Molybdenum oxychloride with improved bulk density

Abstract

To provide a molybdenum oxychloride consolidated mass showing improved physical characteristics such as increased bulk density, improved size / shape uniformity, and improved heat transfer, and a method of producing the same, and to provide a molybdenum oxychloride composition for use in forming a consolidated mass.SOLUTION: There are provided a molybdenum oxychloride consolidated mass including molybdenum oxychloride and a binder in an amount of less than 10 wt.% and having a bulk density of over 0.85 g / cc, and a molybdenum oxychloride composition including molybdenum oxychloride and a binder in an amount of less than 10 wt.% and having a bulk density of over 0.75 g / cc.SELECTED DRAWING: None

Description

Technical Field

[0001] Cross - reference to Related Applications

[0001] This application claims priority to U.S. Provisional Patent Application No. 62 / 923,892, filed October 21, 2019, the entire disclosure of which is incorporated herein by reference.

[0002]

[0002] This disclosure relates to molybdenum oxychloride compositions and compacts, such as pellets made therefrom. In particular, the disclosure relates to molybdenum oxychloride compositions that exhibit improvements in bulk density and contain little to no binder, if any.

Background Art

[0003]

[0003] Conventional molybdenum oxychloride compositions are often typically used in powder form in high - temperature thin - film sublimation processing chambers. Generally, these molybdenum oxychloride compositions are synthesized in the form of low - density (fluffy) powders and typically have a relatively large average crystal size, e.g., cross - body measurements, and / or a low surface area. In operation, the powder is heated to a temperature at which deposition occurs until it sublimates.

[0004]

[0004] Generally speaking, powders (often pelletizing binders) can be pressed into pellets, e.g., tablets. However, powders with a relatively large average crystal size often cause problems in pellet formation, perhaps due to a reduced likelihood of crystal - to - crystal adhesion, and may result in pellets with a low bulk density. Importantly, low - density pellets essentially contain little of the powder composition. In the case of molybdenum oxychloride pellets, low - density pellets may contain little molybdenum oxychloride. Thus, low - density pellets often have to be re - loaded into the thin - film sublimation processing chamber, including in some subsequent processes, resulting in downtime and a reduction in the efficiency of the overall process.

[0005] In some cases, a binder can be added to improve crystal adhesion, thereby promoting improvement in pellet formation. Unfortunately, the introduction of the binder causes further problems, such as a decrease in overall pellet purity, and additional processing, such as purification after pelletization or "burn-off" of the binder, must be addressed before use of the pellets in the proposed application areas. Importantly, the addition of the binder can also contribute to a decrease in the bulk density of the pellets.

[0006]

[0006] Furthermore, conventional molybdenum oxychloride powders suffer from insufficient particle size uniformity, and / or insufficient shape uniformity and / or uneven heat transfer throughout their bulk, resulting in non-uniform deposition.

[0007]

[0007] In addition, conventional molybdenum oxychloride powders are associated with difficulties in packaging and transportation due to their low density; for example, it has been found that the powder (or low-density compacts manufactured therefrom) takes up too much volume with respect to the actual amount of molybdenum oxychloride. Thus, the ability to use effectively available packaging and shipping is not efficient, and additional packaging and shipping means must be employed.

Summary of the Invention

Problems to be Solved by the Invention

[0008]

[0008] In view of conventional molybdenum oxychloride technology, there is a need for improved molybdenum oxychloride compacts that exhibit improved physical properties, such as increased bulk density and improved size / shape uniformity and heat transfer, while reducing or eliminating the need for, for example, binders, and for molybdenum oxychloride compositions (powders) used in the formation of the compacts.

