CN107903066A - A kind of bismuth sulfenyl superconductor and preparation method thereof - Google Patents

A kind of bismuth sulfenyl superconductor and preparation method thereof Download PDF

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CN107903066A
CN107903066A CN201711245901.7A CN201711245901A CN107903066A CN 107903066 A CN107903066 A CN 107903066A CN 201711245901 A CN201711245901 A CN 201711245901A CN 107903066 A CN107903066 A CN 107903066A
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superconductor
sulfenyl
bismuth
obis
mixture
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陈永亮
崔雅静
王瑞龙
苏宇峰
赵勇
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Southwest Jiaotong University
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Abstract

A kind of bismuth sulfenyl superconductor and preparation method thereof.The molecular formula of this kind of bismuth sulfenyl superconductor is La1‑xTaxOBiS2, 0.05≤x≤0.25.Its preparation method is：A, by La2S3、Bi2S3、Bi2O3, Ta and S, according to La1‑xTaxOBiS2Stoichiometric ratio weigh, then ground and mixed obtains raw mixture；B, raw mixture and fluxing agent CsCl are pressed 1：4~10 mass ratio uniformly mixes, and obtains raw material flux mixture；C, raw material flux mixture is sealed in vitreosil pipe, when 900~1000 DEG C of sintering 8~12 are small；600~800 DEG C are cooled to 0.5 DEG C~1 DEG C/h of speed, furnace cooling；With deionized water rinsing 10~20 times, finally 50~100 DEG C it is dry 20~30 it is small when, to obtain the final product.The superconductivity of this kind of bismuth sulfenyl superconductor is stablized, and prepares simple.

