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Method and equipment for synthesizing polycrystal of phosphor, germanium and zinc

A synthesis method and polycrystalline technology are applied in the field of preparation of ternary compound semiconductor materials, which can solve the problems of high vapor pressure, explosion of crucibles, inability to meet the requirements of ZGP single crystal growth and device fabrication, etc. control effect

Inactive Publication Date: 2009-06-03
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in ZnGeP 2 In the process of polycrystalline synthesis, due to the high vapor pressure of P and Zn (P is 12.1 atm at 530°C; Zn is 4 atm at 1030°C), it is very easy to cause the crucible to explode and produce flammable and highly toxic white phosphorus; Zn and P The hot vapor will form binary Zn with high melting point 2 P 3 and ZnP 2 Inclusions etc.
All of these restrict the high-purity single-phase ZnGeP 2 The acquisition of polycrystals makes it unable to meet the requirements of ZGP single crystal growth and device fabrication

Method used

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  • Method and equipment for synthesizing polycrystal of phosphor, germanium and zinc
  • Method and equipment for synthesizing polycrystal of phosphor, germanium and zinc
  • Method and equipment for synthesizing polycrystal of phosphor, germanium and zinc

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Crucible for synthesis

[0034] In this embodiment, the shape and structure of the crucible for synthesis are shown in Figure 1, which consists of a main body 1 and a feeding tube 2. The main body 1 is a quartz glass tube with an inner diameter of 28 mm and a length of 400 mm and closed at both ends. One end is A, The other end is B, a groove is arranged at a length of 45mm from the end of the body B, the length y of the groove is 25mm, the depth h is 1 / 2 of the inner diameter d, and the feed pipe 2 intersects at a distance of In the section with a length of 45mm at the end of the B end of the body, the feed port 3 is opposite to the groove notch, the angle β between the axis and the axis of the body is 60°, and the material is quartz glass.

Embodiment 2

[0035] Example 2: Two-temperature zone tube furnace for synthesis

[0036]In this embodiment, the structure of the two-temperature zone tube furnace for synthesis is shown in Figures 3 and 4, including a furnace body 6, a heating element 9 mounted on the furnace body, a bracket 7 hinged to the furnace body through a hinge 8, Explosion-proof monitoring thermocouple 10, low temperature area temperature control thermocouple 11, high temperature area temperature control thermocouple 12, monitoring temperature controller 13, low temperature area heating temperature controller 14, high temperature area heating temperature controller 15 and explosion-proof temperature automatic controller . The above components are assembled as follows:

[0037] The heating elements 9 are distributed along the axial direction of the furnace body and are connected into two groups of independent heating systems, one group of heating systems provides heat for the low-temperature area of ​​the furnace, ...

Embodiment 3

[0049] Example 3: Synthetic method

[0050] In this embodiment, the raw materials used are zinc (Zn), germanium (Ge), and phosphorus (P), all of which are of 6N grade. When batching, the molar ratio of each raw material is zinc:germanium:phosphorus=1:1:2. According to the above Proper proportion of phosphorus-rich ingredients: zinc 8.87481 grams, germanium 9.85581 grams, phosphorus 8.41137 grams. The crucible used in the synthesis is the crucible described in Example 1; the tube furnace used in the synthesis is

[0051] Example 2 The two-temperature zone tube furnace.

[0052] The synthetic process steps are as follows:

[0053] 1. Crucible cleaning and drying

[0054] After soaking and rinsing the inner wall of the crucible with tap water, inject hydrofluoric acid lotion for 3-5 minutes, then rinse with tap water until neutral, place it in an ultrasonic cleaning tank for 8-10 minutes, and then repeat with high-resistance deionized water. Just rinse off. Drain the cleaned...

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Abstract

This invention discloses a novel method for synthesizing P / Ge / Zn polycrystal. The method combines real time temperature examine in double temperature zones, phosphorus gaseous transportation, mechanical vibration and temperature vibration. The raw materials comprise high-purity Zn, Ge and P at a mol. ratio of 1:1:2, wherein, the addition amount of P is 0.05-0.1 wt. % more than the calculated theoretical amount. The method comprises: (1) washing and drying the crucible; (2) loading the raw materials; (3) synthesizing. The crucible is composed of a main body and a feed pipe. The main body is a sealed quartz glass tube, with one end denoted A and the other end B. A concave groove is set in the main body with a distance of x to end B. The depth of the concave groove, h, is 1 / 2-2 / 3 of the main body inner diameter d. The feed pipe is set in with a distance of x to end B, and opposite to the mouth of the concave groove. The angle beta between the axis of the feed pipe and that of the main body is 45-70 deg.

Description

technical field [0001] The invention belongs to the field of preparation of ternary compound semiconductor materials, in particular to a preparation method of phosphorus germanium zinc polycrystal. Background technique [0002] At present, the material expected to be applied in the mid-infrared band of 3 μm to 5 μm is mainly AgGaS 2 and AgGaSe 2 Crystals, however, are limited for high-power applications due to their low thermal conductivity and low photodamage threshold. In recent years, studies have found that phosphorus germanium zinc (ZnGeP 2 , ZGP for short) crystal not only has large nonlinear optical coefficient, high quality factor, but also has high thermal conductivity and light damage threshold. , It has extensive and important uses in infrared laser weapons, infrared guidance, infrared ranging, infrared remote control, lidar, isotope separation, atmospheric monitoring and other fields. [0003] ZnGeP 2 The synthesis method of polycrystal is mainly direct synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/10
Inventor 赵北君朱世富何知宇陈观雄
Owner SICHUAN UNIV
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