Method for producing molybdenum trioxide having reduced Sb content

Abstract

The present disclosure addresses the problem of providing a method for producing molybdenum trioxide in which the Sb content is reduced. A method for producing molybdenum trioxide comprises a step for mixing a starting material comprising a molybdenum compound or a hydrate thereof with chlorine gas, hydrogen chloride, or a chloride, and a step for heating the resulting mixture at a temperature of 70 DEG C or higher. Furthermore, a method for producing molybdenum trioxide comprises a step for mixing a raw material comprising molybdenum trioxide, ammonium molybdate, or a hydrate thereof with ammonium chloride, and a step for heating the resulting mixture at a temperature of 180 DEG C or higher.

Description

Technical Field

[0001] This invention relates to a method for manufacturing molybdenum trioxide with reduced Sb content. Background Technology

[0002] Molybdenum (Mo) is a promising material for electronic devices due to its low resistivity and chemical stability, such as contact plugs in large-scale integrated circuits (LSI), wiring, word lines in semiconductor memories, or diffusion barrier layers under wiring.

[0003] For example, layers formed from molybdenum or its compounds are formed using chemical vapor deposition (CVD), in which a molybdenum-containing compound is evaporated and vaporized as a precursor, decomposed on the substrate surface, and reacted to form a thin film. In recent years, to uniformly form molybdenum layers in high aspect ratio recesses, techniques have also been used to form thin molybdenum layers using atomic layer deposition (ALD), followed by the formation of thicker layers through CVD, plating, or other methods.

[0004] When using CVD or ALD to form a layer of molybdenum or its compounds, molybdenum oxychloride, which is a compound of chlorine and molybdenum oxide, is used as a precursor.

[0005] Molybdenum trioxide is typically synthesized by chlorinating molybdenum oxide with chlorine gas. High-purity molybdenum oxide is used as the raw material. Patent documents 1-4, for example, illustrate methods for producing high-purity molybdenum or molybdenum oxide. These patent documents disclose the following: molybdenum trioxide is dissolved in ammonia water; after impurity elements are precipitated and separated, ammonium molybdate is crystallized using acid, and then calcined to produce high-purity molybdenum trioxide (molybdenum oxide).

[0006] Existing technical documents Patent documents Patent Document 1: Japanese Patent Publication No. 6-10090 Patent Document 2: Japanese Patent Application Publication No. 2-141507 Patent Document 3: Japanese Patent Publication No. 5-64683 Patent Document 4: Japanese Patent Publication No. 3-7607 Summary of the Invention

[0007] The problem that the invention aims to solve Molybdenum oxychloride, used as a precursor for CVD and ALD, is synthesized by chlorinating molybdenum oxide, such as molybdenum trioxide, with chlorine gas. To improve the purity of the molybdenum oxychloride precursor, the molybdenum oxide used as the raw material needs to be refined. Traditionally, this process involves dissolving the molybdenum trioxide raw material in ammonia water, filtering it to remove solid impurities, adding nitric acid to precipitate ammonium molybdate, and then calcining it to produce molybdenum trioxide.

[0008] However, the molybdenum trioxide obtained by this method has the following problems: it is difficult to reduce the impurity antimony (Sb), or the reduction effect is low, requiring repeated refining to reduce the Sb content, which increases the refining cost. In view of these problems, the present disclosure aims to provide a method for manufacturing molybdenum trioxide that can reduce the Sb content.

[0009] Solution for solving the problem The purpose of this disclosure includes the following.

[0010] [1] A method for manufacturing molybdenum trioxide includes: a step of mixing a raw material consisting of a molybdenum compound or its hydrate with chlorine, hydrogen chloride or chloride, and a step of heating the resulting mixture at a temperature above 70°C.

[0011] [2] A method for manufacturing molybdenum trioxide includes: a step of mixing a raw material consisting of molybdenum trioxide, ammonium molybdate or their hydrates with ammonium chloride, and a step of heating the resulting mixture at a temperature above 180°C.