Description

A kind of bismuth sulfenyl superconductor and preparation method thereof
Technical field
The present invention relates to a kind of bismuth sulfenyl superconductor and preparation method thereof.
Background technology
Superconductor has wide application sky because of its own two big fundamental characteristics of perfect diamganetism and zero resistance Between, thus people constantly explore new superconductor and application.In addition, the generation mechanism of superconductivity is still uncertain, it is new super The discovery of conductor contributes to open research, developing thought.Since superconductivity is found, the exploration work of new superconductive material from It was not interrupted, great breakthrough occurred in 1986, and copper-based oxide high temperature superconductor is found, after effort for many years, Existing commercialized product comes out.2008, it was found that a new class of high temperature superconducting materia --- iron-based superconductor, since it contains There is this magnetic element of iron and attract wide attention.Compared with high-temperature superconductor, cryogenic superconductor due to its prepare it is easy, super Steady performance is led, applied to (such as nuclear magnetic resonance) on many precision instruments.Research, the more new low temperature of exploitation Superconductor, helps to promote the further investigation and extensive use of low-temperature superconducting technology.
The content of the invention
It is an object of the invention to provide a kind of new bismuth sulfenyl superconductor, the superconductivity of this kind of bismuth sulfenyl superconductor are steady It is fixed, prepare simple.
The present invention realizes its goal of the invention, and used technical solution is：A kind of bismuth sulfenyl superconductor, its molecular formula are La1-xTaxOBiS2, 0.05≤x≤0.25.
Compared with prior art, the beneficial effects of the invention are as follows：
The bismuth sulfenyl superconductor of the present invention, its fertile material system is LaOBiS2.Wherein crystal structure by La-O layers and Bi-S layers of alternating accumulation form, and La-O layers are current-carrying word bank layers, and Bi-S layers are conductive layers.The present invention successfully uses Ta5+Ion portion Divide the La in substitution current-carrying word bank layer3+Ion, due to Ta5+Ion ratio La3+Chemical valence height+divalent, use Ta5+Ionic portions substitute La3+When, to LaOBiS2More electronics are filled with system, increase electron concentration, and can be by adjusting the incorporation of Ta To adjust La1-xTaxOBiS2The concentration of electronic carrier in superconductor, so as to change La1-xTaxOBiS2The superconductivity of superconductor Energy.
X-ray diffraction the result shows that, bismuth sulfenyl superconductor of the invention has tetragonal structure, and single phase property is preferable.
Electromagnetic performance measurement result shows, below superconducting transition temperature, it was observed that obvious zero-resistance phenomenon, and have There is good diamagnetic performance.And its superconducting transition temperature is up to 3.3K.
Second object of the present invention is to provide the preparation method of above-mentioned bismuth sulfenyl superconductor.
The present invention realizes its second goal of the invention, and used technical solution is：It is a kind of to prepare described in claim 1 The method of bismuth sulfenyl superconductor, its practice are：
A, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La1-xTaxOBiS2, the change of 0.05≤x≤0.25 Learn metering than weigh, then ground and mixed it is uniform raw mixture；
B, raw mixture and fluxing agent CsCl are pressed 1：4~10 mass ratio uniformly mixes, and obtains raw material-fluxing agent mixing Thing；
C, raw material-flux mixture is sealed in vitreosil pipe, when 900~1000 DEG C of sintering 8~12 are small；Then 600~800 DEG C are cooled to 0.5 DEG C~1 DEG C/h of cooling rate, cools to room temperature with the furnace afterwards；After getting rid of quartz ampoule With deionized water rinsing 10~20 times to remove CsCl, finally by resulting materials 50~100 DEG C it is dry 20~30 it is small when, i.e., .
The preparation method of the present invention is simple, easy to implement, and obtained bismuth sulfenyl superconductor La1-xTaxOBiS2For monocrystalline Body, superconductivity are stablized.
Further, the operation of the step A in preparation method of the present invention and the operation of step B, under argon atmosphere Carry out.
In this way, the oxidation of raw material can be prevented, further ensure that the amount of oxygen in obtained thing by the amount of oxygen in raw material Lai accurate Control, ensures that the superconductivity of thing is made.
The present invention is further described with specific embodiment below in conjunction with the accompanying drawings.
Brief description of the drawings
Fig. 1 is bismuth sulfenyl superconductor La prepared by the embodiment of the present invention one0.93Ta0.07OBiS2Magnetization curve.Wherein, mark The curve noted as ZFC is the magnetization curve cooled down under no magnetic field environment；The curve for being labeled as FC is the magnetic cooled down under magnetic field environment Change curve；Its ordinate is magnetic moment (Moment), and unit is electromagnetism unit emu/g；Abscissa is temperature, unit K (Kelvin)。.
Fig. 2 is bismuth sulfenyl superconductor La prepared by the embodiment of the present invention one0.93Ta0.07OBiS2Resistivity with temperature change Change curve.Wherein：Ordinate is resistivity (Resistivity), and unit is m Ω cm；Abscissa is temperature, unit K (Kelvin)。
Fig. 3 is bismuth sulfenyl superconductor La prepared by the embodiment of the present invention one0.93Ta0.07OBiS2X ray diffracting spectrum.Its In：Ordinate is diffracted intensity, unit counts；Abscissa is 2 θ of the angle of diffraction, and unit is degree (deg).
Embodiment
Embodiment one
A kind of bismuth sulfenyl superconductor, its molecular formula are La0.93Ta0.07OBiS2(namely its molecular formula is La1-xTaxOBiS2, x =0.07).
A kind of method for the bismuth sulfenyl superconductor for preparing this example, its practice are：
A, under argon atmosphere, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La0.93Ta0.07OBiS2Stoichiometric ratio weigh, then ground and mixed it is uniform raw mixture；
B, under argon atmosphere, raw mixture and fluxing agent CsCl are pressed 1：5 mass ratio uniformly mixes, and obtains former Material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 900 DEG C of sintering 10 are small；Then with 1 DEG C/it is small When cooling rate be cooled to 600 DEG C, cool to room temperature with the furnace afterwards；Get rid of after quartz ampoule with deionized water rinsing 10 times with Remove CsCl, finally by resulting materials when 50 DEG C of dryings 30 are small, to obtain the final product.
Fig. 1 is bismuth sulfenyl superconductor La made from the example method0.93Ta0.07OBiS2Magnetization curve.As seen from Figure 1, its Superconducting transition temperature is 3.3K, and below superconducting transition temperature, its diamagnetic performance is good；
