CN114939409B - CoFe (CoFe)2O4Base nano magnetic composite powder and preparation method thereof - Google Patents
CoFe (CoFe)2O4Base nano magnetic composite powder and preparation method thereof Download PDFInfo
- Publication number
- CN114939409B CN114939409B CN202210703230.9A CN202210703230A CN114939409B CN 114939409 B CN114939409 B CN 114939409B CN 202210703230 A CN202210703230 A CN 202210703230A CN 114939409 B CN114939409 B CN 114939409B
- Authority
- CN
- China
- Prior art keywords
- cofe
- nano particles
- solution
- nano
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910003321 CoFe Inorganic materials 0.000 title claims abstract description 82
- 239000000843 powder Substances 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002105 nanoparticle Substances 0.000 claims abstract description 56
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 229910052786 argon Inorganic materials 0.000 claims abstract description 13
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 230000001681 protective effect Effects 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 4
- 229910017052 cobalt Inorganic materials 0.000 abstract description 3
- 239000010941 cobalt Substances 0.000 abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 230000006698 induction Effects 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention relates to CoFe 2O4 -based nano magnetic composite powder and a preparation method thereof, belonging to the technical field of material preparation, and comprising the following steps: dissolving CoC l 2·6H2 O and FeC l 3·6H2 O in hydrochloric acid, mixing and stirring, adding KOH solution, transferring the mixture into an autoclave, filtering, washing and drying to obtain CoFe 2O4 nano particles; reducing the CoFe 2O4 nano particles to obtain CoFe 2 nano particles; and ball milling the CoFe 2O4 nano particles, the CoFe 2 nano particles and N i powder in an argon atmosphere, and annealing in an argon protective atmosphere to obtain the CoFe 2O4 -based nano magnetic composite powder. According to the technical scheme, N i powder and CoFe 2 nano particles are added into cobalt ferrite nano particles, and then a hard phase and a soft phase are dispersed in a ball milling mode, so that annealing induction exchange coupling is performed, and the composite material has a good photocatalysis effect.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to CoFe 2O4 -based nano magnetic composite powder and a preparation method thereof.
Background
The hard/soft magnetic nanocomposite is a focus of extensive research in the past decades due to its wide application in data storage, permanent magnets, energy systems and hard disk drives, and in recent years, the characteristics of magnetic materials have been remarkably improved due to the development of new technologies such as miniaturization of tissues, control of crystallographic orientations, thinning, superlattice, and the like while new materials such as amorphous, rare earth permanent magnet compounds, giant magnetostriction, giant magnetoresistance, and the like are successively discovered. These have made a great contribution to the dramatic improvement of characteristics of electronics, information products, etc., and become the motive force for new product development, and thus, magnetic materials have become important materials for supporting and promoting social development.
CoFe 2O4 is attracting attention due to its excellent magnetic properties compared to other types of ferrite magnets. It has been widely used for manufacturing various magnetic nanocomposite materials, on the other hand, coFe 2O4 as an n-type semiconductor having a narrow band gap, having a considerable photoresponse in the visible region of the spectrum, and having potential use as a semiconductor photocatalyst; however, the photocatalytic performance of CoFe 2O4 is lower than that of conventional photocatalytic materials such as TiO 2 and ZnO, and therefore modification of CoFe 2O4 is required.
Disclosure of Invention
The invention aims to provide CoFe 2O4 -based nano magnetic composite powder and a preparation method thereof, wherein non-agglomerated cobalt ferrite nano particles are synthesized by a hydrothermal method, so that the growth of particle size is controlled by time, ni powder and CoFe 2 nano particles are added into the cobalt ferrite nano particles, and a hard phase and a soft phase are dispersed in a ball milling mode so as to be annealed and induced to exchange and couple, so that the composite material has a good photocatalysis effect.
The invention aims to solve the technical problems: the CoFe 2O4 nanoparticles have poor photocatalytic performance.