Means for Solving the Problems

Means for Solving the Problems

[0009]

[0009] In some embodiments, the present disclosure relates to consolidated masses of molybdenum oxychloride comprising molybdenum oxychloride (greater than 95 wt%) and a binder (ceramic binder, cellulose or hydroxyalkylcellulose, or a mixture thereof) (less than 10 wt%, e.g., less than 5 wt%). The consolidated masses have a bulk density greater than 0.85 g / cc, e.g., greater than 1.4 g / cc. The molybdenum oxychloride may contain crystals, and at least 90% of the crystals may have an average cross body dimension of less than 5 mm and / or a surface area greater than 0.0005 cm 2 / g. The consolidated masses may have a relative density greater than 75% and / or a heat transfer uniformity of less than ±10% across the individual consolidated masses. The consolidated masses may have an average cross body dimension greater than 1 mm.

[0010]

[0010] In some embodiments, the present disclosure relates to a molybdenum oxychloride composition comprising molybdenum oxychloride (greater than 95 wt%) and less than 10% binder. The molybdenum oxychloride composition has a bulk density greater than 0.75 g / cc and / or a tap density greater than 1 g / cc as measured by ASTM B527-2006. The molybdenum oxychloride may contain crystals, and at least 90% of the crystals may have an average cross body dimension of less than 1 mm and / or a surface area greater than 0.0005 cm 2 / g.

[0011]

[0011] In some embodiments, the present disclosure relates to a method of manufacturing a molybdenum oxychloride compact, the method comprising preparing a molybdenum oxychloride composition having a bulk density greater than 0.75 g / cc and comprising molybdenum oxychloride and less than 10% binder, and pressing the molybdenum oxychloride composition to form a compact. The compact has a bulk density greater than 1.4 g / cc. In some cases, the pressing step comprises filling a mold with the molybdenum oxychloride composition and pressing the formed molybdenum oxychloride composition to form a compact. The pressing may be performed at a pressure less than 1000 MPa. The preparing step is a step of synthesizing an intermediate molybdenum oxychloride composition comprising molybdenum oxychloride and less than 10% binder, the intermediate molybdenum oxychloride composition containing crystals and having a bulk density less than 0.75 g / cc, and separating the intermediate molybdenum oxychloride composition to form a molybdenum oxychloride composition.

DETAILED DESCRIPTION OF THE INVENTION

[0012]

[0012] As shown above, conventional molybdenum oxychloride powders have a large average crystal size (compared to the powders of the present disclosure), e.g., cross-over measurements, and / or a small surface area, and / or may contain a significant amount of binder. As a result, compacts, e.g., pellets made from said powders, have a lower bulk density than desired. Pellets with a low bulk density require frequent loading / reloading of high-temperature semiconductor processing chambers (in some cases, the pellets are processed before being used in the chamber). As a result, downtime occurs, leading to a decrease in the efficiency of the overall process. Furthermore, these powders / pellets cause problems with insufficient particle size and / or shape uniformity, and / or non-uniform heat transfer throughout the bulk, resulting in non-uniform deposition. Also, conventional powders / pellets have problems with packaging and transportation. For example, the pellets Takes up too much volume. Thus, the ability to effectively use available packaging and shipping is not effective, and additional packaging and shipping means must be used.

[0013]

[0013] By the way, the present inventors have found that specific molybdenum oxychloride powder having relatively small crystals can be effectively pressed into a denser consolidated product, such as a pellet. A consolidated product is a broad term encompassing an object obtained as a result of being formed or shaped from a composition, such as the powders disclosed herein. In some cases, the consolidated product is in the form of a pellet, tablet, sphere, disk or pastille, or a combination thereof. The use of the term "pellet" or "pelletization" herein is not intended to limit the scope of the consolidated product or the related process / processing. For example, a "pellet" may be spherical and / or "pelletization" may form a consolidated product shaped into a sphere.