Fig. 2 is the bismuth sulfenyl superconductor La made from the example method0.93Ta0.07OBiS2Resistivity variation with temperature it is bent Line.Zero-resistance phenomenon can clearly be observed by Fig. 2；
Fig. 3 is the bismuth sulfenyl superconductor La made from the example method0.93Ta0.07OBiS2X ray diffracting spectrum, by Fig. 3 Understand obtained La0.93Ta0.07OBiS2New superconductors is monocrystal, and monocrystal is grown along c directions, has corner stratiform knot Structure.
Above test result explanation, the bismuth sulfenyl superconductor La of this example1-xTaxOBiS2With good superconductivity, and The growth of monocrystal is simple and practicable.
Embodiment two
A kind of bismuth sulfenyl superconductor, its molecular formula are La0.95Ta0.05OBiS2(namely its molecular formula is La1-xTaxOBiS2, x =0.05).
A kind of method for the bismuth sulfenyl superconductor for preparing this example, its practice are：
A, under argon atmosphere, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La0.95Ta0.05OBiS2Stoichiometric ratio weigh, then ground and mixed it is uniform raw mixture；
B, under argon atmosphere, raw mixture and fluxing agent CsCl are pressed 1：4 mass ratio uniformly mixes, and obtains former Material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 950 DEG C of sintering 8 are small；Then with 0.5 DEG C/it is small When cooling rate be cooled to 650 DEG C, cool to room temperature with the furnace afterwards；Get rid of after quartz ampoule with deionized water rinsing 15 times with Remove CsCl, finally by resulting materials when 60 DEG C of dryings 20 are small, to obtain the final product.
Bismuth sulfenyl superconductor La made from this example0.95Ta0.05OBiS2, it is 2.1K that experiment, which measures its superconducting transition temperature,.
Embodiment three
A kind of bismuth sulfenyl superconductor, its molecular formula are La0.9Ta0.1OBiS2(namely its molecular formula is La1-xTaxOBiS2, x =0.1).
A kind of method for the bismuth sulfenyl superconductor for preparing this example, its practice are：
A, under argon atmosphere, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La0.9Ta0.1OBiS2Stoichiometric ratio weigh, then ground and mixed it is uniform raw mixture；
B, under argon atmosphere, raw mixture and fluxing agent CsCl are pressed 1：7 mass ratio uniformly mixes, and obtains former Material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 1000 DEG C of sintering 8 are small；Then with 0.7 DEG C/ The cooling rate of hour is cooled to 700 DEG C, cools to room temperature with the furnace afterwards；Deionized water rinsing is used after getting rid of quartz ampoule 20 times To remove CsCl, finally by resulting materials when 60 DEG C of dryings 20 are small, to obtain the final product.
Bismuth sulfenyl superconductor La made from this example0.9Ta0.1OBiS2, it is 3.3K that experiment, which measures its superconducting transition temperature,.
Example IV
A kind of bismuth sulfenyl superconductor, its molecular formula are La0.88Ta0.12OBiS2(namely its molecular formula is i.e. La1- xTaxOBiS2, x=0.12).
A kind of method for the bismuth sulfenyl superconductor for preparing this example, its practice are：
A, under argon atmosphere, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La0.88Ta0.12OBiS2Stoichiometric ratio weigh, then ground and mixed it is uniform raw mixture；
B, under argon atmosphere, raw mixture and fluxing agent CsCl are pressed 1：10 mass ratio uniformly mixes, and obtains Raw material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 900 DEG C of sintering 12 are small；Then with 0.5 DEG C/ The cooling rate of hour is cooled to 600 DEG C, cools to room temperature with the furnace afterwards；Deionized water rinsing is used after getting rid of quartz ampoule 10 times To remove CsCl, finally by resulting materials when 50 DEG C of dryings 22 are small, to obtain the final product.
Bismuth sulfenyl superconductor La made from this example0.88Ta0.12OBiS2, it is 3.2K that experiment, which measures its superconducting transition temperature,.
Embodiment five
A kind of bismuth sulfenyl superconductor, its molecular formula are La0.85Ta0.15OBiS2(namely its molecular formula is La1-xTaxOBiS2, x =0.15).
A kind of method for the bismuth sulfenyl superconductor for preparing this example, its practice are：
A, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La0.85Ta0.15OBiS2Stoichiometric ratio claim Amount, then ground and mixed it is uniform raw mixture；
B, raw mixture and fluxing agent CsCl are pressed 1：8 mass ratio uniformly mixes, and obtains raw material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 950 DEG C of sintering 12 are small；Then with 0.8 DEG C/ The cooling rate of hour is cooled to 700 DEG C, cools to room temperature with the furnace afterwards；Deionized water rinsing is used after getting rid of quartz ampoule 18 times To remove CsCl, finally by resulting materials when 60 DEG C of dryings 25 are small, to obtain the final product.
Bismuth sulfenyl superconductor La made from this example0.85Ta0.15OBiS2, it is 3.1K that experiment, which measures its superconducting transition temperature,.
Embodiment six
A kind of bismuth sulfenyl superconductor, its molecular formula are La0.8Ta0.2OBiS2(namely its molecular formula is La1-xTaxOBiS2, x =0.2).
A kind of method for the bismuth sulfenyl superconductor for preparing this example, its practice are：
A, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La0.8Ta0.2OBiS2Stoichiometric ratio claim Amount, then ground and mixed it is uniform raw mixture；
B, raw mixture and fluxing agent CsCl are pressed 1：4 mass ratio uniformly mixes, and obtains raw material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 1000 DEG C of sintering 8 are small；Then with 1 DEG C/it is small When cooling rate be cooled to 800 DEG C, cool to room temperature with the furnace afterwards；Get rid of after quartz ampoule with deionized water rinsing 20 times with Remove CsCl, finally by resulting materials when 80 DEG C of dryings 20 are small, to obtain the final product.
Bismuth sulfenyl superconductor La made from this example0.85Ta0.15OBiS2, it is 3K that experiment, which measures its superconducting transition temperature,.
Embodiment seven
A kind of bismuth sulfenyl superconductor, its molecular formula are La0.75Ta0.25OBiS2(namely its molecular formula is La1-xTaxOBiS2, x =0.25).
A kind of method for the bismuth sulfenyl superconductor for preparing this example, its practice are：
A, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La0.75Ta0.25OBiS2Stoichiometric ratio claim Amount, then ground and mixed it is uniform raw mixture；
B, raw mixture and fluxing agent CsCl are pressed 1：10 mass ratio uniformly mixes, and obtains raw material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 900 DEG C of sintering 10 are small；Then with 0.5 DEG C/ The cooling rate of hour is cooled to 600 DEG C, cools to room temperature with the furnace afterwards；Deionized water rinsing is used after getting rid of quartz ampoule 15 times To remove CsCl, finally by resulting materials when 50 DEG C of dryings 30 are small, to obtain the final product.
Bismuth sulfenyl superconductor La made from this example0.75Ta0.25OBiS2, it is 2.9K that experiment, which measures its superconducting transition temperature,.