[0012] [3] A method for manufacturing molybdenum trioxide includes: a step of mixing a raw material consisting of molybdenum trioxide, ammonium molybdate or their hydrates with an aqueous solution containing ammonium chloride, and a step of heating the resulting mixture at a temperature above 180°C.

[0013] [4] A method for manufacturing molybdenum trioxide includes: mixing a raw material consisting of molybdenum trioxide, ammonium molybdate or their hydrates with ammonia water, mixing with hydrochloric acid, and heating the resulting mixture at a temperature above 180°C.

[0014] [5] A method for manufacturing molybdenum trioxide includes: mixing a raw material consisting of molybdenum trioxide, ammonium molybdate or their hydrates with hydrochloric acid, mixing with ammonia water, and heating the resulting mixture at a temperature above 180°C.

[0015] [6] The method for manufacturing molybdenum trioxide according to any one of [1] to [5] above, wherein the Sb content in the manufactured molybdenum trioxide is 1 / 3 or less by weight relative to the Sb content contained in the raw material.

[0016] [7] The method for manufacturing molybdenum trioxide according to any one of [1] to [6] above, wherein the S content in the manufactured molybdenum trioxide is 1 / 2 or less by weight relative to the S content contained in the raw material.

[0017] [8] The method for manufacturing molybdenum trioxide according to any one of [1] to [7], wherein the Sb content in the manufactured molybdenum trioxide is 0.2 ppm by weight or less.

[0018] [9] The method for manufacturing molybdenum trioxide according to any one of [1] to [8], wherein the S content in the manufactured molybdenum trioxide is 0.1 ppm by weight or less.

[0019] Invention Effects According to the present invention, a method for manufacturing molybdenum trioxide with reduced Sb content can be provided. Attached Figure Description

[0020] Figure 1 This represents the thermodynamic equilibrium calculation results when a system consisting of a mixture of antimony trioxide (Sb₂O₃) and hydrogen chloride (HCl) is heated from 0°C to 500°C (vertical axis is log). 10 (gram) of the diagram.

[0021] Figure 2 This represents the thermodynamic equilibrium calculation results when a system consisting of a mixture of metallic antimony (Sb) and hydrogen chloride (HCl) is heated from 0°C to 500°C (vertical axis is log). 10 (gram) of the diagram.

[0022] Figure 3 This represents the thermodynamic equilibrium calculation results when a system consisting of a mixture of antimony trioxide (Sb₂O₃) and ammonium chloride (NH₄Cl) is heated from 0°C to 500°C (the vertical axis represents log). 10 (gram) of the diagram.

[0023] Figure 4 This represents the thermodynamic equilibrium calculation results when a system consisting of a mixture of metallic antimony (Sb) and ammonium chloride (NH4Cl) is heated from 0°C to 500°C (the vertical axis represents log). 10 (gram) of the diagram.

[0024] Figure 5 The XRD pattern of molybdenum trioxide obtained by the manufacturing method disclosed herein. Detailed Implementation

[0025] (First Implementation) [Regarding raw materials] Using molybdenum trioxide (MoO3) and ammonium molybdate ((NH4)Mo7O) 24 The raw materials consist of molybdenum compounds, or their hydrates, or other molybdenum compounds. It is preferable to use raw materials with few impurities, and more preferably raw materials with a purity of 90% by weight or more, 99% by weight or more, or 99.9% by weight or more. According to this disclosure, it is possible to significantly reduce the Sb content, which is difficult to remove or has low removal efficiency even when using high-purity raw materials, using conventional methods.

[0026] [Mixed Process] Molybdenum trioxide (MoO3) and ammonium molybdate ((NH4)Mo7O) will be used. 24 The raw materials, consisting of molybdenum compounds or their hydrates, are mixed with chlorine (Cl2), hydrogen chloride (HCl), or chlorides.

