Method for preparing phosphaalkene by utilizing electrochemistry

An electrochemical and phosphorene technology, applied in circuits, electrical components, electrolysis processes, etc., can solve the problems of long time, cumbersome process, low peeling efficiency, etc., and achieve the effect of high yield and low cost

Active Publication Date: 2015-07-15
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, the main method for obtaining phosphorene with black phosphorus as raw material is mechanical exfoliation, but the stripping efficiency of this method is extremely low and the cost is high, so it cannot be used as an effective method for large-scale preparation of phosphorene; another method is Liquid phase intercalation stripping method, but this method still has many disadvantages, such as long stripping time, low yiel

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  • Method for preparing phosphaalkene by utilizing electrochemistry
  • Method for preparing phosphaalkene by utilizing electrochemistry

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0038] Positive electrode: use an area of ​​1cm 2 , a platinum sheet with a thickness of 0.2mm was used as the positive electrode. Negative electrode: Black phosphorus is directly used as the negative electrode. In a 500ml beaker, NaPF 6 Add it into ethylene carbonate to form a 1mol / L electrolyte solution, and add 0.01g of sodium lauryl sulfate thereto. The above two electrodes were placed in parallel with a distance of 2 cm. Connect the two electrodes with wires as an electrochemical device, and apply a 15V DC voltage between the two electrodes for 20 hours.

[0039]After the exfoliation process was completed, the obtained phosphorene and unexfoliated bulk phosphorus were filtered out, washed several times with ethylene carbonate, and then vacuum-dried at 150 °C to constant weight. Add 100 mg of the obtained phosphorene and unexfoliated massive phosphorus into 20 ml of ethylene carbonate for re-dispersion by ultrasonic vibration for 1 h, the ultrasonic frequency is 15 Hz,...

Embodiment 2

[0042] Positive electrode: A platinum cylinder with a diameter of 3 mm is used as the positive electrode. Negative electrode: Black phosphorus is directly used as the negative electrode. In a 500ml beaker, NaBF 4 Add it to a mixed solution of propylene carbonate and tetrahydrofuran to form a 1mol / L electrolyte, wherein the volume ratio of propylene carbonate and tetrahydrofuran is 1:1. The above two electrodes were placed in parallel with a distance of 1 cm. Connect the two electrodes with wires as an electrochemical device, and apply a 20V DC voltage between the two electrodes for 48 hours.

[0043] After the exfoliation process was completed, the obtained phosphorene and unexfoliated bulk phosphorus were filtered out, washed with propylene carbonate several times, and then vacuum-dried at 150 °C to constant weight. Add 100 mg of the obtained phosphorene and unexfoliated massive phosphorus into 20 ml of propylene carbonate for re-dispersion by ultrasonic vibration for 2 h,...

Embodiment 3

[0045] Positive electrode: use an area of ​​1cm 2 , a platinum sheet with a thickness of 0.2mm was used as the positive electrode. Negative electrode: black phosphorus and nickel foam are pressed into an area of ​​1cm by a press 2 electrode sheet and use it as the negative electrode. During the pressing process, the pressure is kept at 15t, and the time is 3min. In a 500ml beaker, the LiPF 6 Add it into a mixed solvent of propylene carbonate and acetonitrile to make a 1.5mol / L electrolyte, wherein the volume ratio of propylene carbonate and acetonitrile is 1:1. The above two electrodes were placed in parallel with a distance of 3 cm. Connect the two electrodes with wires as an electrochemical device, and apply a 2V DC voltage between the two electrodes for 2 hours. Then increase the voltage between positive and negative to 5V. After maintaining the 5V DC voltage for 2 hours, increase the voltage to 20V and continue for 15 minutes, then apply -10V DC voltage to the positi...

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Abstract

The invention discloses a method for preparing phosphaalkene by utilizing electrochemistry. The method comprises the following steps: firstly, assembling an electrolytic cell by using an inert electrode as a positive electrode and phosphorus as a negative electrode, wherein in the electrolytic cell, the electrolyte solution is one or several of an aqueous electrolyte solution, an organic electrolyte solution and an ionic liquid electrolyte solution containing the electrolyte; applying direct current or alternating current voltage between the two electrodes of the electrolytic cell and stripping the phosphorus into phosphaalkene under a function of a direct current electric field or an alternating current electric field; and performing filtration treatment to obtain a stripped product, washing the stripped product for a plurality of times by using an organic solvent, centrifugally separating and drying to obtain the required phosphaalkene. According to the method, a phosphaalkene material with good quality, high yield and low cost can be conveniently, quickly and securely produced in an environment-friendly form, and can be applied to multiple fields of secondary ion batteries, supercapacitors, solar batteries, fuel batteries, electro-catalysis, electronic elements, bioanalysis, biological sensors and the like.

Description

technical field [0001] The invention relates to the technical fields of material preparation and energy, in particular to a method for preparing phosphorene by electrochemical methods. Background technique [0002] Phosphorus has a variety of allotropes, and black phosphorus is the most stable one among the allotropes of phosphorus. It is neither soluble in organic solvents nor flammable and chemically reactive. It has a graphite-like flake structure (corrugated layered structure), is conductive, and has a maximum carrier mobility of 65,000 (graphene is 100,000) cm 2 / V.s. Few-layer phosphorene field-effect transistors fabricated so far embody 10 5 About leakage current modulation rate (this value is 10,000 times that of graphene) and good current saturation effect, the carrier mobility can reach 1000cm 2 / V.s, these properties are far superior to the current two-dimensional nanomaterials such as transition metal sulfides, so they are expected to be well applied in nanoel...

Claims

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Application Information

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IPC IPC(8): H01M4/38C25B1/00
CPCC25B1/00H01G11/30H01M4/38H01M4/90Y02E60/10Y02E60/13Y02E60/50
Inventor 崔秀国祖雷连慧琴
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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