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Sublimation purification device for ultra-high purity metallocene source and ultra-high purity metallocene source extraction method thereof

A metallocene, ultra-high technology, applied in the precursor of high-purity metallocene chemical vapor deposition and atomic layer deposition thin film technology, sublimation purification equipment for ultra-high-purity metallocene sources, sublimation purification of high-purity metallocene sources, can solve ultra-high The purity of metal-organic sources relies on imports, cannot meet high-purity requirements, and metallocene sources have high melting and boiling points, so as to achieve the effects of accelerating uniform heat transfer, easy replacement, and accelerated sublimation

Pending Publication Date: 2018-07-20
JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because there are a large number of impurities in the crude product, and the metallocene source has a high melting and boiling point and is easy to sublime, after ordinary rectification or steam rectification, defects such as low product yield and high content of impurities (especially water and oxygen) appear, so it is impossible to Meet the high purity requirements of 99.9999% and above in the semiconductor industry
At present, there is no report on the ultra-high-purity purification method of metallocene sources disclosed in China, and ultra-high-purity metal-organic sources for semiconductors basically rely on imports

Method used

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  • Sublimation purification device for ultra-high purity metallocene source and ultra-high purity metallocene source extraction method thereof
  • Sublimation purification device for ultra-high purity metallocene source and ultra-high purity metallocene source extraction method thereof

Examples

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Effect test

Embodiment 1

[0038] Such as figure 1 As shown, the sublimation purification device of the ultra-high-purity metallocene source includes a reactor 1, a buffer tube 2, a gradient sublimation tube 3, and a front fraction collection tank 6,

[0039] The reactor 1 is a reaction place, its interior is hollow, the bottom is provided with an inert gas inlet pipe 1616, the interior is provided with a gas dispersion plate 13, the exterior is provided with a first heating belt 11 and a first thermal resistance 12, and the inert gas enters The air pipe 16 is provided with a flow controller 8; the first thermal resistor 12 controls the temperature of the first heating belt 11;

[0040] Inert particles 14 are distributed on the gas dispersion plate 13. The reactor 1 has a magnetic stirring function and a built-in magnetic stirrer 15. The inert particles 14 are stirring balls made of polytetrafluoroethylene-wrapped magnetic steel. The diameter ranges from In 5-20mm, at least one diameter specification; ...

Embodiment 2

[0050] In this embodiment, the outer diameter of the quartz tube 32 is 220 mm, and the length of the tube is 1540 mm. Others are the same as in Embodiment 1.

Embodiment 3

[0052] A method for purifying an ultra-high-purity metallocene source using the device described in Example 1, the steps are:

[0053] (1) Place the sublimation purification device of the ultra-high-purity metallocene source described in Example 1 in a glove box protected by an inert atmosphere;

[0054] (2) The inert gas is filled into the sublimation purification device of the ultra-high-purity metallocene source described in Example 1, the inert atmosphere in step (1) and the inert gas in step (2) are high-purity nitrogen, and the mass fraction is not less than 7N; the mass fraction Not less than 7N means the gas purity is not less than 99.99999%;

[0055] (3) Mix 2.5 kg of metallocene source crude product with 2 kg of inert particles 14 and add them into the reactor 1 through the raw material feeding port, and then connect the raw material feeding port and the opening of the head end of the buffer tube 2 through the first clamp; The inert particle 14 is a stirring ball ma...

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Abstract

The invention discloses a sublimation purification device for an ultra-high purity metallocene source. The sublimation purification device includes a reactor, a buffer tube, a gradient sublimation tube and a front fraction collection tank. The invention also discloses a method for using the sublimation purification device for the ultra-high purity metallocene source to extract the ultra-high purity metallocene source. According to the sublimation purification device and the method, by adding inert particles of different particle sizes, the heat mass transfer is further strengthened by magneticstirring, materials are dispersed, agglomeration and inclusion are reduced, uniform heat transfer between materials is accelerated, and the effect of accelerating sublimation is achieved. The addition of high-purity nitrogen can reduce the partial pressure of the metallocene surface, and at the same time, the action of air flow accelerates the sublimation and improves the purification rate. The segmental temperature control of the vacuum distillation of the metallocene source is achieved by a lateral gradient sublimation method, so that the purification rate and the purity of the material areimproved, the product yield is improved, and the high purity metallocene source with the mass fraction greater than or equal to 99.99995% can be obtained.

Description

technical field [0001] The invention relates to the technical field of semiconductor materials, in particular to a method for sublimation and purification of a precursor ultra-high-purity metallocene source for high-purity organometallic chemical vapor deposition and atomic layer deposition thin film technology. The invention also relates to sublimation purification equipment for ultra-high-purity metallocene sources. Background technique [0002] Semiconductor lighting and third-generation semiconductor materials are increasingly being paid attention to by people. Laser lighting, deep ultraviolet LEDs, high-frequency high-power / high-temperature-resistant / radiation-resistant semiconductor microelectronic devices, microwave devices, etc., are widely used in power electronics, information technology, new energy, etc. Technology and other national economic fields, as well as aerospace, military anti-electronic interference, high-power radar and other military and national defen...

Claims

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Application Information

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IPC IPC(8): C07F17/00C07F17/02B01D7/00
CPCB01D7/00C07F17/00C07F17/02
Inventor 廖维林邱曾烨陈飞彪郭晓红涂媛红严楠王宝荣谢贤清雷志伟
Owner JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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