2016-11-09 | 吉林大学 | A kind of based on α Fe2o3acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof |
| CN106966436B (en) * | 2017-04-11 | 2019-01-04 | 深圳市佩成科技有限责任公司 | It is synthesized based on microwave and carries out hollow structure Fe2O3The method of preparation |
| CN106946294A (en) * | 2017-04-11 | 2017-07-14 | 深圳市佩成科技有限责任公司 | Hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation |
| CN106966436A (en) * | 2017-04-11 | 2017-07-21 | 深圳市佩成科技有限责任公司 | Hollow structure Fe is carried out based on microwave synthesis2O3The method of preparation |
| CN106966435A (en) * | 2017-04-11 | 2017-07-21 | 深圳市佩成科技有限责任公司 | Hollow structure Fe is carried out based on oil bath synthesis2O3The method of preparation |
| CN106966435B (en) * | 2017-04-11 | 2019-01-04 | 深圳市佩成科技有限责任公司 | It is synthesized based on oil bath and carries out hollow structure Fe2O3The method of preparation |
| CN107706413A (en) * | 2017-11-08 | 2018-02-16 | 苏州宇量电池有限公司 | A kind of leaf Cyclic dart type iron oxide cathode material of nanometer three and preparation method thereof |
| CN107706413B (en) * | 2017-11-08 | 2020-08-04 | 苏州宇量电池有限公司 | Nano three-leaf boomerang type iron oxide negative electrode material and preparation method thereof |
| CN107946590A (en) * | 2017-11-09 | 2018-04-20 | 湖南友能高新技术有限公司 | A kind of pomegranate type structure di-iron trioxide and preparation method thereof and the application as lithium-ion negative pole active material |
| CN107973348A (en) * | 2017-11-28 | 2018-05-01 | 合肥学院 | A kind of spherical di-iron trioxide of micro-meter scale and preparation method thereof |
| CN108213454A (en) * | 2018-03-28 | 2018-06-29 | 燕山大学 | A kind of preparation method of the flower-shaped fe submicron particles of nano particle assembling |
| CN108213454B (en) * | 2018-03-28 | 2021-02-23 | 燕山大学 | Preparation method of flower-like elementary substance iron submicron particles assembled by nano particles |
| CN110801804A (en) * | 2019-12-09 | 2020-02-18 | 安徽建筑大学 | Metal oxide nano adsorption material with micro-nano hierarchical structure and preparation method thereof |
| CN110903490A (en) * | 2019-12-13 | 2020-03-24 | 湖南文理学院 | Novel metal organic compound semiconductor micro-nano material and preparation method and application thereof |
| CN110903490B (en) * | 2019-12-13 | 2022-06-17 | 湖南文理学院 | Metal organic compound semiconductor micro-nano material and preparation method and application thereof |
| CN114853082A (en) * | 2022-05-08 | 2022-08-05 | 西南石油大学 | Preparation method of spherical ferric oxide negative electrode material of lithium ion battery |
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Application publication date: 20120912 |