KR20070051400A - Preparation of high purity tungsten hexafluoride - Google Patents
Preparation of high purity tungsten hexafluoride Download PDFInfo
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Abstract
본 발명은 고순도 육불화텅스텐(WF6)의 제조방법에 관한 것으로서, 금속 텅스텐(W)과 불소(F2), 삼불화질소(NF3) 또는 이의 혼합물을 반응시켜 육불화텅스텐(WF6)을 제조하는 방법에 있어서, 상기 금속 텅스텐으로서 산소 함량이 500 내지 5000 ppm인 것을 사용하고, 상기 불소 및 삼불화질소로서 산소 함량이 1000 ppm 이하인 것을 사용하는 것을 특징으로 하는, 본 발명의 방법에 의하면, 금속 불순물을 100 ppb 미만의 극미량으로 함유하는 고순도 육불화텅스텐을 효율적으로 제조할 수 있다. The present invention relates to a high-purity tungsten hexafluoride (WF 6 ) method, tungsten hexafluoride (WF 6 ) by reacting metal tungsten (W) and fluorine (F 2 ), nitrogen trifluoride (NF 3 ) or a mixture thereof. According to the method of the present invention, the metal tungsten has an oxygen content of 500 to 5000 ppm and the fluorine and nitrogen trifluoride has an oxygen content of 1000 ppm or less. , High-purity tungsten hexafluoride containing extremely small amount of metal impurities of less than 100 ppb can be efficiently produced.
Description
본 발명은 금속 불순물을 극미량으로 함유하는 고순도 육불화텅스텐(WF6)을 효율적으로 제조하는 방법에 관한 것이다.The present invention relates to a method for efficiently producing high purity tungsten hexafluoride (WF 6 ) containing trace amounts of metal impurities.
육불화텅스텐(WF6)은 반도체의 배선 재료로서 반도체 산업에 널리 이용되고 있다. 최근, 배선 재료로 사용되는 육불화텅스텐의 순도는 점점 고순도의 것이 요구되고 있으며, 현재 사용되고 있는 육불화텅스텐은 99.99999% 정도까지 고순도화되어 있다.Tungsten hexafluoride (WF 6 ) is widely used in the semiconductor industry as a wiring material for semiconductors. In recent years, the purity of tungsten hexafluoride used as a wiring material is increasingly required, and the tungsten hexafluoride currently used is highly purified up to about 99.99999%.
일반적으로, 육불화텅스텐은 금속 텅스텐(W)과 불소(F2) 또는/및 삼불화질소(NF3)를 접촉시켜 제조할 수 있는데, 이와 같은 방법으로 수득된 육불화텅스텐은 통상 100 내지 200 ppb 수준의 미량의 금속 불순물을 함유한다. 따라서, 육불화텅스텐의 순도를 더욱 높이기 위해서는 그 중에 함유되어 있는 금속 불순물의 농도를 100 ppb 이하로 저하시킬 필요가 있다.In general, tungsten hexafluoride can be prepared by contacting metal tungsten (W) with fluorine (F 2 ) or / and nitrogen trifluoride (NF 3 ), and the tungsten hexafluoride obtained by such a method is usually 100 to 200. Contains traces of metal impurities at the ppb level. Therefore, in order to further improve the purity of tungsten hexafluoride, it is necessary to reduce the concentration of the metal impurities contained therein to 100 ppb or less.
그러나, 이들 금속 불순물의 혼입 요인이 정확히 알려져 있지 않아 이제까지 제조된 육불화텅스텐 보다 더 고순도의 것을 제조하는 것은 사실상 거의 불가능하였다.However, the factor of incorporation of these metal impurities is not exactly known, so it was virtually impossible to produce anything of higher purity than ever produced tungsten hexafluoride.
따라서, 본 발명의 목적은 육불화텅스텐 중에 함유되어 있는 미량의 금속 불순물의 농도를 낮추어 고순도 육불화텅스텐을 효율적으로 제조하는 방법을 제공하는 것이다.It is therefore an object of the present invention to provide a method for efficiently producing high purity tungsten hexafluoride by lowering the concentration of trace metal impurities contained in tungsten hexafluoride.
상기 목적을 달성하기 위하여 본 발명에서는, 금속 텅스텐(W)과 불소(F2), 삼불화질소(NF3) 또는 이의 혼합물을 반응시켜 육불화텅스텐(WF6)을 제조하는 방법에 있어서, 상기 금속 텅스텐으로서 산소 함량이 500 내지 5000 ppm인 것을 사용하고, 상기 불소 및 삼불화질소로서 산소 함량이 1000 ppm 이하인 것을 사용하여, 금속 불순물 함량이 100 ppb 미만인 육불화텅스텐을 제조하는 것을 특징으로 하는 방법을 제공한다.In the present invention to achieve the above object, in the method of producing tungsten hexafluoride (WF 6 ) by reacting metal tungsten (W) and fluorine (F 2 ), nitrogen trifluoride (NF 3 ) or a mixture thereof, A method for producing tungsten hexafluoride having a metal impurity content of less than 100 ppb using a metal tungsten having an oxygen content of 500 to 5000 ppm and a fluorine and nitrogen trifluoride having an oxygen content of 1000 ppm or less. To provide.