[0014]

[0014] Traditionally, when pelletizing powders having larger crystals, problems such as insufficient crystal-to-crystal adhesion and low bulk density have occurred. Without being bound by theory, it is assumed that the larger the crystal structure, the smaller the surface area (per unit volume), and thus the lower the chance of forming a consolidated product due to crystal-to-crystal adhesion, i.e., self-adhesion. In the case of molybdenum oxychloride, by using a powder having relatively small crystals, the surface area is improved, enabling better crystal-to-crystal adhesion and more effective pelletization. Furthermore, the consolidated product has surprisingly been found to have a higher bulk density in addition to a higher purity. Advantageously, due to the increased bulk density, the need to reload the pellets in a semiconductor processing chamber is significantly reduced. Thus, the overall production efficiency is greatly improved.

[0015] In some cases, the powder (and the resulting consolidated material) requires, if any, a small amount of binder, but advantageously also contributes to reducing or eliminating problems associated with the purity and density of the binder. Without being bound by theory, it is assumed that the overall bulk density of the consolidated material is improved by using, if any, fewer low-density components, such as the binder. Also, the need for further processing, such as separation after pelletization or "burning out" of the binder, prior to using the consolidated material in a semiconductor processing chamber is, beneficially, reduced or eliminated.

[0016]

[0016] It has also been discovered that the high-density consolidated materials disclosed herein have more consistent uniformity and heat transfer throughout the consolidated material and advantageously provide a more homogeneous deposition in semiconductor applications.

[0017]

[0017] Molybdenum oxychloride is a known compound that is generally available as a yellow or orange solid. For example, molybdenum oxychloride can have the CAS number 13637-68-8. Molybdenum oxychloride has a theoretical density of 3.31 g / cm 3 However, conventional molybdenum oxychloride compositions, such as powders, do not reach this density due to the powder structure. As noted, conventional molybdenum oxychloride compositions, such as powders or pellets, have a much lower actual bulk and / or relative density.

[0018] Consolidated material

[0018] In some embodiments, the present disclosure relates to molybdenum oxychloride consolidated materials. The consolidated material includes a specific molybdenum oxychloride (powder) and, if any, a small amount of binder. The consolidated material has a high bulk density, such as a bulk density greater than 1.4 g / cc. Bulk density is a well-known measurement. For example, bulk density is measured by weighing the amount of material contained in a known volume and calculating the weight per volume of the consolidated material, i.e., the bulk density. It can be done. Another method for measuring the bulk density is provided in ASTM B329 - 2006. Molybdenum oxychloride contains crystals of molybdenum oxychloride, and in some embodiments, the crystals are relatively small. As shown above, the small crystal size surprisingly increases the surface area, enables better crystal-to-crystal adhesion in the compacted material, and at least partially contributes to the improvement of the bulk density. The molybdenum oxychloride powder itself will be discussed in more detail below.

[0019]

[0019] In some embodiments, the bulk density of the compacted material exceeds 0.85 g / cc, for example, exceeds 0.9 g / cc, exceeds 1.0 g / cc, exceeds 1.2 g / cc, exceeds 1.4 g / cc, exceeds 1.5 g / cc, exceeds 1.7 g / cc, exceeds 2.0 g / cc, exceeds 2.1 g / cc, exceeds 2.2 g / cc, exceeds 2.5 g / cc, exceeds 2.7 g / cc or exceeds 3.0 g / cc. From the perspective of the range, the bulk density of the compacted material may be in the range of 0.85 g / cc to 3.1 g / cc, for example, 0.9 g / cc to 3.1 g / cc, 1.0 g / cc to 3.1 g / cc, 1.2 g / cc to 3.1 g / cc, 1.4 g / cc to 3.1 g / cc, 1.4 g / cc to 3.0 g / cc, 1.4 g / cc to 2.2 g / cc, 1.4 g / cc to 2.8 g / cc, 1.5 g / cc to 2.8 g / cc, 1.6 g / cc to 2.5 g / cc, 1.4 g / cc to 2.0 g / cc or 1.6 g / cc to 2.0 g / cc.

