Potassium-doped phenanthrene molecular crystal and preparation method thereof

A technology of molecular crystal and potassium doping is applied in the field of potassium doped phenanthrene molecular crystal and its preparation, so as to achieve the effect of increasing the length of the c-axis and increasing the critical temperature of superconductivity

Inactive Publication Date: 2017-08-11
HUBEI UNIV
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Problems solved by technology

However, the X-ray diffraction spectrum of the potassium-doped phenanthrene crystal material obtained by their preparation method did not show a peak position shift relative to the undoped phenanthrene, indicating that the doping of potassium atoms in the phenanthrene did not cause changes in the molecular crystal structure. significantly changed

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  • Potassium-doped phenanthrene molecular crystal and preparation method thereof
  • Potassium-doped phenanthrene molecular crystal and preparation method thereof
  • Potassium-doped phenanthrene molecular crystal and preparation method thereof

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preparation example Construction

[0018] The second aspect of the present invention provides a kind of preparation method of potassium-doped phenanthrene molecular crystal, which comprises the following steps:

[0019] A. powdery phenanthrene is mixed with potassium element;

[0020] B. When the vacuum degree is lower than 5x10 -4 Potassium-doped phenanthrene molecular crystals are obtained by annealing under the condition that Pa, water and oxygen contents are respectively lower than 0.1ppm, the annealing condition is 160°C-210°C, and the cooling rate is lower than 3°C / hour.

[0021] Preferably, the molar ratio of the phenanthrene molecule to the potassium atom is 1:2-4.

[0022] Preferably, the degree of vacuum in step B is 1×10 -4 ~5x10 -4 Pa, the water content is 0.001-0.1ppm.

[0023] Preferably, the cooling rate in step B is 1-3°C / hour.

[0024] Preferably, the annealing condition in the step B is to keep the temperature at high temperature for 24-48 hours, and then lower the temperature to 25-60°C....

Embodiment 1

[0027] In a glove box with a water content lower than 0.1ppm, the white powder phenanthrene and bright white potassium were weighed and mixed in a molar ratio of 1:3, and packed into a quartz tube.

[0028] Pull high vacuum to 1x10 on the quartz tube containing the sample -4 Pa, seal the quartz tube while vacuuming, so that the sample is sealed in the quartz tube.

[0029] Take part of the sealed quartz tube, marked as a, and put it into a high vacuum annealing furnace. The annealing conditions are heating to 200°C for 40 minutes, constant temperature for 24 hours, and cooling to 50°C in an ice bath. Take the sample out of the quartz tube and put it into the glove box to obtain potassium-doped phenanthrene molecular crystals;

[0030] Take part of the sealed quartz tube, marked as b, and put it into a high vacuum annealing furnace. The annealing conditions are heating to 200°C for 40 minutes, constant temperature for 24 hours, and cooling to 50°C at 5°C / h. Take the sample ou...

Embodiment 2

[0034] In a glove box with a water content of 0.1ppm, weigh and mix the white powder phenanthrene and bright white potassium at a molar ratio of 1:2.5, put them into a quartz tube, and mark the corresponding sample as a;

[0035] In a glove box with a water content of 0.1ppm, weigh and mix the white powder phenanthrene and bright white potassium at a molar ratio of 1:3.0, put them into a quartz tube, and mark the corresponding sample as b;

[0036] In a glove box with a water content of 0.1ppm, weigh and mix the white powder phenanthrene and bright white potassium in a molar ratio of 1:3.5, put them into a quartz tube, and mark the corresponding sample as c;

[0037] In a glove box with a water content of 0.1ppm, weigh and mix the white powder phenanthrene and bright white potassium at a molar ratio of 1:4.0, and put them into a quartz tube. The corresponding sample is marked as d.

[0038] Apply a high vacuum to the quartz tube containing the sample to 10 -4 Pa, seal the qua...

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Abstract

The invention provides a potassium-doped phenanthrene molecular crystal and a preparation method thereof. In the first aspect, the preparation method comprises the following steps: annealing under high-vacuum, anhydrous and anaerobic conditions, and controlling the annealing temperature and cooling rate to ensure that potassium atoms can be effectively doped into phenanthrene molecular crystal layers and among the phenanthrene molecular crystal layers, the c-axis length of a phenanthrene molecular crystal can be increased, and a high-quality crystal material with very good [001] oriented growth can be obtained; in the second aspect, the production of impurities such as potassium hydride can be effectively inhibited by controlling the annealing temperature and cooling rate, the high-purity potassium-doped phenanthrene molecular crystal can be obtained, and superconducting fractions of materials can be increased; and in the third aspect, the potassium atoms can be synchronously doped into the phenanthrene molecular crystal layers and among the phenanthrene molecular crystal layers so as to ensure that phenanthrene can be transformed into a stable metal state from a semiconductor state, and the superconduction critical temperature can be increased.

Description

technical field [0001] The invention relates to the field of organic superconducting materials, in particular to a potassium-doped phenanthrene molecular crystal and a preparation method thereof. Background technique [0002] In a matrix material, a small amount of other elements or compounds are added to make the matrix material produce specific electrical, magnetic and optical properties, so that it has practical application value or specific use. Potassium, as a dopant, was used to dope C60 as early as 1991 to obtain an organic compound superconductor with a superconducting transition temperature of 18K [Hebard, A.F. et al. Superconductivity at 18 K in potassium-doped C60. Nature 350, 600–601( 1991).].]. In 2010, Yoshihiro Kubozono and Ryoji Mitsuhashi of Okayama University in Japan discovered superconductivity by doping perinaphine with alkali metal [Mitsuhashi, R. et al. Superconductivity in alkali-metal-doped picene. Nature 464, 76–79( 2010).], the organic supercondu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C15/30
CPCC30B1/02C30B29/54
Inventor 高云王仁树闫循旺邬小林黄忠兵
Owner HUBEI UNIV
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