Method for preparing iron selenium superconducting material by spark plasma sintering technology

A technology for discharging plasma and superconducting materials, which is applied in the field of preparing iron-selenium superconducting materials by ion sintering technology, can solve the problems of complicated synthesis steps, long preparation time, unfavorable large-scale preparation of superconducting FeSe materials and the like, and achieves the preparation method. Simple and fast, promote the formation of superconducting phase, and achieve the effect of large-scale preparation

Active Publication Date: 2018-10-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Chinese patent 201310288873.2, a method for increasing the superconducting transition temperature of FeSe by adding Mg, mainly reports a method for increasing the superconducting transition temperature of FeSe by adding Mg, which can increase the superconducting transition temperature of FeSe by 20%, but the patent The synthesis steps are cumbersome and the preparation time is long (>18h), which is not conducive to the large-scale preparation of superconducting FeSe materials

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  • Method for preparing iron selenium superconducting material by spark plasma sintering technology
  • Method for preparing iron selenium superconducting material by spark plasma sintering technology
  • Method for preparing iron selenium superconducting material by spark plasma sintering technology

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preparation example Construction

[0040] Such as figure 1 As shown, the specific preparation method of the superconducting iron selenium material of the present invention comprises the following steps:

[0041] (1) According to the molar ratio of 1:x, weigh 5.0g iron selenium and insulator M powder with a total weight, put them in a grinding bowl, and grind for 30 minutes to ensure that the two powders are fully mixed and evenly dispersed; the value range of x is 0.2~ 15.

[0042] (2) Conduct discharge plasma sintering on the ground powder sample: first, put the powder sample into a graphite mold with a diameter of 12.7 mm and a height of 30 mm for compaction, then wrap a layer of carbon felt on the outside of the mold, and finally put the mold into spark plasma sintering furnace. Increase the pressure to 30MPa, evacuate until the vacuum degree is less than 5Pa, and start to apply current to raise the temperature and sinter. Keep the heating rate at 50K / min~100K / min as much as possible, after about 30min th...

Embodiment 1

[0045] Superconducting (FeSe) 1 (SrTiO 3 ) x Material preparation, the specific preparation method is as follows:

[0046] (1) According to the molar ratio 1:x (x=0.2, 1, 4, 10, 15), weigh 5.0 g of iron selenium and strontium titanate powder in a mortar and grind for 30 minutes;

[0047] (2) Put the powder sample obtained in step (1) into a graphite mold with a diameter of 12.7mm, put it into a discharge plasma sintering furnace, pressurize it at 30MPa, evacuate it until the vacuum degree is less than 5Pa, and start to apply current to heat up and sinter for about 30min Raise the temperature to 1173K, keep it warm for 30 minutes, then release the pressure directly, and cool down to room temperature naturally;

[0048] (3) Put the sample obtained by sintering into a CVD tube furnace to anneal the sample, raise the temperature to 1173K at a rate of 10K / min under an argon atmosphere, keep the temperature constant for 90min, and then cool down. flow;

[0049] (4) Regarding sa...

Embodiment 2

[0052] Superconducting (FeSe) 1 (BaTiO 3 ) 1 Material preparation, the specific preparation method is as follows:

[0053] (1) Weigh 5.0 g of iron selenium and barium titanate powder according to the molar ratio of 1:1, place them in an agate mortar, and grind for 30 minutes;

[0054] (2) Put the powder sample obtained in step (1) into a graphite mold with a diameter of 12.7mm, put it into a discharge plasma sintering furnace, pressurize it at 30MPa, evacuate it until the vacuum degree is less than 5Pa, and start to apply current to heat up and sinter for about 30min Raise the temperature to 1173K, keep it warm for 30 minutes, then release the pressure directly, and cool down to room temperature naturally;

[0055] (3) Put the sample obtained by sintering into a CVD tube furnace to anneal the sample, raise the temperature to 1173K at a rate of 10K / min under an argon atmosphere, keep the temperature constant for 90min, and then cool down. flow;

[0056] (4) Regarding the s...

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Abstract

The invention discloses a method for preparing iron selenium superconducting material by spark plasma sintering technology. The chemical formula of the iron selenium superconducting material is (FeSe)1(M)x, wherein the insulator M is one or more of SrTiO3, BaTiO3 and MgO, and the molar ratio of iron selenium (FeSe) to the insulator M is 1:x. The method for preparing the material includes: solid powder mixing, spark plasma sintering (SPS) and annealing. The powder of iron selenium and the powder of the insulator M are weighed respectively according to a certain molar ratio of 1:x, after mechanically grinding and mixing for a certain time, the mixed powder is subjected to spark plasma sintering at a suitable pressure and temperature, and then the sintered sample is annealed under suitable conditions to obtain (FeSe)1(M)x material. The material has a stable superconducting performance, and the superconducting transition temperature is between 10.10K and 13.44K. The material is not sensitive to the raw material ratio, and the value of x ranges from 0.2 to 15. Meanwhile, the material has a high upper critical field which can be up to 16.6T to 26.7T. Thereby the material can be applied in the fields of electric energy, superconducting magnets, biology, medical technology, communication, and microelectronics.

Description

technical field [0001] The invention relates to a method for preparing an iron-selenium superconducting material by a discharge plasma sintering technology, and belongs to the field of superconducting material preparation. Background technique [0002] The most useful property of superconductors is zero resistance. Using them to transmit electricity will greatly reduce heat loss and save energy. According to statistics, about 15% of the electric energy loss is on the transmission line when using copper or aluminum wires for power transmission. In China alone, the annual power loss caused by this is more than 100 billion kWh. If it is changed to superconducting wires for power transmission, the energy saved is equivalent to building dozens of large power plants. With the increase of power demand and the increasing pressure of environmental protection, the development of high-temperature superconducting DC transmission cables is imminent, and the most important parameter limi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01B12/00H01B13/00
CPCH01B12/00H01B13/00Y02E40/60
Inventor 姜鹏张慧敏孟庆龙包信和
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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