The aim of the invention can be achieved by the following technical scheme:
A preparation method of CoFe 2O4 -based nano magnetic composite powder comprises the following steps:
s1, preparation of CoFe 2O4 nano particles: dissolving CoCl 2·6H2 O in a hydrochloric acid solution with the concentration of 2M to obtain a solution A, dissolving FeCl 3·6H2 O in a hydrochloric acid solution with the concentration of 2M to obtain a solution B, mixing the solution A and the solution B, stirring under nitrogen flow, adding a KOH solution with the concentration of 2M, transferring the mixture into an autoclave, heating at the temperature of 200 ℃ for 2-5h, naturally cooling to room temperature after the reaction is finished, filtering, washing with deionized water for 4-5 times, and drying to obtain CoFe 2O4 nano particles;
S2, preparing CoFe 2 nano particles: reducing the CoFe 2O4 nano particles in a tube furnace at a flow rate of H 2 of 300mL/min for 2 hours at 380 ℃ to obtain CoFe 2 nano particles;
S3, preparing CoFe 2O4 -based nano magnetic composite powder: and carrying out intermittent ball milling on the CoFe 2O4 nano particles, the CoFe 2 nano particles and the Ni powder for 2-5 hours in an argon protective atmosphere, and annealing the ball-milled powder in the argon protective atmosphere to obtain the CoFe 2O4 -based nano magnetic composite powder.
Further, in step S1, the usage ratio of CoCl 2·6H2O、FeCl3·6H2 O to KOH solution is 4-5g:9-11g:70-90mL.
Further, in the step S2, the particle size of the CoFe 2O4 nano-particles is 10.3-20.4nm.
Further, in step S3, the mass ratio of CoFe 2O4 nanoparticles, coFe 2 nanoparticles, and Ni powder is 3-5:0.6-1:0.4-1.2.
Further, the heating rate of the tube furnace was 25 ℃/min.
Further, the batch ball milling specifically comprises: after each ball milling for 1h, stop for 10min.
Further, the annealing temperature was 750℃and the annealing time was 1h.
The invention has the beneficial effects that:
According to the technical scheme, the CoFe 2O4 nano particles are synthesized by a hydrothermal method, the hydrothermal method has advantages over other types of crystal growth strategies, and the particle size of the synthesized CoFe 2O4 nano particles can be controlled by controlling the reaction time; by introducing Ni powder, the photocatalysis of the CoFe 2O4 -based nano magnetic composite powder is enhanced, and the mechanism is as follows: visible radiation causes the formation of electron and hole pairs (in the conduction and valence bands, respectively), photo-generated electrons transfer to Ni, holes remain on CoFe 2O4, photo-generated electrons on the Ni surface and conduction bands of CoFe 2O4 react with adsorbed O 2 to form O 2 - radicals, because conduction bands of CoFe 2O4 are more negative than the potential of O 2/O2 -, and furthermore, higher valence bands of CoFe 2O4 favor OH radical generation compared to the desired oxidation-reduction potential of oh·oh-, yielding these active species as strong oxidants that decompose organic substrates.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. A step of
Example 1
A preparation method of CoFe 2O4 -based nano magnetic composite powder comprises the following steps:
s1, dissolving 4gCoCl 2·6H2 O in 10mL of hydrochloric acid solution with the concentration of 2M to obtain solution A, dissolving 9gFeCl 3·6H2 O in 40mL of hydrochloric acid solution with the concentration of 2M to obtain solution B, mixing the solution A and the solution B, stirring under nitrogen flow, adding 70mL of KOH solution with the concentration of 2M, transferring the mixture into an autoclave, heating at the temperature of 200 ℃ for 2h, naturally cooling to room temperature after the reaction is finished, filtering, washing with deionized water for 4 times, and drying to obtain CoFe 2O4 nano particles;
S2, reducing CoFe 2O4 nano particles with the particle size of 10.3nm in a tube furnace at the H 2 flow rate of 300mL/min for 2 hours at 380 ℃ at the heating rate of 25 ℃/min to obtain CoFe 2 nano particles;
S3, carrying out intermittent ball milling on the 3gCoFe 2O4 nano particles, the 0.6gCoFe 2 nano particles and the 0.4gNi powder for 2 hours in an argon protective atmosphere, stopping 10 minutes after each ball milling for 1 hour, and annealing the ball-milled powder for 1 hour at 750 ℃ in the argon protective atmosphere to obtain the CoFe 2O4 -based nano magnetic composite powder.
