Preparation method and application of orthorhombic-phase two-dimensional layered SiP single crystal and film

A two-dimensional layered, orthorhombic phase technology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of small crystal size and poor quality, and achieve high pulse peak power and pulse energy Effect

Active Publication Date: 2016-11-16
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The o-SiP compound was first discovered on the surface of heavily phosphorus-doped single crystal silicon. Researchers can also prepare o-SiP on the surface of single crystal silicon by the gas phase method. Recently, due to its two-dimensional layered structure, it has caused People's research interest, o-SiP was successfully obtained by high-pressure melt method and chemical vapor transport (CVT), but the crystal size obtained was small and the quality was poor

Method used

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  • Preparation method and application of orthorhombic-phase two-dimensional layered SiP single crystal and film
  • Preparation method and application of orthorhombic-phase two-dimensional layered SiP single crystal and film
  • Preparation method and application of orthorhombic-phase two-dimensional layered SiP single crystal and film

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Effect test

Embodiment 1

[0020] (1) Weigh Si, P and Sn according to the ratio of molar ratio Si:P:Sn=1:1:4, Sn is used as metal flux, then put the three kinds of raw materials into the quartz tube, sinter and seal the tube after vacuuming ;

[0021] (2) Put the quartz tube into the heating furnace, adopt a staged heating program, first heat up to 400 in 10 hours, and keep the temperature at a constant temperature for 50 hours; then heat up to 1100 in 20 hours, and keep the temperature at a constant temperature for 30 hours, so that Si and P can fully react;

[0022] (3) The growth furnace is controlled by a precision temperature controller to cool down slowly at a rate of 0.1°C / hour. During this process, o-SiP nucleates and grows gradually; when the temperature of the furnace body drops to 600°C, quickly remove the quartz tube from The furnace is taken out and inverted to separate the grown o-SiP single crystal from the metal flux Sn to obtain a bulk o-SiP single crystal;

[0023] (4) Open the quartz...

Embodiment 2

[0027] (1) Weigh Si, P and Sn according to the ratio of molar ratio Si:P:Sn=1:1.1:6, Sn is used as metal flux, then put the three kinds of raw materials into the quartz tube, sinter and seal the tube after vacuuming ;

[0028] (2) Put the quartz tube into the heating furnace, adopt a staged heating program, first raise the temperature to 600°C in 15 hours, and keep the temperature for 30 hours; then raise the temperature to 1200°C in 30 hours, keep the temperature at 20°C, so that Si and P can fully react;

[0029] (3) The growth furnace is controlled by a precision temperature controller to cool down slowly at a rate of 1°C / hour. During this process, o-SiP nucleates and grows gradually; when the temperature of the furnace body drops to 700°C, quickly remove the quartz tube from The furnace is taken out and inverted to separate the grown o-SiP single crystal from the metal flux Sn to obtain a bulk o-SiP single crystal;

[0030] (4) Open the quartz tube to take out the block, ...

Embodiment 3

[0033] (1) Weigh Si, P and Sn according to the ratio of molar ratio Si:P:Sn=1:1.1:8, Sn is used as metal flux, then put the three kinds of raw materials into the quartz tube, sinter and seal the tube after vacuuming ;

[0034] (2) Put the quartz tube into the heating furnace, adopt a step-by-step heating program, first raise the temperature to 500°C in 12 hours, and keep the temperature at a constant temperature for 40 hours; then raise the temperature to 1150°C in 25 hours, and keep the temperature at a constant temperature for 25 hours, so that Si and P can fully react;

[0035] (3) The temperature of the growth furnace is controlled by a precision temperature controller to slowly cool down at a rate of 7°C / hour. During this process, o-SiP nucleates and grows gradually; when the temperature of the furnace body drops to 640°C, quickly remove the quartz tube from The furnace is taken out and inverted to separate the grown o-SiP single crystal from the metal flux Sn to obtain a...

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Abstract

The invention discloses a preparation method and application of an orthorhombic-phase two-dimensional layered SiP single crystal and a film. The method comprises the following steps that 1, Si, P and Sn are weighed, Sn serves as a metal fluxing agent, then the three raw materials are put in a quartz tube, and after the quartz tube is vacuumized, sintering is conducted for sealing the quartz tube; 2, the quartz tube is put in a heating furnace, a stage temperature rise program is adopted, and Si and P are in a sufficient combination reaction; 3, after o-SiP nucleates and grows, the quartz tube is taken out of a hearth and inverted, and an o-SiP single crystal and the metal fluxing agent Sn are separated; 4, the quartz tube is opened, the material block is taken out, the fluxing agent Sn adhering to the surface of o-SiP is removed, the material block is cleaned up, and a flaky o-SiP crystal is obtained; 5, the o-SiP crystal is immersed in an NaoH solution, sediment is extracted out after ultrasonic treatment, and the sediment is cleaned to obtain the orthorhombic-phase two-dimensional layered SiP single-crystal nano-film with a large size and high quality. The film can be applied to a saturable absorber for modulation of lasers and can be used for passive mode locking of an ultrashort pulse laser and manufacturing of photoelectronic devices or radiation detectors or solar cells.

Description

technical field [0001] The invention relates to a method for growing an orthogonal two-dimensional layered SiP single crystal and thin film by using a metal flux method, and the application of the photoelectric device, belonging to the technical field of application of two-dimensional layered materials and photoelectric functional devices. Background technique [0002] Two-dimensional layered material is a kind of material formed by strong covalent bonds or ionic bonds in the layer, and weak van der Waals force between layers. Due to the weak interaction force between the layers, the layers are easily peeled off from each other, so that single-layer or multi-layer 2D materials can be formed. Graphene, transition metal chalcogenides (MoS 2 、MoSe 2 、WS 2 etc.) and black phosphorus are two-dimensional layered materials that have been widely studied in recent years. Due to their excellent electrical, optical, magnetic, and mechanical properties, they are widely used in new-ge...

Claims

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Application Information

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IPC IPC(8): C30B29/10C30B9/10C30B29/64
CPCC30B9/10C30B29/10C30B29/64
Inventor 王善朋陶绪堂李春龙于童童
Owner SHANDONG UNIV
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