이하 본 발명에 대하여 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명의 방법은 원료로서 산소 함량이 500 내지 5000 ppm인 금속 텅스텐 및 산소 함량이 1000 ppm 이하인 불소, 삼불화질소 또는 이의 혼합물을 사용하는 것을 특징으로 하며, 원료 중에 함유된 산소 함량의 제어를 통해 생성되는 육불화텅스텐 중의 금속 불순물의 농도를 용이하게 낮출 수 있음을 발견하였다. 금속 텅스텐 중의 산소 함량이 5000 ppm을 초과하거나 불소 또는 삼불화질소 중의 산소 함량이 1000 ppm을 초과하면, 생성되는 육불화텅스텐 중에 금속 불순물이 목표하는 수준보다 많게 된다. 또한, 불소 또는 삼불화질소 중의 산소 함량이 1000 ppm 이하로 유지되는 경우에는, 금속 텅스텐 중의 산소 함량을 500 ppm 이하로 과도하게 낮출 필요가 없다.The method of the present invention is characterized by using metal tungsten having an oxygen content of 500 to 5000 ppm and fluorine, nitrogen trifluoride or a mixture thereof having an oxygen content of 1000 ppm or less, and controlling the oxygen content contained in the raw material. It has been found that the concentration of metal impurities in the resulting tungsten hexafluoride can be easily lowered. If the oxygen content in the metal tungsten exceeds 5000 ppm or the oxygen content in fluorine or nitrogen trifluoride exceeds 1000 ppm, then the metal impurity in the resulting tungsten hexafluoride becomes more than the desired level. In addition, when the oxygen content in fluorine or nitrogen trifluoride is maintained at 1000 ppm or less, it is not necessary to excessively lower the oxygen content in metal tungsten to 500 ppm or less.
본 발명의 방법은 금속 텅스텐과 불소, 삼불화질소 또는 이의 혼합물을 250 내지 950℃의 온도 및 10 atm 이하의 압력조건에서 접촉시켜 육불화텅스텐(WF6)을 제조하는 방법에 이용할 수 있으나, 이러한 제조방법에 한정되지는 않는다.The method of the present invention can be used in a method for producing tungsten hexafluoride (WF 6 ) by contacting metal tungsten with fluorine, nitrogen trifluoride or a mixture thereof at a temperature of 250 to 950 ° C. and a pressure condition of 10 atm or less. It is not limited to a manufacturing method.
본 발명의 방법에 있어서, 금속 텅스텐과 불소 및/또는 삼불화질소를 접촉시키기 위해 통상적인 단관식 또는 다관식의 반응기를 사용할 수 있다. 이때, 본 발명의 방법에 따른 반응은 강한 발열반응이므로 반응온도를 250 내지 950℃ 범위에서 일정하게 유지하기 위해서는, 단관식 반응기의 경우는 다량의 육불화텅스텐으로 희석하여 반응속도를 제한하는 것이 바람직하고, 다관식 반응기의 경우는 쉘(shell) 측을 열매체로 냉각하는 것이 바람직하다.In the process of the invention, conventional mono- or multi-tubular reactors can be used for contacting metal tungsten with fluorine and / or nitrogen trifluoride. At this time, since the reaction according to the method of the present invention is a strong exothermic reaction, in order to keep the reaction temperature constant in the range of 250 to 950 ° C., in the case of a single-tube reactor, it is preferable to limit the reaction rate by diluting with a large amount of tungsten hexafluoride. In the case of the multi-tubular reactor, the shell side is preferably cooled by a heat medium.
이와 같은 본 발명의 방법에 의하면, 통상적인 방법으로 수득된 육불화텅스텐 중의 금속 불순물의 함량이 통상 100 내지 200 ppb 수준인 데 반해, 금속 불순물을 100 ppb 미만의 극미량으로 함유하는 고순도 육불화텅스텐을 효율적으로 제조 할 수 있다. According to the method of the present invention, while the content of the metal impurities in the tungsten hexafluoride obtained by the conventional method is usually 100 to 200 ppb level, high purity tungsten hexafluoride containing a very small amount of metal impurities less than 100 ppb It can be manufactured efficiently.
이하, 본 발명을 하기 실시예에 의거하여 좀더 상세하게 설명하고자 한다. 단, 하기 실시예는 본 발명을 예시하기 위한 것일 뿐, 본 발명의 범위가 이들만으로 제한되는 것은 아니다.Hereinafter, the present invention will be described in more detail based on the following examples. However, the following examples are only for illustrating the present invention, and the scope of the present invention is not limited thereto.
