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Rapid synthetic method of polycrystalline raw materials of gallium selenide and doped series of gallium selenide

A synthesis method and technology of gallium selenide are applied in the field of rapid synthesis of gallium selenide and its doped series polycrystalline raw materials, and can solve the problems of high vapor pressure of selenium element, slow heating process, easy to exceed pressure resistance, etc. The effect of good uniformity, fast synthesis rate and large amount of single synthesis

Active Publication Date: 2013-09-11
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, since both gallium and selenium are placed at one end of the synthetic crucible, the vapor pressure of selenium is relatively large when the temperature rises rapidly (Table 1), and it is easy to exceed the pressure resistance of the crucible
Therefore, the heating process of this method is slow, and limited by the conditions, only a small amount of gallium selenide and its doped series polycrystalline raw materials can be synthesized at a single time at high temperature.

Method used

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  • Rapid synthetic method of polycrystalline raw materials of gallium selenide and doped series of gallium selenide

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Experimental program
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Embodiment 1

[0033] Embodiment 1: The synthesis of gallium selenide polycrystalline raw material is carried out according to the following steps:

[0034] ①Clean and dry the synthetic crucible made of quartz with deionized water, and coat the surface of the crucible with a suitable carbon film layer;

[0035] ②Choose gallium and selenium with a purity of 99.999%, and mix them according to the ratio of 1:1, totaling 400g, put the reaction raw materials into a quartz crucible, and evacuate to 10 -2 Pa sealed;

[0036] ③Put 80% of the sealed quartz crucible into the resistance synthesis furnace, plug the contact part of the furnace mouth with high-temperature refractory cotton above 1200°C, and expose the remaining part at the outer end of the synthesis furnace. The angle between the other end of the furnace body and the ground is 15°, as shown in the schematic diagram figure 1 as shown in a;

[0037] ④Quickly raise the temperature of the synthesis furnace to 880°C, and then raise the fina...

Embodiment 2

[0040] Embodiment 2: The synthesis of gallium selenide polycrystalline raw material is carried out as follows:

[0041] ①Clean and dry the synthetic crucible made of quartz with deionized water, and coat the surface of the crucible with a suitable carbon film layer;

[0042]②Choose gallium and selenium with a purity of 99.999%, and mix them according to the ratio of 1:1, totaling 400g, put the reaction raw materials into a quartz crucible, and evacuate to 10 -3 Pa sealed;

[0043] ③Put 95% of the sealed quartz crucible into the resistance synthesis furnace, plug the contact part of the furnace mouth with high-temperature refractory cotton above 1200°C, and expose the rest at the outer end of the synthesis furnace. The angle between the other end of the furnace body and the ground is 5°, as shown in the schematic diagram figure 1 as shown in a;

[0044] ④Quickly raise the temperature of the synthesis furnace to 860°C, then raise the final temperature of the furnace body to 9...

Embodiment 3

[0047] Embodiment 3: The synthesis of gallium selenide doped cadmium polycrystalline raw material is carried out according to the following steps:

[0048] ①Clean and dry the synthetic crucible made of quartz with deionized water, and coat the surface of the crucible with a suitable carbon film layer;

[0049] ②Choose gallium, selenium, and cadmium with a purity of 99.999%, and mix them according to the ratio of 0.98:1:0.02, totaling 400g, put the reaction raw materials into a quartz crucible, and evacuate to 10 -2 Pa sealed;

[0050] ③Put 90% of the sealed quartz crucible into the resistance synthesis furnace, plug the contact part of the furnace mouth with high-temperature refractory cotton above 1200°C, and expose the rest at the outer end of the synthesis furnace. The angle between the other end of the furnace body and the ground is 10°, as shown in the schematic diagram figure 1 as shown in a;

[0051] ④Quickly raise the temperature of the synthesis furnace to 870°C, a...

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Abstract

The invention relates to a rapid synthetic method of polycrystalline raw materials of gallium selenide and doped series of gallium selenide, and the rapid synthetic method can solve the problems that synthetic rates are low, components deviate the stoichiometric ratio and the like in present synthetic methods of polycrystalline raw materials of gallium selenide and doped series of gallium selenide. The rapid synthetic method is characterized in that a single-temperature-zone electric resistance furnace is employed for rapid heating, a furnace body has a small angle of inclination, a synthetic process is visible, and the furnace body uniformly oscillates after the synthesis. The rapid synthetic method comprises concrete steps of: (1) pretreating a crucible for the synthesis, (2) quantifying, (3) raising temperature, (4) oscillating, and (5) reducing temperature. The synthetic polycrystalline raw materials of gallium selenide and doped series of gallium selenide by means of the rapid synthetic method of the invention have the advantages of being fast in synthetic rate, being good in uniformity, being close to the stoichiometric ratio and the like.

Description

technical field [0001] The invention relates to a rapid synthesis method of gallium selenide and its doped series polycrystalline raw materials. Specifically, a single temperature zone synthesis method is used to quickly synthesize high-quality gallium selenide and its doped series polycrystalline raw materials with good uniformity and near stoichiometric ratio, providing a basic guarantee for the subsequent growth of high-quality gallium selenide single crystal . Background technique [0002] Gallium selenide, chemical formula GaSe, its single crystal is a kind of infrared nonlinear crystal material with excellent performance in the middle and long-range band, with wide light transmission band (0.6-20μm) and low absorption coefficient (α≤0.01cm -1 , 1.06μm), large nonlinear polarization coefficient (d 22 ≈54pm / V), high laser damage threshold, large birefringence (0.35), and easy phase matching. [0003] Based on the above excellent properties, gallium selenide and its do...

Claims

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Application Information

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IPC IPC(8): C01B19/04C01G15/00
Inventor 倪友保吴海信王振友毛明生黄昌保程旭东
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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