CN106315656A - Preparation method and application of graphene-coated nano dysprosium oxide - Google Patents
Preparation method and application of graphene-coated nano dysprosium oxide Download PDFInfo
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Abstract
The invention provides a preparation method of graphene-coated nano dysprosium oxide. The method comprises the following steps that dysprosium oxide nanoparticles are prepared through a pyrolysis method; 2, dysprosium oxide nanometer columns are prepared through a hydrothermal method; 3, a graphene oxide solution is prepared; 4, the dysprosium oxide nanoparticles and the dysprosium oxide nanometer columns are added into the graphene oxide solution, stirring and filtering are conducted in sequence, filter residues are obtained, and the filter residues are subjected to heat treatment to obtain graphene-coated nano dysprosium oxide. In addition, the invention provides application of graphene-coated nano dysprosium oxide prepared through the method in the process of preparing two-element-doped magnesium diboride superconducting bulk materials. According to the preparation method, the technological method is simple, graphene with high surface area is adopted as a coating, the dysprosium oxide nanoparticles and the dysprosium oxide nanometer columns can be uniformly dispersed on the graphene without generating agglomeration, and the critical current density Jc performance of the two-element-doped magnesium diboride superconducting bulk materials in a low field and a high field can be improved conveniently.
Description
Technical field
The invention belongs to high temperature superconducting materia technical field, be specifically related to the preparation of the nano oxidized dysprosium of a kind of graphene coated
Method and application thereof.
Background technology
Rare earth oxide dysprosia (Dy2O3) there are excellent physicochemical properties, it is widely used in catalysis material, sends out
In the fields such as luminescent material, solid fuel cell, pinning magnesium diboride superconductive.When the size of dysprosia granule gradually decreases to nanometer
Size, specific surface area increases generation skin effect, and the surface texture difference of nano oxidized dysprosium causes its reactivity the most inconsistent.
In traditional preparation method, nano-oxide is susceptible to reunite, and the highly active surface of more difficult acquisition.
Simultaneously for magnesium diboride super conductive material, in order to improve the performance under magnetic field of mgb 2 superconductor, need
By introducing effective pinning center.In conventional methods where, single-element or hydrocarbon doped with organic matter, such as element are generally used
C etc., improve magnesium diboride High-Field lower critical current density, J c performance.But general all its activity of doped source are relatively low, degree of scatter
Difference, needs higher heat treatment temperature could introduce effective doping, and skewness, it is easy to reunite at grain boundaries,
Reduce intercrystalline connectivity.Therefore, improve nano oxidized dysprosium dispersibility and activity by graphene coated powder, be introduced into
In magnesium diboride, it is achieved binary doped, superconductivity can be improved greatly.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, it is provided that a kind of Graphene bag
Cover the preparation method of nano oxidized dysprosium.This preparation method is simple, it is easy to accomplish industrialization, use Graphene as coating, its
There is higher surface area, beneficially dysprosia nano-particle and dysprosia nano-pillar be evenly dispersed on Graphene, do not produce
Life is reunited, and dysprosia nano-particle and the dysprosia nano-pillar prepared have different morphologies and highly active crystal face, favorably
Prepare binary doped magnesium diboride superconductive bulk in being subsequently applied to.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the nano oxidized dysprosium of a kind of graphene coated
Preparation method, it is characterised in that the method comprises the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium
Solution is placed in pyrolysis reactor furnace, first carries out drying and processing under conditions of temperature is 120 DEG C, then at moist oxygen atmosphere
Under, with heating rate be 0.1 DEG C/min～10 DEG C/min is continuously heating to 500 DEG C, obtains dysprosia nano-particle；Described mixing
In solvent, the volume ratio of ethanol and propanoic acid is 1:1；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of tert-butylamine or the aqueous solution of glycine, is subsequently placed in water
In thermal response still, after hydro-thermal reaction, obtain dysprosia nano-pillar；Tert-butylamine and water in the aqueous solution of described tert-butylamine
Volume ratio is 1:(4～10)；The volume ratio of the Ammonia In Aqueous Solution guanidine-acetic acid water of described glycine is 1:(4～10)；
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains aoxidizing stone
Ink alkene solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:(50～100)；Institute
Stating the concentration of graphene oxide in graphene oxide solution is 0.5mg/mL～10mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:(1～
3) quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by institute after stirring
State filtering residue to be placed in heat-treatment furnace, under inert gas shielding, temperature be 400 DEG C～800 DEG C under conditions of heat treatment 0.5h～
5h, obtains the nano oxidized dysprosium of graphene coated.
