CN105016736A - Preparation method for composite superconducting material with high practicability - Google Patents
Preparation method for composite superconducting material with high practicability Download PDFInfo
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- CN105016736A CN105016736A CN201510396354.7A CN201510396354A CN105016736A CN 105016736 A CN105016736 A CN 105016736A CN 201510396354 A CN201510396354 A CN 201510396354A CN 105016736 A CN105016736 A CN 105016736A
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Abstract
The invention discloses a preparation method for a composite superconducting material with high practicability. The method comprises the steps: thoroughly grinding and mixing B4C and Mg powder, pressing the ground powder mixture into blocks, putting the powder mixture blocks into a ceramic crucible, covering the ceramic crucible with a ceramic inner cover, and sprinkling a proper amount of B2O3 powder along the edge of the inner cover or canning the inner cover with a metal tube, so as to form a sealed raw material; and then, carrying out vacuum sintering at the sintering temperature of 700-900 DEG C, carrying out heat preservation for 60-120 minutes, and then, naturally cooling the sintering product in vacuum, thereby obtaining the MgB2 composite superconducting material. According to the preparation method, cheap B4C powder reacts with Mg powder instead of expensive B powder, the MgB2 composite superconducting material is obtained through solid-phase replacement reaction under vacuum conditions, and C produced from reaction is directly doped into samples, so that a preparation process for a MgB2 superconductor is simplified, the requirements on reaction devices are lowered, meanwhile, the critical current density of the samples is improved, and the production cost for the MgB2 superconductor is greatly reduced.
Description
Technical field
The present invention relates to and relate to new material technology field, specifically, is the preparation method of the composite superconductor that a kind of practicality is high.
Background technology
MgB
2be the cryogenic superconductor with the highest superconducting transition temperature, transition temperature is up to 39.4K, and efficient carrier is cavity type.MgB
2belong to type (i.e. the minus superconductor of interfacial energy).Its lower critical magnetic field is at 27 ~ 48mT, and upper critical field is between 14 ~ 39T, and irreversibility field is between 6 ~ 35T.Critical current J C=106A/cm2 under null field condition.Compared with high-temperature superconductor, MgB
2there is longer coherence length.Energy band analysis shows, MgB
2be a kind of widely can be with compound, valence band is formed primarily of the s track of Mg and B atom and p orbital hybridization.Wherein, B-B keeps covalent bond structure, and Mg is ionic state, and outermost 2 electronics of Mg are all contributed and made it obtain electroconductibility to B.In addition, in the pressure range of current research, along with the rising of pressure, MgB
2tC follow quadratic relation or linear relationship and reduce.MgB
2thermal expansivity and compression factor similar, all there is anisotropic feature: c-axis to the level of response of heat higher than a axle.Under same Elevated Temperature Conditions, lattice constant is approximately 2 times that increase along a axle along the increase of c-axis.
MgB
2take phonon as the superconducting mechanism of medium, isotopic effect result of study shows, MgB
2belong to traditional BCS superconductor, higher debye temperature and strong electronics-phonon interact and result in higher transition temperature.MgB
2in, the isotope index α (B) of B has larger value, and the isotope index α (Mg) very little (0.02) of Mg.Therefore, vibrate the supraconductivity of related phonon to MgB2 with B and play Main Function.Relevant research also finds further: on the one hand, MgB
2resistance temperature-magnetic field dependence relation and intermetallic compound accord with, make it have larger Δ ρ/Δ ρ
0, magnetic resistance follows kohler rule; On the other hand, MgB
2when superconducting state, H
c2(T) curve all deviate from linear relationship when high temperature and low temperature, thus makes MgB
2have relatively high Hc2(T)=16.4T.
But no matter be up to the present MgB
2bulk or MgB
2technology of preparing all more complicated of film, but also not exclusively ripe.MgB
2bulk is the basis of the application of superconduction field of strong electricity and physical property research thereof, MgB
2main or the chemical solid phase reaction of the preparation method of superconductor material, with high-purity Mg powder and B powder for raw material, under high pressure sinters.