실시예 1Example 1
산소 함량이 1400 ppm인 금속 텅스텐과 산소 함량이 300 ppm인 불소를 750℃의 온도 및 1.5 atm의 압력에서 반응시켜 생성된 육불화텅스텐을 응축시킨 후 증류하여 정제된 육불화텅스텐을 수득하였다. 수득된 육불화텅스텐 중의 금속 불순물의 농도를 하기 표 1에 나타내었다.Tungsten hexafluoride was condensed after distillation of the tungsten hexafluoride produced by reacting a metal tungsten having an oxygen content of 1400 ppm and a fluorine having an oxygen content of 300 ppm at a temperature of 750 ° C. and a pressure of 1.5 atm. The concentration of metal impurities in the obtained tungsten hexafluoride is shown in Table 1 below.
실시예 2 내지 7 및 비교예 1 내지 4Examples 2-7 and Comparative Examples 1-4
하기 표 1에 제시된 바와 같은 산소 함량을 갖는 금속 텅스텐과 불소 또는/및 삼불화질소를 사용하여 상기 실시예 1과 동일한 방법으로 정제된 육불화텅스텐을 수득하였다. 수득된 육불화텅스텐 중의 금속 불순물의 농도를 하기 표 1에 나타내었다.Tungsten hexafluoride purified in the same manner as in Example 1 was obtained using metal tungsten and fluorine or / and nitrogen trifluoride having an oxygen content as shown in Table 1 below. The concentration of metal impurities in the obtained tungsten hexafluoride is shown in Table 1 below.
상기 표 1로부터, 산소 함량이 500 내지 5000 ppm인 금속 텅스텐 및 산소 함량이 1000 ppm 이하인 불소/삼불화질소를 사용한 실시예 1 내지 7에서 수득된 육불화텅스텐은 비교예 1 내지 7에서 수득된 육불화텅스텐에 비해 훨씬 적은 량의 금속 불순물을 함유함을 확인할 수 있다.From Table 1, the tungsten hexafluorides obtained in Examples 1 to 7 using metal tungsten having an oxygen content of 500 to 5000 ppm and fluorine / nitrogen trifluoride having an oxygen content of 1000 ppm or less were obtained in Comparative Examples 1 to 7. It can be seen that it contains much less metal impurities than tungsten fluoride.
본 발명의 방법에 의하면, 금속 불순물을 100 ppb 미만의 극미량으로 함유하 는 고순도 육불화텅스텐을 효율적으로 제조할 수 있다.According to the method of the present invention, high-purity tungsten hexafluoride containing an extremely small amount of metal impurities of less than 100 ppb can be efficiently produced.
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Cited By (4)
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CN102786092A (en) * | 2012-08-08 | 2012-11-21 | 黎明化工研究设计院有限责任公司 | Vertical countercurrent fluorinated furnace used for producing tungsten hexafluoride and use method thereof |
WO2019123771A1 (en) * | 2017-12-19 | 2019-06-27 | セントラル硝子株式会社 | Tungsten hexafluoride production method |
TWI716962B (en) * | 2018-08-17 | 2021-01-21 | 日商中央硝子股份有限公司 | Manufacturing method of tungsten hexafluoride |
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KR20100046708A (en) | 2008-10-28 | 2010-05-07 | (주)후성 | Production method of tungsten hexafluoride using fluidized bed reactor and fluidized bed reactor of the same |
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JPH02124723A (en) * | 1988-11-04 | 1990-05-14 | Mitsui Toatsu Chem Inc | Method for purifying tungsten hexafluoride |
JP3162588B2 (en) * | 1994-10-21 | 2001-05-08 | 三井化学株式会社 | Method for producing high-purity nitrogen trifluoride gas |
JP2000119024A (en) | 1998-10-13 | 2000-04-25 | Mitsui Chemicals Inc | Production of tungsten hexafluoride |
JP2001172020A (en) | 1999-12-16 | 2001-06-26 | Stella Chemifa Corp | Method for purifying high-purity tungsten hexafluoride |
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CN102786092A (en) * | 2012-08-08 | 2012-11-21 | 黎明化工研究设计院有限责任公司 | Vertical countercurrent fluorinated furnace used for producing tungsten hexafluoride and use method thereof |
WO2019123771A1 (en) * | 2017-12-19 | 2019-06-27 | セントラル硝子株式会社 | Tungsten hexafluoride production method |
KR20200087848A (en) | 2017-12-19 | 2020-07-21 | 샌트랄 글래스 컴퍼니 리미티드 | Manufacturing method of tungsten fluoride |
CN111491893A (en) * | 2017-12-19 | 2020-08-04 | 中央硝子株式会社 | Method for producing tungsten hexafluoride |
JPWO2019123771A1 (en) * | 2017-12-19 | 2020-12-10 | セントラル硝子株式会社 | Manufacturing method of tungsten hexafluoride |
TWI716962B (en) * | 2018-08-17 | 2021-01-21 | 日商中央硝子股份有限公司 | Manufacturing method of tungsten hexafluoride |
CN116425202A (en) * | 2023-02-23 | 2023-07-14 | 福建德尔科技股份有限公司 | Preparation method of tungsten hexafluoride gas |
CN116425202B (en) * | 2023-02-23 | 2023-11-21 | 福建德尔科技股份有限公司 | Preparation method of tungsten hexafluoride gas |
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