The preparation method of the above-mentioned nano oxidized dysprosium of a kind of graphene coated, it is characterised in that heat up described in step one
Speed is 1 DEG C/min～3 DEG C/min.
The preparation method of the above-mentioned nano oxidized dysprosium of a kind of graphene coated, it is characterised in that moist described in step one
Oxygen atmosphere in the volumn concentration of oxygen be 94%～99.4%, surplus is steam.
The preparation method of the above-mentioned nano oxidized dysprosium of a kind of graphene coated, it is characterised in that hydro-thermal described in step 2
The temperature of reaction is 120 DEG C～220 DEG C, and the response time of described hydro-thermal reaction is 1h～10h.
The preparation method of the above-mentioned nano oxidized dysprosium of a kind of graphene coated, it is characterised in that aoxidize described in step 4
The quality of graphene oxide and dysprosia nano-particle and the ratio of the gross mass of dysprosia nano-pillar mixture in graphene solution
For 1:(50～100).
The preparation method of the above-mentioned nano oxidized dysprosium of a kind of graphene coated, it is characterised in that stir described in step 4
Speed be 100r/min～1000r/min, the time of stirring is 2min～10min.
Meanwhile, present invention also offers the nano oxidized dysprosium of graphene coated that a kind of profit prepared with the aforedescribed process should
With, it is characterised in that the nano oxidized dysprosium of described graphene coated is used for preparing binary doped magnesium diboride superconductive bulk, specifically makes
Standby process is: by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium be 1:2:(0.01～
0.2) ratio mixed grinding, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protecting down, temperature is heat treatment 1h～3h under conditions of 750 DEG C～850 DEG C, obtains binary doped magnesium diboride superconductive bulk.
Above-mentioned application, it is characterised in that the quality purity of described magnesium powder and boron powder all not less than 99%, described high-purity argon
The quality purity of gas is 99.99%.
Above-mentioned application, it is characterised in that the pressure of described compacting is 10MPa～20MPa.
The present invention compared with prior art has the advantage that
1, the present invention prepares dysprosia nano-particle and dysprosia nano-pillar, and uses graphene coated dysprosia nanometer
Granule and dysprosia nano-pillar, the Graphene of layer structure can be strutted by dysprosia nano-pillar, so that dysprosia nano-particle quilt
Being coated in the layer structure of Graphene, beneficially dysprosia nano-particle and dysprosia nano-pillar is dispersed in Graphene
On, fully inhibit the generation that nanoparticle is reunited.Meanwhile, the crystal face (222) of dysprosia nano-pillar is high activity crystal face, application
Its superconductivity can be improved in preparing binary doped magnesium diboride superconductive bulk.
2, the present invention uses Graphene as coating, itself has high surface area and reactivity.Use and first wrap
The processing method cover, restored, beneficially dysprosia nanometer are fully combined and dispersed with Graphene.Meanwhile, Graphene is originally
As carbon doping source when body is alternatively subsequently applied to prepare binary doped magnesium diboride superconductive bulk, magnesium diboride more can be improved
Superconductivity.
3, the present invention can keep the high activity crystal face of nano oxidized dysprosium, the nano oxidized dysprosium of follow-up graphene coated
It is applied to prepare binary doped magnesium diboride superconductive bulk, improves the reactivity of dysprosium doped thing, it is possible to decrease become phase temperature, more
It is easily accessible the lattice of magnesium diboride.The doping particle dysprosia of two kinds of different-shapes and size is more beneficial for surpassing at magnesium diboride
Filling in guide block material, improves superconductivity.