[0027] [Heating process] Figure 1 The results of thermodynamic equilibrium calculations are shown for a system consisting of a mixture of antimony trioxide (Sb₂O₃) and hydrogen chloride (HCl) heated from 0°C to 500°C under atmospheric conditions. (s) represents the solid phase, and (g) represents the gas phase. The calculations were performed using the thermodynamic equilibrium software Factsage. It is assumed that the antimony (Sb) in the raw materials, such as molybdenum trioxide, ammonium molybdate, or other molybdenum compounds or their hydrates, exists in the form of antimony oxide. Figure 1 Thermodynamic calculations show that heating in the presence of hydrogen chloride causes antimony (Sb) in antimony oxide to react with hydrogen chloride to form antimony trichloride (SbCl3). This antimony trichloride is liquid at temperatures above 70°C, with some of it vaporizing. Furthermore, at temperatures above 100°C, it cannot exist in solid or liquid form and instead becomes a gas, thus reducing the amount of Sb present in the raw material as an impurity (in the form of antimony oxide).

[0028] Figure 2 The results of thermodynamic equilibrium calculations are shown for a system consisting of a mixture of antimony (Sb) and hydrogen chloride (HCl) heated from 0°C to 500°C under atmospheric conditions. (s) represents the solid phase, and (g) represents the gas phase. The calculations were performed using the thermodynamic equilibrium software Factsage. Even when the antimony (Sb) in the raw materials, such as molybdenum trioxide, ammonium molybdate, or other molybdenum compounds or their hydrates, exists in a form other than antimony oxide, such as metallic antimony, according to... Figure 2 Thermodynamic calculations show that heating in the presence of hydrogen chloride produces antimony trichloride (SbCl3). This antimony trichloride is liquid at temperatures above 70°C, with some of it vaporizing. Furthermore, at temperatures above 145°C, it cannot exist in either solid or liquid form, instead escaping from the system as a gas, thus reducing the amount of Sb present in the raw material as an impurity (in the form of metallic antimony).

[0029] As one aspect of this disclosure, after mixing a raw material consisting of ammonium molybdate or its hydrate with ammonium chloride, the resulting mixture is heated at a temperature of 70°C or higher. Chlorine, hydrogen chloride, or chloride reacts with Sb impurities contained in the raw material to form SbCl3 (gas), thereby removing the impurity. The heating temperature is preferably 100°C or higher, more preferably 145°C or higher. There is no particular upper limit to the heating temperature, but it is preferably 550°C or lower. Furthermore, the heating time is related to the amount of raw material and the heating temperature, and is preferably set to 1 hour or more. There is no particular upper limit to the heating time, but it is preferably within 72 hours, more preferably within 48 hours, in terms of energy cost. Excess chlorine, hydrogen chloride, or chloride added can be converted into gas and removed. Furthermore, the molybdenum compound or its hydrate, as a raw material, is converted into molybdenum trioxide (solid) by heating, thus simultaneously producing molybdenum trioxide with reduced Sb content.

[0030] (Second Implementation) [Regarding raw materials] Using molybdenum trioxide (MoO3) and ammonium molybdate ((NH4)Mo7O) 24 Raw materials consisting of , or their hydrates. It is preferable to use raw materials with few impurities, and more preferably raw materials with a purity of 90% by weight or more, 99% by weight or more, or 99.9% by weight or more. According to this disclosure, the Sb content, which is difficult to remove or has low removal efficiency even when using high-purity raw materials, can be significantly reduced by conventional methods.

[0031] [Mixed Process] The raw material consisting of molybdenum trioxide, ammonium molybdate, or their hydrates is mixed with ammonium chloride or an aqueous solution containing ammonium chloride.

[0032] The following methods can be listed as combinations of mixtures.

[0033] 1) A method of mixing molybdenum trioxide, ammonium molybdate, or their hydrates (all solids) with ammonium chloride (solid).

[0034] 2) A method of mixing molybdenum trioxide, ammonium molybdate, or their hydrates with an aqueous solution containing ammonium chloride.

[0035] 3) A method of mixing molybdenum trioxide, ammonium molybdate, or their hydrates with ammonia water, followed by mixing with hydrochloric acid.

[0036] 4) A method of mixing molybdenum trioxide, ammonium molybdate, or their hydrates with hydrochloric acid, and then mixing with ammonia.

