Low-temperature hydrothermally synthesized organic phosphonic acid lithium battery anode material LixMmR(PO3)n

A technology of organic phosphonic acid and hydrothermal synthesis, which is applied in battery electrodes, electrode manufacturing, circuits, etc., can solve the problems of lack of controllable composition and structure design, and achieve the effects of optimized charge and discharge performance, low cost, and high product yield

Inactive Publication Date: 2010-06-16

NANJING UNIV

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Problems solved by technology

However, the synthesis of the above-mentioned materials is basically carried out by solid-state reaction under high tem...

Abstract

The invention relates to a low-temperature hydrothermally synthesized organic phosphonic acid lithium battery anode material, and discloses a novel metal organic phosphonic acid lithium coordination compound with a composition of LixMmR(PO3)n (wherein R=an organic group, and M=a transition metal ion) as the lithium battery anode material, and the regulation and control of the composition structure of the material can be realized through changing the organic group R to optimize the deinsertion of a lithium ion in the anode material. A preparation method adopts a low-cost low-temperature low-pressure hydrothermal synthesis technology and has high yield and high purity. A phosphonic acid lithium-rhodium complex with a three-dimensional channel structure is obtained. The discharge capacity of the material for the first time reaches 82.73mAh/g, and the specific capacity is still kept at about 82mAh/g after charge and discharge for 20 times and hardly descends, which indicates that the material synthesized by the method has better charge and discharge stability.

Application Domain

Electrode manufacturing processes

Technology Topic

Charge and dischargeHydrothermal synthesis +8

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[0022] Example 1, Li 2 [Rh 2 (CH 3 C(OH)(PO 3 H 0.5 ) 2 ) 2 ]·4H 2 Synthesis of O

[0023] RhCl 3 ·3H 2 O 2.5723g (9.77mmol), 1-hydroxyethyl diphosphonic acid CH 3 C(OH)(PO 3 H 2 ) 2 ·H 2 Mix O6.5654g (29.30mmol) with 40mL water, adjust the pH of the solution to 3.30 with 1M LiOH, stir at room temperature for 2 hours, put the solution into a polytetrafluoroethylene lined reactor and seal, program the temperature to 140°C, and react at a constant temperature 3. Day, the program was cooled to room temperature, filtered, washed with deionized water, ethanol, and acetone, and dried in vacuo to obtain 3.2673 g of pure green needle-like crystals with a yield of 95.9% (based on Rh). Chemical formula C 4 H 18 O 18 P 4 Li 2 Rh 2 , Elemental analysis (%) calculated value: C, 6.88; H, 2.60; measured value: C: 5.70; H, 2.56.

[0024] Infrared spectrum IR (KBr, cm -1 ): 3508(s), 3419(br,s), 3216(br,s), 2947(m), 1655(s), 1457(m), 1370(s), 1155(vs), 1135(vs) , 1072(vs), 1016(vs), 971(vs), 927(vs), 810(s), 724(m), 653(w), 593(vs), 551(m), 500(s) , 479(s).

[0025] Crystal structure parameters: asymmetric unit chemical formula C 2 H 9 O 9 P 2 LiRh; crystal system Monoclinic; space group P2 1 /c; β=105.23(4)°; Z=4; F(000) value 684; GOF value 1.014; R 1 =0.0598, wR 2 =0.1294[I>2σ(I)]; R 1 = 0.0885, wR 2 =0.1374[all data];

[0026] Li 2 [Rh 2 (CH 3 C(OH)(PO 3 H 0.5 ) 2 ) 2 ]·4H 2 For the first charge-discharge curve of O material, the charge plateau appears at 0.48V and the discharge plateau appears at 0.23V. The appearance of the platform corresponds to the phase change of the material during the charge and discharge process. It can also be seen that between 1.5V and 0V, the lithium insertion and removal of the material are carried out in one step, so the insertion and removal of lithium Only a stable voltage platform appears.

[0027] The discharge capacity of the material reached 82.73mAh/g for the first time, and after the 20th time, the specific capacity remained around 82mAh/g, with almost no drop. This indicates that the cathode material RhLi synthesized by this method has better charge and discharge stability.

Example Embodiment

[0028] Example 2, Li 3 [Ru 2 (CH 3 C(OH)(PO 3 ) 2 ) 2 ]·2H 2 Synthesis of O

[0029] RuCl 3 ·3.5H 2 O 0.1015g (0.38mmol), 1-hydroxyethyl diphosphonic acid CH 3 C(OH)(PO 3 H 2 ) 2 ·H 2 O0.3367g (1.50mmol) was mixed in 4mL water, adjusted to pH=4.70 with 1M LiOH, the mixture was put into a stainless steel reactor lined with polytetrafluoroethylene, the temperature was programmed to 160℃, the temperature was reacted for 4 days, and the temperature was cooled by program To room temperature, filter, wash with deionized water, ethanol, acetone, and vacuum dry to obtain 0.120 g of reddish brown fibrous crystals with a yield of 95% (based on Ru). Chemical formula C 4 H 12 O 16 P 4 Li 3 Ru 2 Elemental analysis (%) measured value: C, 7.10; H, 1.95; theoretical value: C, 7.25; H, 1.82%.

[0030] Infrared spectrum IR (KBr, cm -1 ): 3418(s), 1647(s), 1457(w), 1370(w), 1144(s), 1067(m), 975(s), 915(m), 819(w), 587(s) ), 492(m).

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Improve charge and discharge performance
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Low-temperature hydrothermally synthesized organic phosphonic acid lithium battery anode material LixMmR(PO3)n

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