4, preparation method of the present invention is simple, it is easy to accomplish industrialization.
Below by drawings and Examples, technical scheme is described in further detail.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the nano oxidized dysprosium of graphene coated of the embodiment of the present invention 1 preparation.
Detailed description of the invention
Embodiment 1
The present embodiment is prepared the method for the nano oxidized dysprosium of graphene coated and is comprised the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium
Solution is placed in pyrolysis reactor furnace, first carries out drying and processing under conditions of temperature is 120 DEG C, then at moist oxygen atmosphere
Under, it is that 2 DEG C/min is continuously heating to 500 DEG C with heating rate, obtains dysprosia nano-particle；In described mixed solvent ethanol and
The volume ratio of propanoic acid is 1:1；In the oxygen atmosphere of described humidity, the volumn concentration of oxygen is 96.5%, and surplus is steam；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of tert-butylamine, is subsequently placed in hydrothermal reaction kettle, through hydro-thermal reaction
After obtain dysprosia nano-pillar；In the aqueous solution of described tert-butylamine, tert-butylamine is 1:7 with the volume ratio of water；Described hydro-thermal is anti-
The temperature answered is 170 DEG C, and the response time of described hydro-thermal reaction is 5.5h.
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains aoxidizing stone
Ink alkene solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:75；Described oxidation
In graphene solution, the concentration of graphene oxide is 5mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:2's
Quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by described filter after stirring
Slag is placed in heat-treatment furnace, under inert gas shielding, temperature be 600 DEG C under conditions of heat treatment 2.5h, obtain Graphene bag
Cover nano oxidized dysprosium；The quality of graphene oxide and dysprosia nano-particle and dysprosia nanometer in described graphene oxide solution
The ratio of the gross mass of post mixture is 1:100；The speed of described stirring is 550r/min, and the time of stirring is 6min.
Fig. 1 is the scanning electron microscope (SEM) photograph of the nano oxidized dysprosium of graphene coated of the embodiment of the present invention 1 preparation, can from figure
Go out nanometer dysprosia and there are graininess and two kinds of patterns of column, illustrate to be prepared into dysprosia nanometer by above-mentioned steps one
Grain, has prepared dysprosia nano-pillar by above-mentioned steps two, and dysprosia nano-particle and dysprosia nano-pillar can be equal
It is scattered in the layer structure of Graphene evenly, does not the most exist and reunite significantly.It can be seen that dysprosia nano-particle
Particle diameter be 10nm～100nm, a length of 300nm～500nm of dysprosia nano-pillar, the diameter 10nm of dysprosia nano-pillar～
30nm, the open and flat ungauged regions of Graphene is reunited, is shown as single-layer graphene.
Meanwhile, the nano oxidized dysprosium of graphene coated of embodiment 1 preparation can enter magnesium diboride lattice as doped source,
Improve superconductivity.
The nano oxidized dysprosium of graphene coated prepared by the present embodiment is applied to prepare binary doped magnesium diboride superconductive bulk,
Concrete preparation process is: be 1:2 by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium:
The ratio mixed grinding of 0.1, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protect down, temperature be 800 DEG C under conditions of heat treatment 2h, obtain binary doped magnesium diboride superconductive bulk；Described magnesium powder and boron powder
Quality purity all not less than 99%, the quality purity of described high-purity argon gas is 99.99%；The pressure of described compacting is 10MPa.
Binary doped magnesium diboride superconductive bulk prepared by said method is at 20K, and during 1T, critical current density jc reaches
1.2×105A/cm2。
Embodiment 2
The present embodiment is prepared the method for the nano oxidized dysprosium of graphene coated and is comprised the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium
Solution is placed in pyrolysis reactor furnace, first carries out drying and processing under conditions of temperature is 120 DEG C, then at moist oxygen atmosphere
Under, it is that 5 DEG C/min is continuously heating to 500 DEG C with heating rate, obtains dysprosia nano-particle；In described mixed solvent ethanol and
The volume ratio of propanoic acid is 1:1；In the oxygen atmosphere of described humidity, the volumn concentration of oxygen is 94%, and surplus is steam；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of glycine, is subsequently placed in hydrothermal reaction kettle, through hydro-thermal reaction
After obtain dysprosia nano-pillar；The Ammonia In Aqueous Solution guanidine-acetic acid of described glycine and the volume ratio of water are 1:4；Described hydro-thermal is anti-
The temperature answered is 120 DEG C, and the response time of described hydro-thermal reaction is 10h.