[0037] [Heating process] Figure 3The results of thermodynamic equilibrium calculations are shown for a system consisting of a mixture of antimony trioxide (Sb₂O₃) and ammonium chloride (NH₄Cl) heated from 0°C to 500°C under atmospheric conditions. (s) represents the solid phase, and (g) represents the gas phase. The calculations were performed using the thermodynamic equilibrium software FactSage. It is assumed that the antimony (Sb) contained in the molybdenum trioxide, ammonium molybdate, or other molybdenum compounds, or their hydrates, as raw materials, exists in the form of antimony oxide. Figure 3 Thermodynamic calculations show that when antimony oxide is heated in the presence of ammonium chloride, antimony (Sb) reacts with ammonium chloride to produce antimony trichloride (SbCl3) and ammonia (NH3). Both antimony trichloride and ammonia are gases and escape from the system, thus reducing the amount of Sb present as an impurity in the raw materials.

[0038] Figure 4 The results of thermodynamic equilibrium calculations are shown for a system consisting of a mixture of antimony (Sb) and ammonium chloride (NH4Cl) heated from 0°C to 500°C under atmospheric conditions. (s) represents the solid phase, and (g) represents the gas phase. The calculations were performed using the thermodynamic equilibrium calculation software Factsage. Even when the antimony (Sb) contained in the molybdenum trioxide, ammonium molybdate, or other molybdenum compounds, or their hydrates, as raw materials, exists in a form other than antimony oxide, such as metallic antimony, according to... Figure 4 Thermodynamic calculations show that heating in the presence of ammonium chloride causes antimony (Sb) to react with ammonium chloride to produce antimony trichloride (SbCl2) and ammonia (NH3). Since both antimony trichloride and ammonia are gases, they escape from the system, thus reducing the amount of Sb present as an impurity in the raw materials.

[0039] As one aspect of this disclosure (corresponding to (1) in the mixing process section), after mixing a raw material consisting of molybdenum trioxide, ammonium molybdate, or their hydrates with ammonium chloride, the resulting mixture is heated at a temperature of 180°C or higher (preferably 270°C or higher, more preferably 400°C or higher). During heating, the ammonium chloride reacts with the impurity Sb contained in the raw material to form SbCl3 (gas), thereby removing it. There is no particular upper limit to the heating temperature, but it is preferably 550°C or lower. Furthermore, the heating time is also related to the amount of raw material and the heating temperature, and is preferably set to 1 hour or more. There is no particular upper limit to the heating time, but it is preferably within 72 hours, and more preferably within 48 hours, in terms of energy cost. Excess ammonium chloride can be converted into gas and removed. Furthermore, the ammonium molybdate or its hydrate, as a raw material, is converted into molybdenum trioxide (solid) by heating, thus simultaneously producing molybdenum trioxide with reduced Sb content.

[0040] As one aspect of this disclosure (relative to (2) in the mixing process section), after mixing a raw material consisting of molybdenum trioxide, ammonium molybdate, or their hydrates with an aqueous solution containing ammonium chloride, the mixture is heated. During heating, water evaporates and ammonium chloride precipitates. The precipitated ammonium chloride reacts with impurities Sb contained in the raw material to form SbCl3 (gas), thereby removing them. At this time, heating can be performed at a relatively low temperature of around 100°C to evaporate the water and precipitate the ammonium chloride and molybdenum compound. The mixture of ammonium chloride and molybdenum compound can then be heated at a temperature of 180°C or higher (preferably 270°C or higher, more preferably 400°C or higher). Alternatively, such staged heating can be omitted, and heating can be performed from the beginning at a temperature of 180°C or higher (preferably 270°C or higher, more preferably 400°C or higher).

[0041] As one embodiment of this disclosure (corresponding to (3) in the mixing step section), a raw material consisting of molybdenum trioxide, ammonium molybdate, or their hydrates is mixed with ammonia water. At this time, depending on the pH and the amount of ammonia water added, some or all of the raw material will dissolve in the ammonia water, but there may also be undissolved residue. In addition, pure water can be added to the mixed solution, and the amount of pure water added is not particularly limited. Next, hydrochloric acid is mixed into the mixed solution. The amount of hydrochloric acid mixed is not limited, but it is preferable to add it until the pH becomes 9 to 6. At this time, molybdenum compounds or molybdenum compound ions, ammonium ions, and chloride ions are present in the mixture.

