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Preparation method and application of orthorhombic two-dimensional layered sip single crystal and thin film

A two-dimensional layered, single crystal thin film technology, used in 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: 2018-10-16
SHANDONG UNIV
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  • Summary
  • 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 two-dimensional layered sip single crystal and thin film
  • Preparation method and application of orthorhombic two-dimensional layered sip single crystal and thin film
  • Preparation method and application of orthorhombic two-dimensional layered sip single crystal and thin film

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Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0021] (2) Put the quartz tube into a heating furnace, and adopt a stepwise heating program. Firstly, the temperature is raised to 400 in 10 hours, and the temperature is kept for 50 hours; then the temperature is raised to 1100 in 20 hours, and the temperature is kept for 30 hours, so that Si and P are fully compounded and reacted;

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

[0023] (4)...

Embodiment 2

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

[0028] (2) Put the quartz tube into a heating furnace, and adopt a stepwise heating program. Firstly, the temperature is raised to 600°C in 15 hours and kept at a constant temperature for 30 hours; then the temperature is raised to 1200°C in 30 hours at a constant temperature of 20, so that Si and P are fully compounded and reacted;

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

[0030] (4)...

Embodiment 3

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

[0034] (2) Put the quartz tube into a heating furnace, and adopt a stepwise heating program. First, the temperature is raised to 500°C in 12 hours, and the temperature is kept constant for 40 hours; then the temperature is raised to 1150°C in 25 hours, and the temperature is kept constant for 25 hours, so that Si and P are fully compounded.

[0035] (3) 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 gradually grows; when the furnace body temperature drops to 640°C, quickly remove the quartz tube from The furnace is taken out and turned upside down to separate the grown o-SiP single crystal from the metal flux Sn to obtain a bulk o-SiP single crystal;

[0036...

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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 orthogonal phase two-dimensional layered SiP single crystals and thin films by using a metal flux method, and its photoelectric device application, belonging to the technical field of two-dimensional layered materials and photoelectric functional device applications. Background technique [0002] The two-dimensional layered material is a type of material formed by strong covalent bonds or ionic bonds within the layers, and weak van der Waals forces between the layers. Due to the weak interaction force between the layers, the layers are easily peeled from each other, so that single-layer or multilayer two-dimensional materials can be formed. Graphene, transition metal chalcogenides (MoS 2 , MoSe 2 , WS 2 Etc.) and black phosphorous are two-dimensional layered materials that have been widely studied in recent years. Because of their excellent electrical, optical, magnetic, and mechanical properties, they are used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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