Example 2
A preparation method of CoFe 2O4 -based nano magnetic composite powder comprises the following steps:
S1, dissolving 4.5g of CoCl 2·6H2 O in 10mL of hydrochloric acid solution with the concentration of 2M to obtain solution A, dissolving 10g of FeCl 3·6H2 O in 40mL of hydrochloric acid solution with the concentration of 2M to obtain solution B, mixing the solution A and the solution B, stirring under nitrogen flow, adding 70mL of KOH solution with the concentration of 2M, transferring the mixture into an autoclave, heating at the temperature of 200 ℃ for 3h, naturally cooling to room temperature after the reaction is finished, filtering, washing with deionized water for 5 times, and drying to obtain CoFe 2O4 nano particles;
S2, reducing CoFe 2O4 nano particles with the particle size of 15nm in a tube furnace at the H 2 flow rate of 300mL/min for 2 hours at 380 ℃ at the heating rate of 25 ℃/min to obtain CoFe 2 nano particles;
S3, performing intermediate ball milling on 4g of CoFe 2O4 nano particles, 0.8gCoFe 2 nano particles and 0.8gNi powder for 2h in an argon protective atmosphere, stopping 10min after each ball milling for 1h, and annealing the ball-milled powder for 1h at 750 ℃ in the argon protective atmosphere to obtain the CoFe 2O4 -based nano magnetic composite powder.
Example 3
A preparation method of CoFe 2O4 -based nano magnetic composite powder comprises the following steps:
S1, dissolving 5gCoCl 2·6H2 O in 10mL of hydrochloric acid solution with the concentration of 2M to obtain solution A, dissolving 11g of FeCl 3·6H2 O in 40mL of hydrochloric acid solution with the concentration of 2M to obtain solution B, mixing the solution A and the solution B, stirring under nitrogen flow, adding 70mL of KOH solution with the concentration of 2M, transferring the mixture into an autoclave, heating at the temperature of 200 ℃ for 4 hours, naturally cooling to room temperature after the reaction is finished, filtering, washing with deionized water for 5 times, and drying to obtain CoFe 2O4 nano particles;
S2, reducing CoFe 2O4 nano particles with the particle size of 20nm in a tube furnace at the H 2 flow rate of 300mL/min for 2 hours at 380 ℃ at the heating rate of 25 ℃/min to obtain CoFe 2 nano particles;
S3, performing intermediate ball milling on 5g of CoFe 2O4 nano particles, 1g of CoFe 2 nano particles and 1.2g of Ni powder in an argon protective atmosphere for 2h, stopping 10min after each ball milling for 1h, and annealing the ball-milled powder in the argon protective atmosphere at 750 ℃ for 1h to obtain the CoFe 2O4 -based nano magnetic composite powder.
In examples 1 to 3, the average crystal size D X, the average nanoparticle diameter D T, the saturation magnetization Ms and the coercivity Hc of the CoFe 2O4 -based nano-magnetic composite powders synthesized at different reaction times t are shown in table 1 below:
TABLE 1
| Project | t(h) | DX(nm) | DT(nm) | Ms(Am2/kg) | Hc(kA/m) |
| Example 1 | 2 | 10.3 | 21.6 | 68.6 | 119.3 |
| Example 2 | 4 | 15.6 | 24.8 | 71.1 | 117.5 |
| Example 3 | 6 | 20.4 | 27.5 | 71.9 | 143.7 |
As can be seen from the table 1, the technical scheme of the invention realizes stable rise of the magnetization Ms and the coercive force Hc of the CoFe 2O4 -based nano magnetic composite powder by controlling different reaction times t.
Example 4
A preparation method of CoFe 2O4 -based nano magnetic composite powder comprises the following steps:
s1, dissolving 5g of CoCl 2·6H2 O in 10mL of hydrochloric acid solution with the concentration of 2M to obtain solution A, dissolving 11g of FeCl 3·6H2 O in 40mL of hydrochloric acid solution with the concentration of 2M to obtain solution B, mixing the solution A and the solution B, stirring under nitrogen flow, adding 70mL of KOH solution with the concentration of 2M, transferring the mixture into an autoclave, heating at the temperature of 200 ℃ for 4h, naturally cooling to room temperature after the reaction is finished, filtering, washing with deionized water for 5 times, and drying to obtain CoFe 2O4 nano particles;
S2, reducing CoFe 2O4 nano particles with the particle size of 20nm in a tube furnace at the H 2 flow rate of 300mL/min for 2 hours at 380 ℃ at the heating rate of 25 ℃/min to obtain CoFe 2 nano particles;
S3, performing intermediate ball milling on 5g of CoFe 2O4 nano particles, 1g of CoFe 2 nano particles and 1.2g of Ni powder for 3 hours in an argon protective atmosphere, stopping 10 minutes after each ball milling for 1 hour, and annealing the ball-milled powder for 1 hour at 750 ℃ in the argon protective atmosphere to obtain the CoFe 2O4 -based nano magnetic composite powder.
Example 5
This example differs from example 4 in that batch ball milling was replaced with batch ball milling for 3 hours, and the remaining steps and starting materials were the same.