[0042] Next, the mixture containing hydrochloric acid is heated. Heating evaporates the water, causing ammonium chloride to precipitate. The precipitated ammonium chloride reacts with Sb, an impurity contained in the raw material, to form SbCl3 (gas), thereby removing it. At this point, heating can be performed at a relatively low temperature of around 100°C to evaporate the water and precipitate ammonium chloride and molybdenum compounds. After this, the mixture of ammonium chloride and molybdenum compounds is heated at a temperature of 180°C or higher (preferably 270°C or higher, more preferably 400°C or higher). Alternatively, this staged heating can be omitted, and heating can be performed from the beginning at a temperature of 180°C or higher (preferably 270°C or higher, more preferably 400°C or higher).

[0043] As one aspect of this disclosure (corresponding to (4) in the mixing process section), a raw material consisting of molybdenum trioxide, ammonium molybdate, or their hydrates can be mixed with hydrochloric acid. At this time, the raw material is insoluble in hydrochloric acid and exists in a suspended state. When the suspension is heated at 55-65°C, some or all of the raw material will dissolve depending on the amount of hydrochloric acid mixed. When the temperature of the mixture is maintained at about 60°C while ammonia is mixed, ammonium molybdate and ammonium chloride will precipitate. After precipitation, the mixture is allowed to stand for about 30 minutes, and the supernatant is separated from the solids (ammonium molybdate and ammonium chloride) by decantation. This series of processes can be repeated, and the solid obtained by precipitation and separation can be mixed with hydrochloric acid and heated again, followed by mixing with ammonia to precipitate and separate ammonium molybdate and ammonium chloride. Then, the precipitated and separated solids are heated at a temperature of 180°C or higher (preferably 270°C or higher, more preferably 400°C or higher). Thus, the impurity Sb in the raw material reacts with ammonium chloride to become SbCl3 gas, which can then be removed from the solid.

[0044] Furthermore, in one embodiment of this disclosure (corresponding to (4) in the mixing step section), heating may not be performed after mixing the raw material composed of molybdenum trioxide, ammonium molybdate, or their hydrates with hydrochloric acid. Depending on the amount of hydrochloric acid added, the raw material may sometimes dissolve, or it may not need to be specifically dissolved. Next, by adding ammonia to the mixed solution, a mixture of the raw material and an aqueous solution containing ammonium chloride can be prepared. Then, the mixture is heated at a temperature of 180°C or higher (preferably 270°C or higher, more preferably 400°C or higher). As a result, the impurity Sb contained in the raw material reacts with the ammonium chloride to become SbCl3 gas, thereby being removed from the solid.

[0045] According to the above manufacturing method, molybdenum trioxide with reduced Sb can be obtained, which is difficult or difficult to remove using conventional methods. In particular, the Sb content relative to the Sb content in the raw material can be reduced to less than 1 / 3 by weight. Further, it can be reduced to less than 1 / 5, and especially to less than 1 / 10. In addition, the Sb content can be reduced to less than 0.2 ppm by weight, and further reduced to less than 0.1 ppm by weight. Whether using high-purity or low-purity raw materials, the Sb content can be reduced to less than 0.05 ppm by weight by increasing the amount of ammonium chloride mixed in.

[0046] Regarding the reduction of sulfur (S), the manufacturing method disclosed herein can yield molybdenum trioxide with reduced S content. Specifically, the S content can be reduced to less than 1 / 2 by weight relative to the S content in the raw material. Furthermore, it can be reduced to less than 1 / 3, and particularly to less than 1 / 10. Moreover, the S content can be reduced to less than 0.1 ppm by weight, and when using high-purity raw materials, the S content can be reduced to less than 0.05 ppm by weight.