Claims (3)

1. a kind of bismuth sulfenyl superconductor, its molecular formula is La1-xTaxOBiS2, wherein 0.05≤x≤0.25.
2. a kind of method of the bismuth sulfenyl superconductor prepared described in claim 1, its practice are：
A, by La2S3、Bi2S3、Bi2O3, Ta and S totally five kinds of materials, according to La1-xTaxOBiS2, the chemistry meter of 0.05≤x≤0.25 Amount than weigh, then ground and mixed it is uniform raw mixture；
B, raw mixture and fluxing agent CsCl are pressed 1：4~10 mass ratio uniformly mixes, and obtains raw material-flux mixture；
C, raw material-flux mixture is sealed in vitreosil pipe, when 900~1000 DEG C of sintering 8~12 are small；Then with 0.5 DEG C~1 DEG C/h of cooling rate is cooled to 600~800 DEG C, cools to room temperature with the furnace afterwards；Used after getting rid of quartz ampoule Deionized water rinsing 10~20 times to remove CsCl, finally by resulting materials 50~100 DEG C it is dry 20~30 it is small when, to obtain the final product.
A kind of 3. method for preparing bismuth sulfenyl superconductor as claimed in claim 2, it is characterised in that：The behaviour of the step A Make the operation with step B, carried out under argon atmosphere.
CN201711245901.7A 2017-12-01 2017-12-01 A kind of bismuth sulfenyl superconductor and preparation method thereof Pending CN107903066A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109576773A (en) * 2019-01-08 2019-04-05 西南交通大学 Bismuth sulfenyl superconductive monocrystal and preparation method thereof

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CN101456736A (en) * 2009-01-05 2009-06-17 西南交通大学 Iridium doped iron base superconductor and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN88100501A (en) * 1987-01-30 1988-08-10 株式会社日立制作所 Oxide superconductor
CN101061555A (en) * 2005-04-06 2007-10-24 住友电气工业株式会社 Process for producing bismuth-based oxide superconductor, and superconductive wire
CN101456736A (en) * 2009-01-05 2009-06-17 西南交通大学 Iridium doped iron base superconductor and preparation method thereof

Non-Patent Citations (1)

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Title
王瑞龙: "La1-xTaxOBiS2超导体单晶生长及超导性能研究", 《中国优秀硕士学位论文全文数据库 工程科技II辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109576773A (en) * 2019-01-08 2019-04-05 西南交通大学 Bismuth sulfenyl superconductive monocrystal and preparation method thereof

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