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Ultra-high purity tungsten chlorides

A technology of tungsten chloride and potassium chloride, which is applied in the direction of tungsten halide, gaseous chemical plating, chemical instruments and methods, etc., can solve the problem of high content of tungsten and iron in the application of electronics

Pending Publication Date: 2020-06-23
VERSUM MATERIALS US LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has been shown to remove significant amounts of Fe from crude tungsten chloride, the iron content in tungsten chloride purified by this method is still too high for electronic applications

Method used

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  • Ultra-high purity tungsten chlorides
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  • Ultra-high purity tungsten chlorides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0126] Example 1: Purification of tungsten hexachloride in the presence of sodium chloride

[0127] 63.6 g of crude tungsten hexachloride was mixed with 6.3 g of pre-dried sodium chloride and charged into a glass sublimator. The sublimator was preheated to 250 degrees Celsius for two hours under nitrogen atmosphere and ambient pressure. After this step, the sublimator was cooled to 180 degrees Celsius and placed under a vacuum of 80 mTorr to collect the purified tungsten hexachloride on a cold finger cooled with a stream of room temperature nitrogen. After 2 hours of sublimation, 60 g of purified tungsten hexachloride was collected on the cold finger.

[0128] Trace metal analysis by inductively coupled plasma mass spectrometry (ICP-MS) showed significant reductions in iron, chromium, nickel, and copper, as shown in Table 1.

[0129] Table 1

[0130]

[0131] 55 g of purified tungsten hexachloride from the first sublimation were mixed with 5.5 g of pre-dried sodium chl...

Embodiment 2

[0132] Example 2: Purification of Tungsten Hexachloride in the Presence of Potassium Chloride

[0133] Crude tungsten hexachloride was mixed with various amounts of pre-dried potassium chloride to study the effect of potassium chloride loading on the purification of trace impurities of tungsten hexachloride. Both mixtures were pre-ground using a mortar and pestle to achieve better contact between tungsten hexachloride and potassium chloride. The mixture was preheated at 250 °C for 2 hours. Tungsten hexachloride was sublimed from the mixture at 180 °C for 2 hours under a vacuum of 50-80 mTorr.

[0134] Purified tungsten hexachloride was collected on a cold finger and analyzed for trace metals using ICP-MS. The dependence of trace metal removal on KCl loading is shown in Table 2.

[0135] Table 2

[0136]

[0137] Results showed that the method demonstrated high-purity tungsten hexachloride with less than 0.5 ppm iron and less than 0.1 ppm molybdenum. Higher potassium ...

Embodiment 3

[0138] Embodiment 3: the synthesis of high-purity tungsten pentachloride

[0139] High-purity tungsten hexachloride containing less than 0.5 ppm of iron and molybdenum impurities is loaded into a glass boiler vessel and heated to 290 degrees Celsius. 1 standard liter per minute (SLPM) of purge gas containing 5 vol% hydrogen was supplied to the vessel to bring vapor into the tubular reactor heated to 400 degrees Celsius. The flow rate and vapor retention time were maintained to complete the conversion of tungsten hexachloride to tungsten pentachloride. High-purity tungsten pentachloride is collected from the cooled condenser. The amount of iron and molybdenum impurities in the purified tungsten pentachloride was measured to be less than 0.5 ppm.

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Abstract

Condensable metal halide materials, such as but not limited to tungsten hexachloride and tungsten pentachloride can be used deposit films metal or metal containing films in a chemical vapor deposition(CVD) or atomic layer deposition process. Described herein are high purity tungsten hexachloride and tungsten pentachloride systems and methods to purify tungsten hexachloride and tungsten pentachloride raw materials. There is provided a purified tungsten hexachloride and tungsten pentachloride containing less than 10 ppm, preferably less than 5 ppm, more preferably less than 1 ppm, and most preferably less than 0.5 ppm of iron and / or molybdenum; and less than 10 ppm, preferably less than 5 ppm of all other trace metals combined including but not limited to aluminum, potassium and sodium.

Description

[0001] Cross References to Related Applications [0002] This application claims the benefit of U.S. Provisional Patent Application No. 62 / 780,417, filed December 17, 2018, which is incorporated herein by reference as if fully set forth. technical field [0003] The present invention generally relates to the preparation of ultra-high purity tungsten chlorides, including tungsten hexachloride (WCl 6 ) and tungsten pentachloride (WCl 5 )) method, the tungsten chloride will be used in electronics industry applications. Background technique [0004] Metal halides such as TaCl 5 , WCl 6 , WCl 5 , WF 6 、MoCl 5 , HfCl 4 , ZrCl 4 and AlCl 3 , are widely used in the electronics industry as precursors for the deposition of metal, metal oxide and metal nitride films. For certain applications, the semiconductor industry requires high-purity precursors with trace metal impurities well below 10 ppm. This is because the increasing speed and complexity of semiconductor integrate...

Claims

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Application Information

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IPC IPC(8): C01G41/04
CPCC01G41/04C01P2006/80B01D7/00Y02P10/20C23C16/14
Inventor 伍笑晞S·V·伊瓦诺维N·奥斯特瓦尔德
Owner VERSUM MATERIALS US LLC
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