[0047] [Example] The following description is based on embodiments and comparative examples. It should be noted that this embodiment is merely an example and is not intended to limit the invention in any way. The invention is limited only by the claims and includes various modifications beyond the embodiments described herein.

[0048] (Example 1) 75 g of ammonium molybdate tetrahydrate raw material with a purity of ≥99.9% was mixed with 150 ml of ammonia water (concentration: 28 wt%) and 250 ml of water. The ammonium molybdate raw material dissolved in the ammonia water. Then, 100 ml of hydrochloric acid (concentration: 36 wt%) was mixed into this solution. The pH was then set to 6.99. The resulting solution was heated at 480°C for 8 hours to obtain molybdenum trioxide (solid).

[0049] The results of ICP-MS (inductively coupled plasma mass spectrometry) analysis showed that the Sb content in the final molybdenum trioxide was less than 0.1 ppm by weight (below the detection limit), which is less than 1 / 6 of the Sb content in the raw material ammonium molybdate tetrahydrate, which contained 0.6 ppm by weight.

[0050] (Example 2) 75 g of molybdenum trioxide raw material with a purity of 98% or higher was mixed with 150 ml of ammonia water (concentration: 28 wt%) and 250 ml of water. The molybdenum trioxide raw material dissolved in the ammonia water. Then, 65 ml of hydrochloric acid (concentration: 36 wt%) was mixed into this solution. The pH was then set to 8.26. The resulting solution was heated at 480°C for 5 hours to obtain molybdenum trioxide (solid).

[0051] The results of ICP-MS (inductively coupled plasma mass spectrometry) analysis showed that the Sb content in the final molybdenum trioxide was 0.2 ppm by weight, which is 3.2 ppm by weight compared to the Sb content in the raw material molybdenum trioxide, representing a reduction to 1 / 16 of the Sb content in the raw material.

[0052] (Example 3) 75 g of molybdenum trioxide raw material with a purity of ≥98% was mixed with 363 mL of hydrochloric acid (concentration: 36 wt%). At this point, the molybdenum trioxide raw material was insoluble in the hydrochloric acid. The suspension was heated at 60°C for 1 hour, dissolving the molybdenum trioxide raw material. While maintaining the temperature of the solution at 60°C, 270 mL of ammonia water (concentration: 28 wt%) was mixed. At this point, ammonium molybdate (solid) and ammonium chloride (solid) were obtained in the solution, with a supernatant pH of 1.00. After the suspension containing ammonium molybdate was allowed to stand for 30 minutes, the supernatant was removed by decantation. This process was repeated three times for the ammonium molybdate (solid): mixing hydrochloric acid, heating at 60°C for 1 hour, then mixing ammonia water, allowing to stand, and removing the supernatant by decantation. The resulting ammonium molybdate (solid) was then heated at 480°C for 6 hours to obtain molybdenum trioxide (solid).

[0053] The results of ICP-MS (inductively coupled plasma mass spectrometry) analysis showed that the Sb content in the final molybdenum trioxide was less than 0.1 ppm by weight (below the detection limit), which is less than 1 / 32 of the Sb content in the raw material, compared to 3.2 ppm by weight in the raw material molybdenum trioxide.

[0054] Furthermore, analysis using GD-MS (glow discharge mass spectrometry) showed that the final molybdenum trioxide contained less than 0.05 ppm by weight (below the detection limit) of Sb and less than 0.05 ppm by weight (below the detection limit) of S. This can reduce the S content to less than 1 / 17 of that in the raw material.

[0055] (Example 4) Ammonium molybdate tetrahydrate raw material (5002 g) with a purity of ≥98% was mixed with ammonium chloride (999 g) with a purity of ≥99.5%. At this point, the mixture was in powder form. Heating the mixture at 480°C for 6 hours yielded a gray solid. Analysis by XRD showed... Figure 5 As shown, all observed peaks belong to molybdenum trioxide, confirming that the obtained solid substance is molybdenum trioxide.