Example 6
This example differs from example 4 in that batch ball milling was replaced with batch ball milling for 3 hours, 5 hours, and the remaining steps and raw materials were the same.
The degradation rate experiments of the CoFe 2O4 -based nano magnetic composite powder prepared in examples 4-6 show that the irradiation time is 90min, the catalyst dosage is 0.4g/L and the initial dye concentration is 5ppm, and the test results are shown in the following table 2.
TABLE 2
| Project | Final dye concentration (ppm) | Degradation rate (%) |
| Example 4 | 1.04 | 79.2 |
| Example 5 | 0.97 | 80.6 |
| Example 6 | 0.825 | 83.5 |
As can be seen from the table 2, the technical scheme of the invention realizes the increase of the degradation rate of the CoFe 2O4 -based nano magnetic composite powder from 79.2% to 83.5% by controlling the ball milling time of the CoFe 2O4 nano particles, the CoFe 2 nano particles and the Ni powder, and has good photodegradation catalysis effect on dye.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (2)
1. A preparation method of CoFe 2O4 -based nano magnetic composite powder is characterized by comprising the following steps: the method comprises the following steps:
S1, preparation of CoFe 2O4 nano particles: dissolving CoCl 2·6H2 O in a hydrochloric acid solution with the concentration of 2M to obtain a solution A, dissolving FeCl 3·6H2 O in a hydrochloric acid solution with the concentration of 2M to obtain a solution B, mixing the solution A and the solution B, stirring under nitrogen flow, adding a KOH solution with the concentration of 2M, transferring the mixture into an autoclave, heating at the temperature of 200 ℃ for 2-5h, naturally cooling to room temperature after the reaction is finished, filtering, washing with deionized water for 4-5 times, and drying to obtain CoFe 2O4 nano particles;
S2, preparing CoFe 2 nano particles: reducing the CoFe 2O4 nano particles in a tube furnace at a flow rate of H 2 of 300mL/min for 2 hours at 380 ℃ to obtain CoFe 2 nano particles;
S3, preparing CoFe 2O4 -based nano magnetic composite powder: intermittently ball-milling the CoFe 2O4 nano particles, the CoFe 2 nano particles and Ni powder for 2-5 hours in an argon protective atmosphere, and annealing the ball-milled powder in the argon protective atmosphere to obtain the CoFe 2O4 -based nano magnetic composite powder;
in the step S1, the dosage ratio of the CoCl 2·6H2O、FeCl 3·6H2 O to the KOH solution is 4-5g:9-11g:70-90mL;
In the step S2, the particle size of the CoFe 2O4 nano particles is 10.3-20.4nm;
In the step S3, the mass ratio of the CoFe 2O4 nano particles to the CoFe 2 nano particles to the Ni powder is 3-5:0.6-1:0.4-1.2;
the heating rate of the tube furnace is 25 ℃/min;
the batch ball milling is specifically as follows: stopping for 10min after ball milling for 1 h;
The annealing temperature was 750℃and the annealing time was 1h.
2. A CoFe 2O4 -based nano-magnetic composite powder produced by the production method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210703230.9A CN114939409B (en) | 2022-06-21 | 2022-06-21 | CoFe (CoFe)2O4Base nano magnetic composite powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210703230.9A CN114939409B (en) | 2022-06-21 | 2022-06-21 | CoFe (CoFe)2O4Base nano magnetic composite powder and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114939409A CN114939409A (en) | 2022-08-26 |
| CN114939409B true CN114939409B (en) | 2024-05-31 |
Family
ID=82910637
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210703230.9A Active CN114939409B (en) | 2022-06-21 | 2022-06-21 | CoFe (CoFe)2O4Base nano magnetic composite powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114939409B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115612583B (en) * | 2022-09-26 | 2023-10-03 | 重庆大学 | Fermentation process for producing fat and ethanol by reinforcing saccharomyces cerevisiae by nano particles |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105214674A (en) * | 2015-09-17 | 2016-01-06 | 淮南师范学院 | Nano Co Fe 1.95y 0.05o 4the preparation of powder and the method for catalytic degradation methyl orange |
| CN105855539A (en) * | 2016-04-13 | 2016-08-17 | 安徽大学 | Construction method for nanostructures provided with CoFe2 cores and CoFe2O4 shells and applied to photocatalysis field |