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains aoxidizing stone
Ink alkene solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:50；Described oxidation
In graphene solution, the concentration of graphene oxide is 0.5mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:1's
Quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by described filter after stirring
Slag is placed in heat-treatment furnace, under inert gas shielding, temperature be 400 DEG C under conditions of heat treatment 5h, obtain graphene coated
Nano oxidized dysprosium；The quality of graphene oxide and dysprosia nano-particle and dysprosia nano-pillar in described graphene oxide solution
The ratio of the gross mass of mixture is 1:85；The speed of described stirring is 100r/min, and the time of stirring is 10min.
Meanwhile, the nano oxidized dysprosium of graphene coated that prepared by the present embodiment can enter magnesium diboride lattice as doping
Source, improves superconductivity.
The nano oxidized dysprosium of graphene coated prepared by the present embodiment is applied to prepare binary doped magnesium diboride superconductive bulk,
Concrete preparation process is: be 1:2 by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium:
The ratio mixed grinding of 0.01, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protect down, temperature be 750 DEG C under conditions of heat treatment 3h, obtain binary doped magnesium diboride superconductive bulk；Described magnesium powder and boron powder
Quality purity all not less than 99%, the quality purity of described high-purity argon gas is 99.99%；The pressure of described compacting is 15MPa.
Binary doped magnesium diboride superconductive bulk prepared by said method is at 20K, and during 1T, critical current density jc reaches 1
×105A/cm2。
Embodiment 3
The present embodiment is prepared the method for the nano oxidized dysprosium of graphene coated and is comprised the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium
Solution is placed in pyrolysis reactor furnace, first carries out drying and processing under conditions of temperature is 120 DEG C, then at moist oxygen atmosphere
Under, it is that 1 DEG C/min is continuously heating to 500 DEG C with heating rate, obtains dysprosia nano-particle；In described mixed solvent ethanol and
The volume ratio of propanoic acid is 1:1；In the oxygen atmosphere of described humidity, the volumn concentration of oxygen is 99.4%, and surplus is steam；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of tert-butylamine, is subsequently placed in hydrothermal reaction kettle, through hydro-thermal reaction
After obtain dysprosia nano-pillar；In the aqueous solution of described tert-butylamine, tert-butylamine is 1:10 with the volume ratio of water；Described hydro-thermal
The temperature of reaction is 220 DEG C, and the response time of described hydro-thermal reaction is 1h.
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains aoxidizing stone
Ink alkene solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:100；Described oxidation
In graphene solution, the concentration of graphene oxide is 10mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:3's
Quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by described filter after stirring
Slag is placed in heat-treatment furnace, under inert gas shielding, temperature be 800 DEG C under conditions of heat treatment 0.5h, obtain Graphene bag
Cover nano oxidized dysprosium；The quality of graphene oxide and dysprosia nano-particle and dysprosia nanometer in described graphene oxide solution
The ratio of the gross mass of post mixture is 1:75；The speed of described stirring is 1000r/min, and the time of stirring is 2min.
Meanwhile, the nano oxidized dysprosium of graphene coated that prepared by the present embodiment can enter magnesium diboride lattice as doping
Source, improves superconductivity.
The nano oxidized dysprosium of graphene coated prepared by the present embodiment is applied to prepare binary doped magnesium diboride superconductive bulk,
Concrete preparation process is: be 1:2 by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium:
The ratio mixed grinding of 0.2, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protect down, temperature be 850 DEG C under conditions of heat treatment 1h, obtain binary doped magnesium diboride superconductive bulk；Described magnesium powder and boron powder
Quality purity all not less than 99%, the quality purity of described high-purity argon gas is 99.99%；The pressure of described compacting is 20MPa.
Binary doped magnesium diboride superconductive bulk prepared by said method is at 20K, and during 1T, critical current density jc reaches 7
×104A/cm2。
Embodiment 4
The present embodiment is prepared the method for the nano oxidized dysprosium of graphene coated and is comprised the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium
Solution is placed in pyrolysis reactor furnace, first carries out drying and processing under conditions of temperature is 120 DEG C, then at moist oxygen atmosphere
Under, it is that 0.1 DEG C/min is continuously heating to 500 DEG C with heating rate, obtains dysprosia nano-particle；Ethanol in described mixed solvent
It is 1:1 with the volume ratio of propanoic acid；In the oxygen atmosphere of described humidity, the volumn concentration of oxygen is 94%, and surplus is steam；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of glycine, is subsequently placed in hydrothermal reaction kettle, through hydro-thermal reaction
After obtain dysprosia nano-pillar；The Ammonia In Aqueous Solution guanidine-acetic acid of described glycine and the volume ratio of water are 1:8；Described hydro-thermal is anti-
The temperature answered is 220 DEG C, and the response time of described hydro-thermal reaction is 8h.
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains aoxidizing stone
Ink alkene solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:100；Described oxidation
In graphene solution, the concentration of graphene oxide is 3mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:2's
Quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by described filter after stirring
Slag is placed in heat-treatment furnace, under inert gas shielding, temperature be 600 DEG C under conditions of heat treatment 3h, obtain graphene coated
Nano oxidized dysprosium；The quality of graphene oxide and dysprosia nano-particle and dysprosia nano-pillar in described graphene oxide solution
The ratio of the gross mass of mixture is 1:85；The speed of described stirring is 800r/min, and the time of stirring is 4min.
Meanwhile, the nano oxidized dysprosium of graphene coated that prepared by the present embodiment can enter magnesium diboride lattice as doping
Source, improves superconductivity.
The nano oxidized dysprosium of graphene coated prepared by the present embodiment is applied to prepare binary doped magnesium diboride superconductive bulk,
Concrete preparation process is: be 1:2 by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium:
The ratio mixed grinding of 0.15, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protect down, temperature be 700 DEG C under conditions of heat treatment 2h, obtain binary doped magnesium diboride superconductive bulk；Described magnesium powder and boron powder
Quality purity all not less than 99%, the quality purity of described high-purity argon gas is 99.99%；The pressure of described compacting is 15MPa.
Binary doped magnesium diboride superconductive bulk prepared by said method is at 20K, and during 1T, critical current density jc reaches 1
×105A/cm2。
Embodiment 5
The present embodiment is prepared the method for the nano oxidized dysprosium of graphene coated and is comprised the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium
Solution is placed in pyrolysis reactor furnace, first carries out drying and processing under conditions of temperature is 120 DEG C, then at moist oxygen atmosphere
Under, it is that 10 DEG C/min is continuously heating to 500 DEG C with heating rate, obtains dysprosia nano-particle；Ethanol in described mixed solvent
It is 1:1 with the volume ratio of propanoic acid；In the oxygen atmosphere of described humidity, the volumn concentration of oxygen is 96%, and surplus is steam；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of tert-butylamine, is subsequently placed in hydrothermal reaction kettle, through hydro-thermal reaction
After obtain dysprosia nano-pillar；In the aqueous solution of described tert-butylamine, tert-butylamine is 1:6 with the volume ratio of water；Described hydro-thermal is anti-
The temperature answered is 150 DEG C, and the response time of described hydro-thermal reaction is 5h.
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains aoxidizing stone
Ink alkene solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:60；Described oxidation
In graphene solution, the concentration of graphene oxide is 7mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:3's
Quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by described filter after stirring
Slag is placed in heat-treatment furnace, under inert gas shielding, temperature be 700 DEG C under conditions of heat treatment 4h, obtain graphene coated
Nano oxidized dysprosium；The quality of graphene oxide and dysprosia nano-particle and dysprosia nano-pillar in described graphene oxide solution
The ratio of the gross mass of mixture is 1:50；The speed of described stirring is 300r/min, and the time of stirring is 8min.
Meanwhile, the nano oxidized dysprosium of graphene coated that prepared by the present embodiment can enter magnesium diboride lattice as doping
Source, improves superconductivity.
The nano oxidized dysprosium of graphene coated prepared by the present embodiment is applied to prepare binary doped magnesium diboride superconductive bulk,
Concrete preparation process is: be 1:2 by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium:
The ratio mixed grinding of 0.1, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protect down, temperature be 850 DEG C under conditions of heat treatment 3h, obtain binary doped magnesium diboride superconductive bulk；Described magnesium powder and boron powder
Quality purity all not less than 99%, the quality purity of described high-purity argon gas is 99.99%；The pressure of described compacting is 20MPa.
Binary doped magnesium diboride superconductive bulk prepared by said method is at 20K, and during 1T, critical current density jc reaches 9
×104A/cm2。
Embodiment 6
The present embodiment is prepared the method for the nano oxidized dysprosium of graphene coated and is comprised the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium
Solution is placed in pyrolysis reactor furnace, first carries out drying and processing under conditions of temperature is 120 DEG C, then at water vapor partial pressure is
Under the moist oxygen atmosphere of 2000Pa, it is that 7.5 DEG C/min is continuously heating to 500 DEG C with heating rate, obtains dysprosia nanometer
Granule；In described mixed solvent, the volume ratio of ethanol and propanoic acid is 1:1；The volume hundred of oxygen in the oxygen atmosphere of described humidity
Dividing content is 98%, and surplus is steam；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of glycine, is subsequently placed in hydrothermal reaction kettle, through hydro-thermal reaction
After obtain dysprosia nano-pillar；The Ammonia In Aqueous Solution guanidine-acetic acid of described glycine and the volume ratio of water are 1:7；Described hydro-thermal is anti-
The temperature answered is 200 DEG C, and the response time of described hydro-thermal reaction is 7h.
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains aoxidizing stone
Ink alkene solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:80；Described oxidation
In graphene solution, the concentration of graphene oxide is 10mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:1's
Quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by described filter after stirring
Slag is placed in heat-treatment furnace, under inert gas shielding, temperature be 800 DEG C under conditions of heat treatment 2h, obtain graphene coated
Nano oxidized dysprosium；The quality of graphene oxide and dysprosia nano-particle and dysprosia nano-pillar in described graphene oxide solution
The ratio of the gross mass of mixture is 1:65；The speed of described stirring is 1000r/min, and the time of stirring is 5min.
Meanwhile, the nano oxidized dysprosium of graphene coated that prepared by the present embodiment can enter magnesium diboride lattice as doping
Source, improves superconductivity.
The nano oxidized dysprosium of graphene coated prepared by the present embodiment is applied to prepare binary doped magnesium diboride superconductive bulk,
Concrete preparation process is: be 1:2 by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium:
The ratio mixed grinding of 0.07, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protect down, temperature be 800 DEG C under conditions of heat treatment 2h, obtain binary doped magnesium diboride superconductive bulk；Described magnesium powder and boron powder
Quality purity all not less than 99%, the quality purity of described high-purity argon gas is 99.99%；The pressure of described compacting is 15MPa.
Binary doped magnesium diboride superconductive bulk prepared by said method is at 20K, and during 1T, critical current density jc reaches 8
×104A/cm2。
The above, be only presently preferred embodiments of the present invention, and the present invention not does any restriction, every according to invention skill
Any simple modification, change and the equivalent structure change that above example is made by art essence, all still falls within the technology of the present invention
In the protection domain of scheme.
Claims (9)
1. the preparation method of the nano oxidized dysprosium of graphene coated, it is characterised in that the method comprises the following steps:
Step one, acetic acid dysprosium is dissolved in the mixed solvent of ethanol and propanoic acid, obtains acetic acid dysprosium solution, by described acetic acid dysprosium solution
It is placed in pyrolysis reactor furnace, under conditions of temperature is 120 DEG C, first carries out drying and processing, then under moist oxygen atmosphere,
With heating rate be 0.1 DEG C/min～10 DEG C/min is continuously heating to 500 DEG C, obtains dysprosia nano-particle；Described mixing is molten
In agent, the volume ratio of ethanol and propanoic acid is 1:1；
Step 2, Dysprosium trinitrate is dissolved in the aqueous solution of tert-butylamine or the aqueous solution of glycine, is subsequently placed in hydro-thermal anti-
Answer in still, after hydro-thermal reaction, obtain dysprosia nano-pillar；Tert-butylamine and the volume of water in the aqueous solution of described tert-butylamine
Ratio is 1:(4～10)；The Ammonia In Aqueous Solution guanidine-acetic acid of described glycine and the volume ratio of water are 1:(4～10)；
Step 3, it is added to graphene oxide in the mixed solvent of deionized water and ethanol stir, obtains graphene oxide
Solution；In the mixed solvent of described deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:(50～100)；Described oxygen
In functionalized graphene solution, the concentration of graphene oxide is 0.5mg/mL～10mg/mL；
Step 4, dysprosia nano-pillar described in dysprosia nano-particle described in step one and step 2 is pressed 1:(1～3)
Quality is added to than after mix homogeneously described in step 3 in graphene oxide solution, filters, obtain filtering residue, by described filter after stirring
Slag is placed in heat-treatment furnace, and in inert gas shielding, temperature is heat treatment 0.5h～5h under conditions of 400 DEG C～800 DEG C, obtains
The nano oxidized dysprosium of graphene coated.
The preparation method of the nano oxidized dysprosium of a kind of graphene coated the most according to claim 1, it is characterised in that step one
Described in heating rate be 1 DEG C/min～5 DEG C/min.
The preparation method of the nano oxidized dysprosium of a kind of graphene coated the most according to claim 1, it is characterised in that step one
Described in moist oxygen atmosphere the volumn concentration of oxygen be 94%～99.4%, surplus is steam.
The preparation method of the nano oxidized dysprosium of a kind of graphene coated the most according to claim 1, it is characterised in that step 2
Described in the temperature of hydro-thermal reaction be 120 DEG C～220 DEG C, the response time of described hydro-thermal reaction is 1h～10h.
The preparation method of the nano oxidized dysprosium of a kind of graphene coated the most according to claim 1, it is characterised in that step 4
Described in the quality of graphene oxide and dysprosia nano-particle and dysprosia nano-pillar mixture in graphene oxide solution
The ratio of gross mass is 1:(50～100).
The preparation method of the nano oxidized dysprosium of a kind of graphene coated the most according to claim 1, it is characterised in that step 4
Described in stirring speed be 100r/min～1000r/min, the time of stirring is 2min～10min.
7. the nano oxidized dysprosium of graphene coated that prepared by method as described in a claim any one of claim 1～6
Application, it is characterised in that described ink alkene is coated with nano oxidized dysprosium and is used for preparing binary doped magnesium diboride superconductive bulk, specifically makes
Standby process is: by magnesium powder, boron powder and the nano oxidized dysprosium of graphene coated according to the atomic ratio of magnesium, boron and dysprosium be 1:2:(0.01～
0.2) ratio mixed grinding, is then pressed into block, then is placed in heat-treatment furnace by described block, protects in high-purity argon gas atmosphere
Protecting, temperature is heat treatment 1h～3h under conditions of 750 DEG C～850 DEG C, obtains binary doped magnesium diboride superconductive bulk.
Application the most according to claim 7, it is characterised in that the quality purity of described magnesium powder and boron powder is all not less than
99%, the quality purity of described high-purity argon gas is 99.99%.
Application the most according to claim 7, it is characterised in that the pressure of described compacting is 10MPa～20MPa.
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