[0056] Analysis using ICP-MS (Inductively Coupled Plasma Mass Spectrometry) showed that the Sb content in the final molybdenum trioxide was less than 0.1 ppm by weight (below the detection limit), compared to 0.5 ppm by weight in the raw material ammonium molybdate tetrahydrate, representing a reduction to less than 1 / 5 of the Sb content in the raw material. Further analysis using GD-MS (Glow Discharge Mass Spectrometry) showed that the Sb content in the final molybdenum trioxide was less than 0.05 ppm by weight (below the detection limit).

[0057] Furthermore, compared to the sulfur content of 3.1 ppm by weight in the raw material ammonium molybdate tetrahydrate, the sulfur content in the final molybdenum trioxide is 0.96 ppm by weight, which can be reduced to about one-third of the sulfur content in the raw material.

[0058] (Comparative Example 1) 75 g of ammonium molybdate tetrahydrate raw material with a purity of ≥99.9% was mixed with 250 ml of water. The resulting solution was heated at 470 °C for 8 hours to obtain molybdenum trioxide (solid). Analysis using ICP-MS (inductively coupled plasma mass spectrometry) showed that the Sb content in the final molybdenum trioxide was 0.6 ppm by weight, unchanged from the initial Sb content in the ammonium molybdate tetrahydrate raw material.

[0059] According to embodiments of the present invention, the content of antimony (Sb), which is difficult to remove or has low removal efficiency by conventional methods, can be reduced, potentially improving product quality. Improved quality is related to a stable supply of finished products and reduced losses of this finite resource of raw metal. Therefore, one embodiment of the present invention may contribute to UN-led Sustainable Development Goals (SDGs) Goal 9, “Building resilient infrastructure, fostering inclusive and sustainable industry and driving innovation,” and Goal 12, “Ensuring sustainable consumption and production patterns.”

[0060] Industrial availability The molybdenum trioxide obtained by the manufacturing method of the present invention is particularly useful as a molybdenum oxychloride raw material used as a precursor for CVD and ALD.

Claims

1. A method for manufacturing molybdenum trioxide, comprising: The process of mixing raw materials consisting of molybdenum compounds or their hydrates with chlorine, hydrogen chloride, or chlorides, and The process of heating the resulting mixture at a temperature above 70°C.

2. A method for manufacturing molybdenum trioxide, comprising: The process of mixing raw materials consisting of molybdenum trioxide, ammonium molybdate, or their hydrates with ammonium chloride, and The process of heating the resulting mixture at a temperature above 180°C.

3. A method for manufacturing molybdenum trioxide, comprising: The process of mixing a raw material consisting of molybdenum trioxide, ammonium molybdate, or their hydrates with an aqueous solution containing ammonium chloride, and The process of heating the resulting mixture at a temperature above 180°C.

4. A method for manufacturing molybdenum trioxide, comprising: The process involves mixing raw materials consisting of molybdenum trioxide, ammonium molybdate, or their hydrates with ammonia, then mixing with hydrochloric acid, and heating the resulting mixture at a temperature above 180°C.

5. A method for manufacturing molybdenum trioxide, comprising: The process involves mixing raw materials consisting of molybdenum trioxide, ammonium molybdate, or their hydrates with hydrochloric acid, then mixing with ammonia water, and heating the resulting mixture at a temperature above 180°C.

6. The method for manufacturing molybdenum trioxide according to any one of claims 1 to 5, wherein, The Sb content in the manufactured molybdenum trioxide is less than 1 / 3 by weight relative to the Sb content in the raw material.

7. The method for manufacturing molybdenum trioxide according to any one of claims 1 to 5, wherein, The sulfur content in the manufactured molybdenum trioxide is less than 1 / 2 by weight relative to the sulfur content in the raw materials.

8. The method for manufacturing molybdenum trioxide according to any one of claims 1 to 5, wherein, The Sb content in the manufactured molybdenum trioxide is less than 0.2 ppm by weight.

9. The method for manufacturing molybdenum trioxide according to any one of claims 1 to 5, wherein, The sulfur content in the manufactured molybdenum trioxide is less than 0.1 ppm by weight.

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