| CN114446673A (en) * | 2022-01-14 | 2022-05-06 | 河北工业大学 | Three-dimensional net-shaped thin-sheet CoFe2O4@ NiO composite material, preparation method and application |
-
2022
- 2022-06-21 CN CN202210703230.9A patent/CN114939409B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105214674A (en) * | 2015-09-17 | 2016-01-06 | 淮南师范学院 | Nano Co Fe 1.95y 0.05o 4the preparation of powder and the method for catalytic degradation methyl orange |
| CN105855539A (en) * | 2016-04-13 | 2016-08-17 | 安徽大学 | Construction method for nanostructures provided with CoFe2 cores and CoFe2O4 shells and applied to photocatalysis field |
| CN114446673A (en) * | 2022-01-14 | 2022-05-06 | 河北工业大学 | Three-dimensional net-shaped thin-sheet CoFe2O4@ NiO composite material, preparation method and application |
Non-Patent Citations (3)
| Title |
|---|
| CoFe_2与CoFe_2O_4质量比及MgO稀释对CoFe_2@CoFe_2O_4磁性的影响;马永青;刘畅;王敏;;复合材料学报(04);全文 * |
| 二氧化钛/铁酸钴磁性光催化材料的制备及表征;孙东峰;宋明;韩一丹;张秀玲;;无机盐工业(10);全文 * |
| 硬磁CoFe_2O_4/软磁CoFe_2复合物的磁性研究;马永青;黄松;徐士涛;;安徽大学学报(自然科学版)(01);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114939409A (en) | 2022-08-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102909381B (en) | Method for preparing high coercive force manganese-bismuth magnetic powder by doping cobalt nano-particles | |
| CN103123837B (en) | alcoholic solution and sintered magnet | |
| Esmaili et al. | The effect of Nd and Zr co-substitution on structural, magnetic and photocatalytic properties of Bi1-xNdxFe1-xZrxO3 nanoparticles | |
| CN114939409B (en) | CoFe (CoFe)2O4Base nano magnetic composite powder and preparation method thereof | |
| Khorasanizadeh et al. | Ultrasound-accelerated synthesis of uniform DyVO4 nanoparticles as high activity visible-light-driven photocatalyst | |
| EP3319093B1 (en) | Method of synthesising a magnetic material | |
| Mohseni et al. | Enhancement of maximum energy product in exchange-coupled BaFe12O19/Fe3O4 core-shell-like nanocomposites | |
| JP2010189679A (en) | Method for producing iron-cobalt alloy nanoparticle, and iron-cobalt alloy nanoparticle | |
| CN102139375A (en) | Method for preparing micron-size superfine iron powder | |
| Zheng et al. | Controllable synthesis of monodispersed iron oxide nanoparticles by an oxidation-precipitation combined with solvothermal process | |
| Jangam et al. | Effect of cobalt substitution in Zn1-xCoxFeCrO4 ferri-chromate: emerging light absorber for degradation of model textile dye | |
| CN104985194B (en) | A kind of preparation method at oxide dispersion intensifying iron cobalt nano composite powder end | |
| CN106861697A (en) | New class fenton catalyst that a kind of ferroferric oxide nano granules are combined with silicon oxide nanofiber and preparation method thereof | |
| Mahdikhah et al. | Magnetic and photocatalytic properties of CoFe 2 O 4/Ni nanocomposites | |
| Wang et al. | Nd2Fe14B hard magnetic powders: Chemical synthesis and mechanism of coercivity | |
| CN108435179B (en) | Preparation method of double-activity monatomic ammonia synthesis catalyst | |
| CN114524463B (en) | Super-large-size high-length-diameter-ratio ferroferric oxide two-dimensional nano sheet and preparation method thereof | |
| Dong et al. | Synthesis and photocatalytic activity of Fe 3 O 4–WO 3–CQD multifunctional system | |
| CN1320176C (en) | Magnetic modified nanometer zinc oxide whiskers and production thereof | |
| JP2011207731A (en) | Ferrite particle and method for manufacturing the same | |
| Dhanalakshmi et al. | Synergistic magnetic field-photocatalysis for the concurrent removal of inorganic and organic contaminants over PrFeO3/ZnO heterostructures | |
| Zhang et al. | Synthesis of novel Mn 3 O 4 concave octahedral microcrystals and their anomalous magnetic properties | |
| CN114602518A (en) | Self-assembled three-dimensional BiOI/BaFe12O19Magnetic photocatalyst and preparation method and application thereof | |
| CN107364896A (en) | A kind of good and inexpensive strontium ferrite raw powder's production technology of magnetic property | |
| KR20110043181A (en) | The method for preparation of monodisperse iron oxide nanoparticles using electron beam irradiation and monodisperse iron oxide nanoparticles thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |