CN107265414A - A kind of preparation method for heterogeneous nano chain of destroying first and then establish - Google Patents
A kind of preparation method for heterogeneous nano chain of destroying first and then establish Download PDFInfo
- Publication number
- CN107265414A CN107265414A CN201710383681.8A CN201710383681A CN107265414A CN 107265414 A CN107265414 A CN 107265414A CN 201710383681 A CN201710383681 A CN 201710383681A CN 107265414 A CN107265414 A CN 107265414A
- Authority
- CN
- China
- Prior art keywords
- conditional
- magnetic field
- electrolyte
- range
- power supply
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
Abstract
The invention discloses a kind of preparation method for heterogeneous nano chain of destroying first and then establish, the heterogeneous nano chain is Fe N/Fe3O4Heterogeneous nano chain, can be prepared from by Fe-N Alloyses particle by the method for electrochemical oxidation.By changing voltage, time, the species of electrolyte and temperature, the pH value of electrochemical reaction, the magnetic field size of application etc., regulation and control Fe N/Fe3O4Length, width, the ratio and dispersiveness of two-phase of heterogeneous nano chain.Oxidation voltage can be the V of 30 V ~ 50；Electrolyte temperature is from room temperature to 60 °C；PH value range is from 2 to 0.3；The time of electrochemical oxidation reactions was from 50 minutes to 80 minutes；Externally-applied magnetic field is more than 0.2 T.This preparation method does not need template, it is not necessary to any organic additive, and reaction condition is gentle, and magnetic field intensity can easily be accommodated, and preparation process is simple and environment-friendly, and the heterogeneous nano chain of surface cleaning can be made.
Description
Technical field
The present invention relates to heterogeneous nano chain preparation method field, specifically a kind of preparation for heterogeneous nano chain of destroying first and then establish
Method.
Background technology
In recent years, ordered nano-structure magnetic material is received more and more due to its property and potential application
Concern.1-dimention nano magnetic material is used as a member in nanostructured magnetic material extended familys, wherein nano chain or chain structure
(including nanotube and nano wire) has also attracted many concerns because of its novel optical, electromagnetic performance etc. and with potential application.Thing
In reality, in numerous applications, such as in the application for being related to electrical communications and magnetic switch, the sequence of nano particle plays crucial make
With.Magnetic chain-like nanometer structure is also manufacture electronic device, Magnetic Sensor, catalyst, ultracapacitor, microwave absorption material simultaneously
The important component of material and battery.
Constructing based on chain-like nanometer structure, has developed various methods, including the use of sol-gel process, template
Method and chemical reduction method etc..In the above-mentioned methods, due to its control growth and the diversity of form, templated synthesis is that synthesis is received
Rice chain most common method.But, template is complicated because of synthesis, and cost is high, yields poorly, and limits its application, and finally
Template is dissolved with etchant solution and removed, therefore, the nano chain obtained is difficult the surface with cleaning.Chemical reduction method leads to
Cross and various complexing agents and organic solvent added during liquid phase reactor, introduce new foreign ion, final process when
Time is very difficult to except clean.Another adds the method for induced by magnetic field to be to prepare one-dimensional magnetic linkage or line in hydrothermal reaction process
A kind of effective means, but this method is induced for hydro-thermal reaction externally-applied magnetic field, magnet is placed in reactor, with reaction solution
Body is contacted, and magnet corrosion-vulnerable is simultaneously polluted to reactant；Environment temperature is high, and the intensity of magnetization of magnet can reduce；Due to anti-
Kettle inner space is answered to limit, regulation magnitude of field intensity is inconvenient.
Based on above-mentioned consideration, exploitation is a kind of to have that preparation technology is simple, reaction condition can easily be accommodated, cheap, simultaneously
The method that the synthesis nano chain of clean surface can be obtained is significant.
The content of the invention
It is different to solve prior art it is an object of the invention to provide a kind of preparation method for heterogeneous nano chain of destroying first and then establish
The problem of matter nano chain preparation method is difficult to adjust, pollutes larger.
In order to achieve the above object, the technical solution adopted in the present invention is：
A kind of preparation method for heterogeneous nano chain of destroying first and then establish, it is characterised in that：Comprise the following steps successively：
(1) electrolyte used in electrochemistry experiment, is prepared：
Acid solution is configured, using this acid solution as the electrolyte of electrochemical reaction, the concentration of acid solution is
Any one concentration value in the range of 0.01mol/L~0.3mol/L；
(2) electrolytic cell, is prepared：
Measure and account for the electrolyte of the volume of electrolytic cell 4/5 and pour into electrolytic cell, then weigh the Fe particles by nitrogen treatment
Pour into glass tube, the amount that Fe particles are weighed can fill up glass tube, the mouth of pipe of glass tube is stifled with the rubber stopper punched
On；Glass tube is put into electrolytic cell again, it is ensured that electrolyte submerges glass tube；It is finally that platinized platinum and platinum filament insertion is punched
Rubber stopper on, wherein platinum filament one end insertion glass tube in by nitrogen treatment Fe particles in, platinized platinum be in glass tubule
It is not in contact outside with Fe particles, using platinized platinum as the negative electrode of connection power supply, the positive electrode of connection power supply is used as using platinum filament；
(3) externally-applied magnetic field, is prepared：
Permanent magnet is placed respectively in two symmetrical sides of the inner electrolytic cell of step (2), and both sides permanent magnet magnetism is attracting, by two
Side permanent magnet forms the magnetic field that magnetic field intensity is more than 0.2T into electrolytic cell；
(4) electrochemical treatments, are carried out to the Fe particles in glass tube by nitrogen treatment：
The electrolytic cell that step (3) is applied with into magnetic field is integrally put into water-bath together with glass tube therein, by water-bath
Isoperibol is provided, the temperature value of isoperibol is any one temperature value of room temperature~70 DEG C；Then using DC stabilization electricity
Source is connected with the electrode on glass tube rubber stopper, and the positive pole of wherein DC stable power supply is connected with platinum filament, DC stable power supply
Negative pole is connected with platinized platinum, provides a burning voltage into glass tube from DC stable power supply, to passing through in glass tube at nitridation
The Fe particles of reason carry out electrochemical treatments, and the stable voltage is 20V~60V any one magnitude of voltage；Electrochemical treatments one
DC stable power supply is closed after the section time, the electrochemical treatments time is 40mins~90mins any one time value；
(5), using the concentration of acid solution in step (1) as condition one, the magnetic field intensity applied using in step (3) is bar
Part two, using the temperature value of isoperibol in step (4) as condition three, the stable electricity provided with DC stable power supply in step (4)
Pressure value is as condition four, using the electrochemical treatments time in step (4) as condition five, by repeat step (1), (2), (3),
(4) and change condition one, two, three, four, five, several samples are made, by all samples washes of absolute alcohol 2~5 times, then
Each sample is put into vacuum drying chamber again after upper strata absolute ethyl alcohol is poured out, in vacuum drying chamber using vacuum as-
0.05~-0.15, temperature is dry 5~7 hours under conditions of 40 DEG C~60 DEG C, obtains Fe-N/Fe3O4Heterogeneous nano chain.
A kind of preparation method of described heterogeneous nano chain of destroying first and then establish, it is characterised in that：The electricity of step (1) conditional one
It is 0.01mol/L to solve the selection of liquid concentration, and the magnetic field intensity that step (3) conditional two applies is the stationary magnetic field more than 0.2T, step
Suddenly the temperature value of the isoperibol of (4) conditional three is 60 DEG C, the stable electricity that the DC stable power supply of step (4) conditional four is provided
Pressure value is 30V, and the electrochemical treatments time of step (4) conditional five is 80mins, and sample 0.01mol30V80M is made；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
DC stable power supply provide stable voltage be 30V, the electrochemical treatments time of step (4) conditional five be 50mins~
Any one time value in 70mins, is made sample 0.01mol30V50M~80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is any one magnitude of voltage in the range of 30V~50V, step (4) conditional five
The electrochemical treatments time is any one time value in the range of 50mins~80mins, obtained sample 0.01mol30V~
50V50M~80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is appointing in the range of room temperature~60 DEG C
One temperature value of meaning, the stable voltage that the DC stable power supply of step (4) conditional four is provided is appointing in the range of 30V~50V
One magnitude of voltage of meaning, when the electrochemical treatments time of step (4) conditional five is any one in the range of 50mins~80mins
Between be worth, sample 0.01mol30V~50V50M~80M27~60 DEG C are made；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, changes the magnetic that step (3) conditional two applies
Field intensity, but still magnetic field intensity is more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is room temperature~60 DEG C model
Any one interior temperature value is enclosed, the stable voltage that the DC stable power supply of step (4) conditional four is provided is 30V~50V models
Any one interior magnitude of voltage is enclosed, the electrochemical treatments time of step (4) conditional five is appointing in the range of 50mins~80mins
One time value of meaning, is made sample 0.01mol30V~50V50M~80M27~60 DEG C >=0.2T.
A kind of preparation method of described heterogeneous nano chain of destroying first and then establish, it is characterised in that：The electricity of step (1) conditional one
It is 0.1mol/L to solve the selection of liquid concentration, and the magnetic field intensity that step (3) conditional two applies is the stationary magnetic field more than 0.2 T, step
Suddenly the temperature value of the isoperibol of (4) conditional three is 60 DEG C, the stable electricity that the DC stable power supply of step (4) conditional four is provided
Pressure value is 40V, and the electrochemical treatments time of step (4) conditional five is 80mins, and sample 0.1mol40V80M is made；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
DC stable power supply provide stable voltage be 40V, the electrochemical treatments time of step (4) conditional five be 50mins~
Any one time value in 70mins, is made sample 0.1mol40V50M~70M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is any one magnitude of voltage in the range of 30V~50V, step (4) conditional five
The electrochemical treatments time is any one time value in the range of 50mins~80mins, obtained sample 0.1mol30V~
50V50M~80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is appointing in the range of room temperature~60 DEG C
One temperature value of meaning, the stable voltage that the DC stable power supply of step (4) conditional four is provided is appointing in the range of 30V~50V
One magnitude of voltage of meaning, when the electrochemical treatments time of step (4) conditional five is any one in the range of 50mins~80mins
Between be worth, sample 0.1mol30V~50V50M~80M27~60 DEG C are made；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, changes the magnetic that step (3) conditional two applies
Field intensity, but still magnetic field intensity is more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is room temperature~60 DEG C model
Any one interior temperature value is enclosed, the stable voltage that the DC stable power supply of step (4) conditional four is provided is 30V~50V models
Any one interior magnitude of voltage is enclosed, the electrochemical treatments time of step (4) conditional five is appointing in the range of 50mins~80mins
One time value of meaning, is made sample 0.1mol30V~50V50M~80M27~60 DEG C >=0.2T.
A kind of preparation method of described heterogeneous nano chain of destroying first and then establish, it is characterised in that：The electricity of step (1) conditional one
It is 0.3mol/L to solve the selection of liquid concentration, and the magnetic field intensity that step (3) conditional two applies is the stationary magnetic field more than 0.2 T, step
Suddenly the temperature value of the isoperibol of (4) conditional three is 60 DEG C, the stable electricity that the DC stable power supply of step (4) conditional four is provided
Pressure value is 50V, and the electrochemical treatments time of step (4) conditional five is 80mins, and sample 0.3mol50V80M is made；
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
DC stable power supply provide stable voltage be 50V, the electrochemical treatments time of step (4) conditional five be 50mins~
Any one time value in the range of 70mins, is made sample 0.3mol50V50M~70M.
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is any one magnitude of voltage in the range of 30V~50V, step (4) conditional five
The electrochemical treatments time is any one time value in the range of 50mins~80mins, obtained sample 0.3mol30V~
50V50M~80M.
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is appointing in the range of room temperature~60 DEG C
One temperature value of meaning, the stable voltage that the DC stable power supply of step (4) conditional four is provided is appointing in the range of 30V~50V
One magnitude of voltage of meaning, when the electrochemical treatments time of step (4) conditional five is any one in the range of 50mins~80mins
Between be worth, sample 0.3mol30V~50V50M~80M27~60 DEG C are made.
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, changes the magnetic that step (3) conditional two applies
Field intensity, but still magnetic field intensity is more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is room temperature~60 DEG C model
Any one interior temperature value is enclosed, the stable voltage that the DC stable power supply of step (4) conditional four is provided is 30V~50V models
Any one interior magnitude of voltage is enclosed, the electrochemical treatments time of step (4) conditional five is appointing in the range of 50mins~80mins
One time value of meaning, is made sample 0.1mol30V~50V50M~80M27~60 DEG C >=0.2T.
A kind of preparation method of described heterogeneous nano chain of destroying first and then establish, it is characterised in that：In step (5), vacuum drying
Vacuum is preferably preferably 50 DEG C of -0.1, temperature, preferably 6 hours drying time in case.
In the present invention, the species of acid solution can select suitable species according to actual needs.
, can be by fe under NH3 atmosphere by the Fe particulate materials of nitrogen treatment in the present invention, annealing temperature 280
~500 DEG C, 2~10h of annealing is made.
Present invention partial nitridation in ammonia environment by Fe nano-particles, forms Fe and Fe-N complex particles；Then will
In the electrolyte that this complex particle is immersed in homemade electrochemical cell, Pt wire anodes insertion particle；Negative electrode is used as with Pt pieces
(as shown in Figure 1).In appropriate Arrays Aluminum Films in Acid Solution and temperature, anodic oxidation voltage and appropriate electrolyte ph, appropriate is outer
Plus can be made into Fe-N/Fe under the conditions of magnetic field etc.3O4Heterogeneous nano chain.
Preparation method of the present invention does not need template, it is not necessary to any organic additive, and reaction condition is gentle, magnetic field intensity
It can easily be accommodated, preparation process is simple and environment-friendly, the heterogeneous nano chain of surface cleaning can be made.
Brief description of the drawings
Fig. 1 is the schematic diagram of electrochemistry apparatus for preparation.
Fig. 2 is the iron-based nitrogen-containing alloy (Fe after fe (Fe) ammonia is annealed2N) the X-ray diffracting spectrum of sample.Its
In, abscissa is the angle of diffraction, and ordinate is relative intensity.
Fig. 3 (a) is the Fe particles by nitrogen treatment in 0.3mol/L electrolyte, 6O DEG C of reaction temperature, reaction time
The X-ray diffraction for the sample (30V, 40V, 50V) that 80mins is obtained after series voltage (30,40,50V) electrochemical reaction
Collection of illustrative plates and Fe2N standard PDF cards (No.72-2126) and Fe3O4Standard PDF cards (No.77-1545).
Fig. 3 (b) is the Fe particles by nitrogen treatment in response voltage 50V, 6O DEG C of reaction temperature, reaction time
Obtained in electrolyte (0.01,0.1,0.3mol/L) of the 80mins by series concentration after electrochemical reaction sample (0.01,
0.1st, 0.3mol/L) X-ray diffracting spectrum and Fe2N standard PDF cards (No.72-2126) and Fe3O4Standard
PDF cards (No.77-1545).
Fig. 4 (a) is the Fe particles by nitrogen treatment in 0.3mol/L electrolyte, 6O DEG C of reaction temperature, reaction time
80mins response voltages 50V TEM figures.
Fig. 4 (b) is the Fe particles by nitrogen treatment in 0.3mol/L electrolyte, 6O DEG C of reaction temperature, reaction time
80mins response voltages 50V SEM figures
Fig. 5 is the Fe particles by nitrogen treatment in 0.1mol/L electrolyte, 6O DEG C of reaction temperature, reaction time 80mins
Response voltage 40V TEM figures.
Fig. 6 is the Fe particles by nitrogen treatment in 0.01mol/L electrolyte, 6O DEG C of reaction temperature, reaction time
80mins response voltages 30V TEM figures.
Embodiment
A kind of preparation method for heterogeneous nano chain of destroying first and then establish, comprises the following steps successively：
(1) electrolyte used in electrochemistry experiment, is prepared：
Acid solution is configured, using this acid solution as the electrolyte of electrochemical reaction, the concentration of acid solution is
Any one concentration value in the range of 0.01mol/L~0.3mol/L；
(2) electrolytic cell, is prepared：
Measure and account for the electrolyte of the volume of electrolytic cell 4/5 and pour into electrolytic cell, then weigh the Fe particles by nitrogen treatment
Pour into glass tube, the amount that Fe particles are weighed can fill up glass tube, the mouth of pipe of glass tube is stifled with the rubber stopper punched
On；Glass tube is put into electrolytic cell again, it is ensured that electrolyte submerges glass tube；It is finally that platinized platinum and platinum filament insertion is punched
Rubber stopper on, wherein platinum filament one end insertion glass tube in by nitrogen treatment Fe particles in, platinized platinum be in glass tubule
It is not in contact outside with Fe particles, using platinized platinum as the negative electrode of connection power supply, the positive electrode of connection power supply is used as using platinum filament；
(3) externally-applied magnetic field, is prepared：
Permanent magnet is placed respectively in two symmetrical sides of the inner electrolytic cell of step (2), and both sides permanent magnet magnetism is attracting, by two
Side permanent magnet forms the magnetic field that magnetic field intensity is more than 0.2T into electrolytic cell；
(4) electrochemical treatments, are carried out to the Fe particles in glass tube by nitrogen treatment：
The electrolytic cell that step (3) is applied with into magnetic field is integrally put into water-bath together with glass tube therein, by water-bath
Isoperibol is provided, the temperature value of isoperibol is any one temperature value of room temperature~70 DEG C；Then using DC stabilization electricity
Source is connected with the electrode on glass tube rubber stopper, and the positive pole of wherein DC stable power supply is connected with platinum filament, DC stable power supply
Negative pole is connected with platinized platinum, provides a burning voltage into glass tube from DC stable power supply, to passing through in glass tube at nitridation
The Fe particles of reason carry out electrochemical treatments, and the stable voltage is 20V~60V any one magnitude of voltage；Electrochemical treatments one
DC stable power supply is closed after the section time, the electrochemical treatments time is 40mins~90mins any one time value；
(5), using the concentration of acid solution in step (1) as condition one, the magnetic field intensity applied using in step (3) is bar
Part two, using the temperature value of isoperibol in step (4) as condition three, the stable electricity provided with DC stable power supply in step (4)
Pressure value is as condition four, using the electrochemical treatments time in step (4) as condition five, by repeat step (1), (2), (3),
(4) and change condition one, two, three, four, five, several samples are made, by all samples washes of absolute alcohol 2~5 times, then
Each sample is put into vacuum drying chamber again after upper strata absolute ethyl alcohol is poured out, in vacuum drying chamber using vacuum as-
0.05~-0.15, temperature is dry 5~7 hours under conditions of 40 DEG C~60 DEG C, obtains Fe-N/Fe3O4Heterogeneous nano chain.
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is 30V, and the electrochemical treatments time of step (4) conditional five is 80mins, is made
Sample 0.01mol30V80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
DC stable power supply provide stable voltage be 30V, the electrochemical treatments time of step (4) conditional five be 50mins~
Any one time value in 70mins, is made sample 0.01mol30V50M~80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is any one magnitude of voltage in the range of 30V~50V, step (4) conditional five
The electrochemical treatments time is any one time value in the range of 50mins~80mins, obtained sample 0.01mol30V~
50V50M~80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is appointing in the range of room temperature~60 DEG C
One temperature value of meaning, the stable voltage that the DC stable power supply of step (4) conditional four is provided is appointing in the range of 30V~50V
One magnitude of voltage of meaning, when the electrochemical treatments time of step (4) conditional five is any one in the range of 50mins~80mins
Between be worth, sample 0.01mol30V~50V50M~80M27~60 DEG C are made；
The selection of the concentration of electrolyte of step (1) conditional one is 0.01mol/L, changes the magnetic that step (3) conditional two applies
Field intensity, but still magnetic field intensity is more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is room temperature~60 DEG C model
Any one interior temperature value is enclosed, the stable voltage that the DC stable power supply of step (4) conditional four is provided is 30V~50V models
Any one interior magnitude of voltage is enclosed, the electrochemical treatments time of step (4) conditional five is appointing in the range of 50mins~80mins
One time value of meaning, is made sample 0.01mol30V~50V50M~80M27~60 DEG C >=0.2T.
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is 40V, and the electrochemical treatments time of step (4) conditional five is 80mins, is made
Sample 0.1mol40V80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
DC stable power supply provide stable voltage be 40V, the electrochemical treatments time of step (4) conditional five be 50mins~
Any one time value in 70mins, is made sample 0.1mol40V50M~70M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is any one magnitude of voltage in the range of 30V~50V, step (4) conditional five
The electrochemical treatments time is any one time value in the range of 50mins~80mins, obtained sample 0.1mol30V~
50V50M~80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is appointing in the range of room temperature~60 DEG C
One temperature value of meaning, the stable voltage that the DC stable power supply of step (4) conditional four is provided is appointing in the range of 30V~50V
One magnitude of voltage of meaning, when the electrochemical treatments time of step (4) conditional five is any one in the range of 50mins~80mins
Between be worth, sample 0.1mol30V~50V50M~80M27~60 DEG C are made；
The selection of the concentration of electrolyte of step (1) conditional one is 0.1mol/L, changes the magnetic that step (3) conditional two applies
Field intensity, but still magnetic field intensity is more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is room temperature~60 DEG C model
Any one interior temperature value is enclosed, the stable voltage that the DC stable power supply of step (4) conditional four is provided is 30V~50V models
Any one interior magnitude of voltage is enclosed, the electrochemical treatments time of step (4) conditional five is appointing in the range of 50mins~80mins
One time value of meaning, is made sample 0.1mol30V~50V50M~80M27~60 DEG C >=0.2T.
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is 50V, and the electrochemical treatments time of step (4) conditional five is 80mins, is made
Sample 0.3mol50V80M；
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
DC stable power supply provide stable voltage be 50V, the electrochemical treatments time of step (4) conditional five be 50mins~
Any one time value in the range of 70mins, is made sample 0.3mol50V50M~70M.
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is 60 DEG C, step (4) conditional four
The stable voltage that DC stable power supply is provided is any one magnitude of voltage in the range of 30V~50V, step (4) conditional five
The electrochemical treatments time is any one time value in the range of 50mins~80mins, obtained sample 0.3mol30V~
50V50M~80M.
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, and the magnetic field that step (3) conditional two applies is strong
Spend for the stationary magnetic field more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is appointing in the range of room temperature~60 DEG C
One temperature value of meaning, the stable voltage that the DC stable power supply of step (4) conditional four is provided is appointing in the range of 30V~50V
One magnitude of voltage of meaning, when the electrochemical treatments time of step (4) conditional five is any one in the range of 50mins~80mins
Between be worth, sample 0.3mol30V~50V50M~80M27~60 DEG C are made.
The selection of the concentration of electrolyte of step (1) conditional one is 0.3mol/L, changes the magnetic that step (3) conditional two applies
Field intensity, but still magnetic field intensity is more than 0.2T, the temperature value of the isoperibol of step (4) conditional three is room temperature~60 DEG C model
Any one interior temperature value is enclosed, the stable voltage that the DC stable power supply of step (4) conditional four is provided is 30V~50V models
Any one interior magnitude of voltage is enclosed, the electrochemical treatments time of step (4) conditional five is appointing in the range of 50mins~80mins
One time value of meaning, is made sample 0.1mol30V~50V50M~80M27~60 DEG C >=0.2T.
In step (5), vacuum is preferably preferably 50 DEG C of -0.1, temperature in vacuum drying chamber, and drying time preferably 6 is small
When.
Embodiment 1：Fe-N/Fe3O4The preparation of heterogeneous nano chain
(1) electrolyte used in electrochemistry experiment is prepared：
Electrolyte is to measure the hydrochloric acid solution that mass fraction is 37%HCl by different proportion, adds deionized water, fully
Stir evenly and obtain the different electrolyte solution of concentration (0.01mol/L~0.3mol/L)；
(2) electrolytic cell is prepared
Electrolyte is measured to pour into electrolytic cell；In the Fe particles for the process nitrogen treatment for weighing certain mass, pour into
In thin glass tube, then thin glass tube is put into square electrolytic cell, electrolyte will submerge thin glass tube.Platinized platinum and platinum filament are inserted
On punched rubber stopper, in the Fe particles for the process nitrogen treatment that one end of platinum filament is inserted to thin glass tube；
(3) externally-applied magnetic field is prepared
Two block permanent magnets, magnetic field intensity ＞ 0.2T are placed in the both sides of the inner square electrolytic cell of step (2).
(4) to carrying out electrochemical treatments by the Fe particles of nitrogen treatment：
On the basis of step (3), the electrolytic cell for being provided with externally-applied magnetic field is put into after 0.01mol/L electrolyte, put
Enter in water-bath, DC stable power supply is adjusted to a certain magnitude of voltage (50V) with water-bath one constant temperature (60 DEG C) of offer and closed afterwards
Power supply is closed, positive source platinum filament one end is accessed into, negative pole access platinized platinum one end turns on the power beginning timing, to by nitridation
The Fe particles of reason carry out electrochemical treatments, and certain time, (80 mins) closed power supply afterwards.Take out glass tube and pour out sample, be made
Sample 0.01mol50V80M.
(5) change concentration of electrolyte (0.1mol/L), measure again after electrolyte in step (2), the voltage of access power supply
Sample is made on the basis of 60 DEG C, to change reaction time (80mins) repeat step (4) in (40V), reaction temperature
0.1mol40V80M。
(6) change concentration of electrolyte (0.3mol/L), measure again after electrolyte in step (2), reaction time
80mins, reaction temperature are 60 DEG C, accessed on the basis of the voltage (50V) of power supply, repeat step (4), and sample is made
0.3mol50V80M。
(7) will obtained 3 samples washes of absolute alcohol 3 to 4 times, be put into vacuum drying chamber, vacuum for-
Dried 6 hours in the case of 0.1,50 DEG C.
Embodiment 2：Verify the presence of nitrided iron/ferric oxide nano chain
1st, the presence of checking product nitrided iron/iron oxide
With x-ray diffractometer (XRD；DX-2000SSC) the Fe-N/Fe that in testing example 1 prepared by electrochemistry3O4It is heterogeneous
Nano chain, corresponding X-ray diffracting spectrum, is shown in Fig. 3.By the position of each diffraction maximum in Fig. 3 and relative intensity and standard PDF
Card (Fe2N)(No.72-2126)、Fe3O4(No.77-1545)) compared to knowable to, the obtained sample of present invention experiment is nitridation
The mixed phase of iron/iron oxide.
2nd, the pattern that nitrided iron/iron oxide is nano chain is confirmed
With transmission electron microscope (TEM；) and cold field emission formula ESEM (S-4800) testing example JEM-2100
1 series of samples prepared, obtains the transmission plot and scanning figure of each sample, sees Fig. 2~Fig. 6.It can be seen that in Fig. 2~Fig. 6
Prepared sample is 40~110nm of width, and length is 1~15 μm of long chain structure.
Embodiment 3：The sign of gained sample
(1) according to the PDF cards (No.72-2126) of standard, it may be determined that pass through ammonia by original Fe nanometer particles
The sample of annealing is single-phase nitrided iron Fe2N.As shown in Figure 2.
(2) Fe-N Alloyses particle is added first0.1mol/L electrolyte, electrolyte temperature passes through water-bath
Control.Then the voltage output of power supply is set to 30V~50V, reacted 80 minutes.Magnetic particle is finally separating out, with anhydrous
Alcohol washes several times, are dried in vacuo (vacuum 0.1,50 DEG C and 6h).Shown in the XRD of sample such as Fig. 3 (a).Except Fe in figure2N
Diffraction maximum outside, occur in that other diffraction maximums.According to standard PDF cards (No.77-1545), these diffraction maximums can be characterized
For Fe3O4。Fe3O4Highest peak positioned at 2 θ=35.6 ° (311) diffraction maximum.
(3) Fe-N Alloyses particle is addedElectrolyte in, the voltage output of power supply is set to 50V, be electrolysed
The concentration of liquid is set to 0.01,0.1,0.3mol/L, react 80 minutes.Magnetic particle is finally separating out, is cleaned with absolute alcohol
Several times, it is dried in vacuo (vacuum 0.1,50 DEG C and 6h).Shown in the XRD of sample such as Fig. 3 (b).Except Fe in figure2N diffraction maximum
Outside, occur in that other diffraction maximums.According to standard PDF cards (No.77-1545), these diffraction maximums can be characterized as Fe3O4。
Fe3O4Highest peak positioned at 2 θ=35.6 ° (311) diffraction maximum.
(4) Fe-N Alloyses particle is addedElectrolyte in, the voltage output of power supply is set to 50V, be electrolysed
The concentration of liquid is set to 0.3mol/L, reacts 80 minutes, is finally separating out magnetic particle, is cleaned with absolute alcohol several times, vacuum
Dry (vacuum 0.1,50 DEG C and 6h).Shown in TEM and SEM such as Fig. 3 (b) of sample.Shown according to result, sample is simple grain
40~110nm of width that son is constituted, length is 3~8 μm of long nano chains.Nano chain is arranged together bunchy assembling structure.
(5) Fe-N Alloyses particle is addedElectrolyte in, the voltage output of power supply is set to 40V, be electrolysed
The concentration of liquid is set to 0.1mol/L, reacts 80 minutes, is finally separating out magnetic particle, is cleaned with absolute alcohol several times, vacuum
Dry (vacuum 0.1,50 DEG C and 6h).The TEM of sample is as shown in Figure 5.Shown according to result, sample is what single-particle was constituted
40~110nm of width, length is 2~14 μm of long nano chains.
(6) Fe-N Alloyses particle is addedElectrolyte in, the voltage output of power supply is set to 50V, electrolyte
Concentration be set to 0.01mol/L, react 60 minutes, be finally separating out magnetic particle, cleaned with absolute alcohol several times, vacuum
Dry (vacuum 0.1,50 DEG C and 6h).The TEM of sample is as shown in Figure 6.Shown according to result, sample is what single-particle was constituted
40~110nm of width, length is 1~15 μm of long nano chain.The degree of scatter of nano chain is preferable.
Claims (5)
1. a kind of preparation method for heterogeneous nano chain of destroying first and then establish, it is characterised in that：Comprise the following steps successively：
（1）, prepare electrolyte used in electrochemistry experiment：
Acid solution is configured, using this acid solution as the electrolyte of electrochemical reaction, the concentration of acid solution is 0.01 mol/
Any one concentration value in the range of the mol/L of L~0.3；
（2）, prepare electrolytic cell：
Measure and account for the electrolyte of the volume of electrolytic cell 4/5 and pour into electrolytic cell, then weigh and poured into by the Fe particles of nitrogen treatment
In glass tube, the amount that Fe particles are weighed can fill up glass tube, and the mouth of pipe of glass tube is blocked with the rubber stopper punched；Again
Glass tube is put into electrolytic cell, it is ensured that electrolyte submerges glass tube；Platinized platinum and platinum filament are finally inserted into punched rubber
Beyond the Great Wall, wherein platinum filament one end insertion glass tube in by nitrogen treatment Fe particles in, platinized platinum be in glass tubule outside not with
Fe particles are in contact, and using platinized platinum as the negative electrode of connection power supply, the positive electrode of connection power supply is used as using platinum filament；
（3）, prepare externally-applied magnetic field：
In step（2）In two symmetrical sides of electrolytic cell place permanent magnet respectively, both sides permanent magnet magnetism is attracting, by both sides permanent magnetism
Body forms the magnetic field that magnetic field intensity is more than 0.2 T into electrolytic cell；
（4）, in glass tube by nitrogen treatment Fe particles carry out electrochemical treatments：
By step（3）The electrolytic cell for being applied with magnetic field is integrally put into water-bath together with glass tube therein, is provided by water-bath
Isoperibol, the temperature value of isoperibol is any one temperature value of room temperature~70 DEG C；Then using DC stable power supply with
Electrode connection on glass tube rubber stopper, the positive pole of wherein DC stable power supply is connected with platinum filament, the negative pole of DC stable power supply
It is connected with platinized platinum, a burning voltage is provided from DC stable power supply into glass tube, to passes through nitrogen treatment in glass tube
Fe particles carry out electrochemical treatments, and the stable voltage is 20V~60V any one magnitude of voltage；During one section of electrochemical treatments
Between after close DC stable power supply, the electrochemical treatments time be 40mins~90mins any one time value；
（5）, with step（1）The concentration of middle acid solution is condition one, with step（3）The magnetic field intensity of middle application is condition two,
With step（4）The temperature value of middle isoperibol is condition three, with step（4）The stable voltage that middle DC stable power supply is provided is made
For condition four, with step（4）The middle electrochemical treatments time, as condition five, passes through repeat step（1）、（2）、（3）、（4）And change
Change condition one, two, three, four, five, is made several samples, by all samples washes of absolute alcohol 2~5 times, then by upper strata without
Each sample is put into vacuum drying chamber by water-ethanol again after pouring out, in vacuum drying chamber using vacuum as -0.05~-
0.15th, temperature is dry 5~7 hours under conditions of 40 DEG C~60 DEG C, obtains Fe-N/Fe3O4Heterogeneous nano chain.
2. a kind of preparation method of heterogeneous nano chain of destroying first and then establish according to claim 1, it is characterised in that：Step（1）
The selection of the concentration of electrolyte of conditional one is 0.01mol/L, step（3）The magnetic field intensity that conditional two applies is more than 0.2 T's
Stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The DC stable power supply of conditional four is carried
The stable voltage of confession is 30V, step（4）The electrochemical treatments time of conditional five is 80mins, and sample is made
0.01mol30V80M；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.01mol/L, step（3）Conditional two apply magnetic field intensity be
More than 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The direct current of conditional four
The stable voltage that stabilized power source is provided is 30V, step（4）The electrochemical treatments time of conditional five is the mins of 50 mins~70
In any one time value, sample 0.01mol30V50M~80M is made；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.01mol/L, step（3）Conditional two apply magnetic field intensity be
More than 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The direct current of conditional four
The stable voltage that stabilized power source is provided is any one magnitude of voltage in the range of 30V~50V, step（4）The electrification of conditional five
Processing time is any one time value in the range of the mins of 50 mins~80, and sample 0.01mol30V~50V50M is made
~80M；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.01mol/L, step（3）Conditional two apply magnetic field intensity be
More than 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is any one in the range of room temperature~60 DEG C
Individual temperature value, step（4）The stable voltage that the DC stable power supply of conditional four is provided is any one in the range of 30V~50V
Individual magnitude of voltage, step（4）The electrochemical treatments time of conditional five is any one time in the range of the mins of 50 mins~80
Value, is made sample 0.01mol30V~50V50M~80M27~60 DEG C；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.01mol/L, changes step（3）The magnetic field that conditional two applies is strong
Degree, but still magnetic field intensity is more than 0.2 T, step（4）The temperature value of the isoperibol of conditional three is in the range of room temperature~60 DEG C
Any one temperature value, step（4）The stable voltage that the DC stable power supply of conditional four is provided is in the range of 30V~50V
Any one magnitude of voltage, step（4）The electrochemical treatments time of conditional five is any in the range of the mins of 50 mins~80
One time value, is made sample 0.01mol30V~50V50M~80M27~60 DEG C >=0.2T.
3. a kind of preparation method of heterogeneous nano chain of destroying first and then establish according to claim 1, it is characterised in that：Step（1）
The selection of the concentration of electrolyte of conditional one is 0.1mol/L, step（3）The magnetic field intensity that conditional two applies is the perseverance more than 0.2 T
Fixed-field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The DC stable power supply of conditional four is provided
Stable voltage be 40V, step（4）The electrochemical treatments time of conditional five is 80 mins, and sample is made
0.1mol40V80M；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.1mol/L, step（3）The magnetic field intensity that conditional two applies is big
In 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The direct current of conditional four is steady
The stable voltage for determining power supply offer is 40V, step（4）During the electrochemical treatments time of conditional five is the mins of 50 mins~70
Any one time value, sample 0.1mol40V50M~70M is made；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.1mol/L, step（3）The magnetic field intensity that conditional two applies is big
In 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The direct current of conditional four is steady
The stable voltage for determining power supply offer is any one magnitude of voltage in the range of 30V~50V, step（4）The electrochemistry of conditional five
Processing time is any one time value in the range of the mins of 50 mins~80, be made sample 0.1mol30V~50V50M~
80M；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.1mol/L, step（3）The magnetic field intensity that conditional two applies is big
In 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is any one in the range of room temperature~60 DEG C
Temperature value, step（4）The stable voltage that the DC stable power supply of conditional four is provided is any one in the range of 30V~50V
Magnitude of voltage, step（4）The electrochemical treatments time of conditional five is any one time value in the range of the mins of 50 mins~80,
Sample 0.1mol30V~50V50M~80M27~60 DEG C are made；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.1mol/L, changes step（3）The magnetic field that conditional two applies is strong
Degree, but still magnetic field intensity is more than 0.2 T, step（4）The temperature value of the isoperibol of conditional three is in the range of room temperature~60 DEG C
Any one temperature value, step（4）The stable voltage that the DC stable power supply of conditional four is provided is in the range of 30V~50V
Any one magnitude of voltage, step（4）The electrochemical treatments time of conditional five is any in the range of the mins of 50 mins~80
One time value, is made sample 0.1mol30V~50V50M~80M27~60 DEG C >=0.2T.
4. a kind of preparation method of heterogeneous nano chain of destroying first and then establish according to claim 1, it is characterised in that：Step（1）
The selection of the concentration of electrolyte of conditional one is 0.3mol/L, step（3）The magnetic field intensity that conditional two applies is the perseverance more than 0.2 T
Fixed-field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The DC stable power supply of conditional four is provided
Stable voltage be 50V, step（4）The electrochemical treatments time of conditional five is 80 mins, and sample is made
0.3mol50V80M；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.3mol/L, step（3）The magnetic field intensity that conditional two applies is big
In 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The direct current of conditional four is steady
The stable voltage for determining power supply offer is 50V, step（4）The electrochemical treatments time of conditional five is the mins models of 50 mins~70
Any one interior time value is enclosed, sample 0.3mol50V50M~70M is made；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.3mol/L, step（3）The magnetic field intensity that conditional two applies is big
In 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is 60 DEG C, step（4）The direct current of conditional four is steady
The stable voltage for determining power supply offer is any one magnitude of voltage in the range of 30V~50V, step（4）The electrochemistry of conditional five
Processing time is any one time value in the range of the mins of 50 mins~80, be made sample 0.3mol30V~50V50M~
80M；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.3mol/L, step（3）The magnetic field intensity that conditional two applies is big
In 0.2 T stationary magnetic field, step（4）The temperature value of the isoperibol of conditional three is any one in the range of room temperature~60 DEG C
Temperature value, step（4）The stable voltage that the DC stable power supply of conditional four is provided is any one in the range of 30V~50V
Magnitude of voltage, step（4）The electrochemical treatments time of conditional five is any one time value in the range of the mins of 50 mins~80,
Sample 0.3mol30V~50V50M~80M27~60 DEG C are made；
Step（1）The selection of the concentration of electrolyte of conditional one is 0.3mol/L, changes step（3）The magnetic field that conditional two applies is strong
Degree, but still magnetic field intensity is more than 0.2 T, step（4）The temperature value of the isoperibol of conditional three is in the range of room temperature~60 DEG C
Any one temperature value, step（4）The stable voltage that the DC stable power supply of conditional four is provided is in the range of 30V~50V
Any one magnitude of voltage, step（4）The electrochemical treatments time of conditional five is any in the range of the mins of 50 mins~80
One time value, is made sample 0.1mol30V~50V50M~80M27~60 DEG C >=0.2T.
5. a kind of preparation method of heterogeneous nano chain of destroying first and then establish according to claim 1, it is characterised in that：Step（5）
In, vacuum is preferably preferably 50 DEG C of -0.1, temperature, preferably 6 hours drying time in vacuum drying chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710383681.8A CN107265414A (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method for heterogeneous nano chain of destroying first and then establish |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710383681.8A CN107265414A (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method for heterogeneous nano chain of destroying first and then establish |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107265414A true CN107265414A (en) | 2017-10-20 |
Family
ID=60065638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710383681.8A Pending CN107265414A (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method for heterogeneous nano chain of destroying first and then establish |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107265414A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111732127A (en) * | 2020-07-02 | 2020-10-02 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587025A (en) * | 2004-08-13 | 2005-03-02 | 清华大学 | Magnetic field inducing method for growing magnetic one dimension nano line array |
| CN102925937A (en) * | 2012-09-07 | 2013-02-13 | 上海大学 | Method and device for continuously preparing high-silicon steel ribbon under magnetic field |
| CN104817119A (en) * | 2015-04-03 | 2015-08-05 | 安徽师范大学 | Preparation method and applications of transition metallide |
| CN106312049A (en) * | 2016-09-22 | 2017-01-11 | 安徽大学 | Electrochemical control method for thickness of shell layer of Fe/Fe2O3 core/shell structure |
-
2017
- 2017-05-26 CN CN201710383681.8A patent/CN107265414A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587025A (en) * | 2004-08-13 | 2005-03-02 | 清华大学 | Magnetic field inducing method for growing magnetic one dimension nano line array |
| CN102925937A (en) * | 2012-09-07 | 2013-02-13 | 上海大学 | Method and device for continuously preparing high-silicon steel ribbon under magnetic field |
| CN104817119A (en) * | 2015-04-03 | 2015-08-05 | 安徽师范大学 | Preparation method and applications of transition metallide |
| CN106312049A (en) * | 2016-09-22 | 2017-01-11 | 安徽大学 | Electrochemical control method for thickness of shell layer of Fe/Fe2O3 core/shell structure |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111732127A (en) * | 2020-07-02 | 2020-10-02 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
| CN111732127B (en) * | 2020-07-02 | 2022-04-19 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dubois et al. | Spectroelectrochemical study of the C60 and C70 fullerenes and their mono-, di-, tri-and tetraanions | |
| Ashkenani et al. | Selective voltammetric determination of Cu (II) based on multiwalled carbon nanotube and nano-porous Cu-ion imprinted polymer | |
| Hu et al. | α‐Fe2O3 nanorings prepared by a microwave‐assisted hydrothermal process and their sensing properties | |
| Legrand et al. | Study of oxidation products formed on iron in solutions containing bicarbonate/carbonate | |
| Galindo et al. | Electrochemical synthesis of NiFe2O4 nanoparticles: Characterization and their catalytic applications | |
| Xiong et al. | Electrochemical detection of ultra-trace Cu (II) and interaction mechanism analysis between amine-groups functionalized CoFe2O4/reduced graphene oxide composites and metal ion | |
| Jana et al. | Shape-selective synthesis, magnetic properties, and catalytic activity of single crystalline β-MnO2 nanoparticles | |
| CN105259243B (en) | The preparation method of molybdenum sulfide compound and its in water is detected Cr VI application | |
| Sang et al. | Electrochemical reaction of nitrobenzene and its derivatives on glassy carbon electrode modified with MnFe2O4 colloid nanocrystal assemblies | |
| Shen et al. | Prussian blue hollow nanostructures: Sacrificial template synthesis and application in hydrogen peroxide sensing | |
| Kumar et al. | Facile size-controllable synthesis of single crystalline β-MnO 2 nanorods under varying acidic strengths | |
| Xia et al. | Reliable electroanalysis of Hg (II) in water via flower-like porous MnCo2O4: Excellent multilayer adsorption and (Mn, Co)(II)/(Mn, Co)(III) cycles | |
| Wang et al. | Fast preparation, characterization, and property study of α-Fe2O3 nanoparticles via a simple solution-combusting method | |
| CN107265414A (en) | A kind of preparation method for heterogeneous nano chain of destroying first and then establish | |
| Raymundo-Pereira et al. | A nanostructured label-free platform based on an ultrathin film for ultrasensitive detection of a secosteroid hormone | |
| Venosta et al. | Comparative studies of hybrid functional materials based on different carbon structures decorated with nano-magnetite. Suitable application as platforms for enzyme-free electrochemical sensing of hydrogen peroxide | |
| Aghazadeh et al. | Gd 3+ doped Fe 3 O 4 nanoparticles with proper magnetic and supercapacitive characteristics: A novel synthesis platform and characterization | |
| Divagar et al. | Surface imprinted Ag decorated MnO2 thin film electrodes for the synergic electrochemical detection of bacterial pathogens | |
| Nazeer et al. | Optical, photocatalytic, electrochemical, magnetic, dielectric, and ferroelectric properties of Cd-and Er-doped BiFeO3 prepared via a facile microemulsion route | |
| Dong et al. | Designed 3D porous core-shell vanadium oxide microspheres for the simultaneous electrochemical sensing of toxic metal ions | |
| Pham et al. | Toward a comprehensive understanding of effect of cation distribution and M2+ constituent in spinel ferrite nanocrystals MFe2O4 (M= Co, Mn, and Ni) on the electrochemical response in sensitive detection of chloramphenicol | |
| Sanati et al. | A new nanostructure approach based on Pr (OH) 3/GQD and imidazolium ionic liquid for voltammetric analysis of tramadol | |
| Carla et al. | Electrochemical characterization of core@ shell CoFe 2 O 4/Au composite | |
| Abood et al. | New Fe2O3 Nanoparticles Modified Carbon Paste Electrode: A Cyclic Voltammetric Study | |
| Yuan et al. | Improved potentiometric response of solid-contact lanthanum (III) selective electrode |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171020 |
|
| WD01 | Invention patent application deemed withdrawn after publication |