But due to highly volatile and the easily oxidizable of Mg, preparation technology is comparatively complicated, need parcel, high pressure, require higher to sintering condition like this, the necessary sealed high pressure of sintering oven, logical argon, hydrogen high pressure mixed gas in sintering process, the acquisition of especially high-purity B is more difficult and expensive.Critical current density separately due to pure magnesium diboride super conductive material is very fast with foreign field decay, limits the application of magnesium diboride super conductive material under high field environments.In order to improve the current-carrying performance under High-Field, people have to utilize doping, introduce flux pinning, improve the upper critical field of magnesium diboride super conductive material.
For prior art Problems existing, active research modification method, boronation magnesium base composite material preparation method and the new glass forming theory of exploring practicality are significant.
Summary of the invention
The object of the present invention is to provide the preparation method of the composite superconductor that a kind of practicality is high, utilize cheap B
4c powder replaces the B powder of high price and Mg powder to react, and utilizes crucible selfsealings technology, under vacuum, obtains MgB by solid phase replacement(metathesis)reaction
2composite superconductor, and the C that reaction generates directly adulterates in the sample to which, both simplifies MgB like this
2the preparation technology of superconductor, reduces the requirement to reaction unit, also improves the critical current density of sample simultaneously, has saved MgB greatly again
2the production cost of superconductor.
The present invention is achieved through the following technical solutions: the preparation method of the composite superconductor that a kind of practicality is high, comprises following preparation process and step:
A. the preparation of base material: by B
4c and Mg powder presses predetermined mol ratio, Mg:B=(0.8 ~ 1.2): 2.2 weigh, and then fully grind after drying, and the compacting of ground mixing raw material powder is formed mixing raw material block;
B. the sealing of base material: by described mixing raw material block, put into ceramic crucible, build with ceramic inner cap, be then sprinkled into appropriate B at inner cap edge
2o
3powder, or described mixing raw material block is put into metal capsule pipe, two ends seal; To implement the sealing to raw material, form sealing raw material;
C. the sintering of base material: sealing raw material is put into vacuum sintering furnace, or put into the process furnace being connected with shielding gas and sinter; Vacuum tightness remains on below 3Pa; The temperature schedule heated up is: 400 ~ 450 DEG C are incubated 1 ~ 2 hour, and 600 ~ 650 DEG C are incubated 1 ~ 2 hour, and 700 ~ 900 DEG C are incubated 60 ~ 120 minutes; Finally under vacuum atmosphere, naturally cool to room temperature; Finally obtain MgB2 composite superconductor.
Compared with prior art, the present invention has following beneficial effect:
The present invention utilizes cheap B
4c powder replaces the B powder of high price and Mg powder to react, and utilizes crucible selfsealings technology, under vacuum, obtains MgB by solid phase replacement(metathesis)reaction
2composite superconductor, and the C that reaction generates directly adulterates in the sample to which, both simplifies MgB like this
2the preparation technology of superconductor, reduces the requirement to reaction unit, also improves the critical current density of sample simultaneously, has saved MgB greatly again
2the production cost of superconductor.
The present invention is directed to MgB traditional at present
2the defect of superconductor material preparation method, as equipment configuration requires high, complicated process of preparation, manufacturing cost high etc., and the one provided is inexpensive, practical, the simple MgB of technique
2the preparation method of superconductive composite materials.
Embodiment
Below in conjunction with embodiment, the invention will be further described, and embodiments of the present invention include but not limited to the following example.
Embodiment 1:
A preparation method for the composite superconductor that practicality is high, comprises following preparation process and step:
A. the preparation of base material: by B
4c and Mg powder presses predetermined mol ratio, Mg:B=(0.8 ~ 1.2): 2.2 weigh, and then fully grind after drying, and the compacting of ground mixing raw material powder is formed mixing raw material block;
B. the sealing of base material: by described mixing raw material block, put into ceramic crucible, build with ceramic inner cap, be then sprinkled into appropriate B at inner cap edge
2o
3powder, or described mixing raw material block is put into metal capsule pipe, two ends seal; To implement the sealing to raw material, form sealing raw material;
C. the sintering of base material: sealing raw material is put into vacuum sintering furnace, or put into the process furnace being connected with shielding gas and sinter; Vacuum tightness remains on below 3Pa; The temperature schedule heated up is: 400 ~ 450 DEG C are incubated 1 ~ 2 hour, and 600 ~ 650 DEG C are incubated 1 ~ 2 hour, and 700 ~ 900 DEG C are incubated 60 ~ 120 minutes; Finally under vacuum atmosphere, naturally cool to room temperature; Finally obtain MgB2 composite superconductor.
Embodiment 2:
The present embodiment is at the enterprising one-step optimization in the basis of above-described embodiment, and the preparation method of the composite superconductor that a kind of practicality is high, comprises following preparation process and step:
A. the preparation of base material: by B
4c and Mg powder presses predetermined mol ratio after drying, and Mg:B=0.8:2.2 weighs, and then fully grinds, and the compacting of ground mixing raw material powder is formed mixing raw material block;
B. the sealing of base material: by described mixing raw material block, put into ceramic crucible, build with ceramic inner cap, be then sprinkled into appropriate B at inner cap edge
2o
3powder, or described mixing raw material block is put into metal capsule pipe, two ends seal; To implement the sealing to raw material, form sealing raw material;
C. the sintering of base material: sealing raw material is put into the vacuum sintering furnace that vacuum tightness remains on below 3Pa and sinter; First be warming up to 400 DEG C of insulations 1.5 hours, be warming up to 600 DEG C of insulations 1 hour, be finally warming up to 750 DEG C of insulations 80 minutes again; Finally under vacuum atmosphere, naturally cool to room temperature; Finally obtain MgB2 composite superconductor.
Analyzed by the measurement of standard four lead resistance, magnetic susceptibility measurement and X-Ray, magnesium diboride super conductive material prepared by the present embodiment possesses good superconductivity, and its critical transition temperature is higher than 33K, and superconducting phase is MgB
2.
Embodiment 3:
The present embodiment is at the enterprising one-step optimization in the basis of embodiment 1, and the preparation method of the composite superconductor that a kind of practicality is high, comprises following preparation process and step:
A. the preparation of base material: by B
4c and Mg powder presses predetermined mol ratio after drying, and Mg:B=1:2.2 weighs, and then fully grinds, and the compacting of ground mixing raw material powder is formed mixing raw material block;
B. the sealing of base material: by described mixing raw material block, put into ceramic crucible, build with ceramic inner cap, be then sprinkled into appropriate B at inner cap edge
2o
3powder, or described mixing raw material block is put into metal capsule pipe, two ends seal; To implement the sealing to raw material, form sealing raw material;
C. the sintering of base material: sealing raw material is put into the process furnace being connected with shielding gas that vacuum tightness remains on below 3Pa and sinter; First be warming up to 420 DEG C of insulations 1.5 hours, be warming up to 630 DEG C of insulations 1 hour, be finally warming up to 800 DEG C of insulations 90 minutes again; Finally under vacuum atmosphere, naturally cool to room temperature; Finally obtain MgB2 composite superconductor.
Analyzed by the measurement of standard four lead resistance, magnetic susceptibility measurement and X-Ray, magnesium diboride super conductive material prepared by the present embodiment possesses good superconductivity, and its critical transition temperature is higher than 35K, and superconducting phase is MgB
2.
Embodiment 4:
The present embodiment is in the preparation method of the high composite superconductor of the basis of embodiment 1 a kind of practicality of enterprising one-step optimization, comprises following preparation process and step:
A. the preparation of base material: by B
4c and Mg powder presses predetermined mol ratio after drying, and Mg:B=1.1:2.2 weighs, and then fully grinds, and the compacting of ground mixing raw material powder is formed mixing raw material block;
B. the sealing of base material: by described mixing raw material block, put into ceramic crucible, build with ceramic inner cap, be then sprinkled into appropriate B at inner cap edge
2o
3powder, or described mixing raw material block is put into metal capsule pipe, two ends seal; To implement the sealing to raw material, form sealing raw material;
C. the sintering of base material: sealing raw material is put into the vacuum sintering furnace that vacuum tightness remains on below 3Pa and sinter; First be warming up to 450 DEG C of insulations 2 hours, be warming up to 600 DEG C of insulations 1 hour, be finally warming up to 900 DEG C of insulations 100 minutes again; Finally under vacuum atmosphere, naturally cool to room temperature; Finally obtain MgB2 composite superconductor.
Analyzed by the measurement of standard four lead resistance, magnetic susceptibility measurement and X-Ray, magnesium diboride super conductive material prepared by the present embodiment possesses good superconductivity, and its critical transition temperature is higher than 34K, and superconducting phase is MgB
2.
Embodiment 5:
The present embodiment is the enterprising one-step optimization in basis of embodiment 1, and the preparation method of the composite superconductor that a kind of practicality is high, comprises following preparation process and step:
A. the preparation of base material: by B
4c and Mg powder presses predetermined mol ratio after drying, and Mg:B=1.2:2.2 weighs, and then fully grinds, and the compacting of ground mixing raw material powder is formed mixing raw material block;
B. the sealing of base material: by described mixing raw material block, put into ceramic crucible, build with ceramic inner cap, be then sprinkled into appropriate B at inner cap edge
2o
3powder, or described mixing raw material block is put into metal capsule pipe, two ends seal; To implement the sealing to raw material, form sealing raw material;
C. the sintering of base material: sealing raw material is put into the process furnace being connected with shielding gas that vacuum tightness remains on below 3Pa and sinter; First be warming up to 450 DEG C of insulations 1.5 hours, be warming up to 650 DEG C of insulations 1 hour, be finally warming up to 900 DEG C of insulations 120 minutes again; Finally under vacuum atmosphere, naturally cool to room temperature; Finally obtain MgB2 composite superconductor.
Analyzed by the measurement of standard four lead resistance, magnetic susceptibility measurement and X-Ray, magnesium diboride super conductive material prepared by the present embodiment possesses good superconductivity, and its critical transition temperature is higher than 29.4K, and superconducting phase is MgB
2.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.
Claims (1)
1. a preparation method for the composite superconductor that practicality is high, is characterized in that: comprise following preparation process and step:
A. the preparation of base material: by B
4c and Mg powder presses predetermined mol ratio, Mg:B=(0.8 ~ 1.2): 2.2 weigh, and then fully grind after drying, and the compacting of ground mixing raw material powder is formed mixing raw material block;
B. the sealing of base material: by described mixing raw material block, put into ceramic crucible, build with ceramic inner cap, be then sprinkled into appropriate B at inner cap edge
2o
3powder, or described mixing raw material block is put into metal capsule pipe, two ends seal; To implement the sealing to raw material, form sealing raw material;
C. the sintering of base material: sealing raw material is put into vacuum sintering furnace, or put into the process furnace being connected with shielding gas and sinter; Vacuum tightness remains on below 3Pa; The temperature schedule heated up is: 400 ~ 450 DEG C are incubated 1 ~ 2 hour, and 600 ~ 650 DEG C are incubated 1 ~ 2 hour, and 700 ~ 900 DEG C are incubated 60 ~ 120 minutes; Finally under vacuum atmosphere, naturally cool to room temperature; Finally obtain MgB2 composite superconductor.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183473A (en) * | 2019-05-23 | 2019-08-30 | 深圳先进技术研究院 | A kind of new superconduction material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074309A (en) * | 2010-11-28 | 2011-05-25 | 上海大学 | Method for preparing magnesium diboride composite superconducting material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074309A (en) * | 2010-11-28 | 2011-05-25 | 上海大学 | Method for preparing magnesium diboride composite superconducting material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183473A (en) * | 2019-05-23 | 2019-08-30 | 深圳先进技术研究院 | A kind of new superconduction material and preparation method thereof |
| CN110183473B (en) * | 2019-05-23 | 2021-09-14 | 深圳先进技术研究院 | Novel superconducting material and preparation method thereof |
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Application publication date: 20151104 |