[0020]

[0020] The consolidated material can also be characterized in terms of relative density. For example, the relative density of the consolidated material can exceed 75%, for example, exceed 80%, exceed 85%, exceed 86.5%, exceed 87%, exceed 88%, exceed 90%, exceed 92%, exceed 95%, exceed 97%, or exceed 99%. From the perspective of range, the relative density of the consolidated material can be in the range of 75% - 99.9%, for example, 85% - 99%, 88% - 99%, 90% - 98%, 91% - 97% or 92% - 96%. In some cases, relative density is a measure of how much air or impurities are present in the pellet. Relative density can be calculated as the ratio of the actual measured density to the maximum theoretical density, for example, 3.31 for molybdenum oxychloride. The inventors have found that the use of the powders of the present disclosure provides a small amount of air / impurities and unexpectedly provides improvements in density and conductivity.

[0021]

[0021] In some embodiments, by using molybdenum oxychloride powder having relatively small crystals, higher density consolidated materials can be achieved in many cases without using a binder.

[0022]

[0022] In some embodiments, at least 90% of the molybdenum oxychloride crystals have an average across dimension of less than 5 mm, for example, less than 4 mm, less than 3 mm, less than 2 mm, less than 1 mm, less than 0.7 mm, less than 0.5 mm, less than 0.3 mm, less than 0.1 mm, or less than 0.05 mm. From the perspective of range, at least 90% of the crystals can have an average across dimension in the range of 0.01 mm - 5 mm, for example, 0.05 mm - 3 mm, 0.05 mm - 2 mm, 0.1 mm - 3 mm, 0.1 mm - 2 mm, 0.1 mm - 1 mm, 0.3 mm - 3 mm, 0.3 mm - 2 mm or 0.5 mm - 1.5 mm. From the perspective of the lower limit, at least 90% of the molybdenum oxychloride crystals have an average across dimension exceeding 0.01 mm, for example, exceeding 0.05 mm, exceeding 0.1 mm, exceeding 0.3 mm, exceeding 0.5 mm, or exceeding 0.7 mm.

[0023] In some embodiments, the crystals of the consolidated material can have a large surface area. For example, the crystals can have a surface area greater than 0.0005 cm 2 / g, such as greater than 0.001 cm 2 / g, greater than 0.005 cm 2 / g, greater than 0.007 cm 2 / g, greater than 0.01 cm 2 / g, greater than 0.012 cm 2 / g, greater than 0.015 cm 2 / g, greater than 0.017 cm 2 / g, greater than 0.02 cm 2 / g, greater than 0.025 cm 2 / g, greater than 0.05 cm 2 / g, greater than 0.1 cm 2 / g, or can have a surface area greater than 0.25 cm 2 / g. From a range perspective, the crystals can have a surface area in the range of 0.0005 cm 2 / g to 1.0 cm 2 / g, such as in the range of 0.001 cm 2 / g to 0.5 cm 2 / g, 0.005 cm 2 / g to 0.1 cm 2 / g, 0.007 cm 2 / g to 0.1 cm 2 / g, 0.01 cm 2 / g to 0.1 cm 2 / g or 0.012 cm 2 / g to 0.05 cm 2 / g.

[0024]

[0024] In some cases, the molybdenum oxychloride compact is a high-purity pellet. For example, the compact may contain more than 95 wt%, such as more than 96 wt%, more than 97 wt%, more than 98 wt%, more than 99 wt%, or more than 99.5 wt% molybdenum oxychloride. From a range perspective, the compact may contain 80 wt% to 99.999 wt%, such as 90 wt% to 99.999 wt%, 95 wt% to 99.99 wt%, or 97 wt% to 99 wt% molybdenum oxychloride. From a lower limit perspective, the compact may contain less than 99.99 wt%, such as less than 99.9 wt%, less than 99.5 wt%, less than 99.3 wt%, or less than 99 wt% molybdenum oxychloride. Surprisingly, if any, the use of a smaller amount of binder in the compact, such as impurities, advantageously contributes to purity improvement.

[0025]

[0025] As shown above, the use of a small amount of binder, if any, provided the aforementioned benefits. In some embodiments, the compact contains less than 10 wt%, such as less than wt%, less than 5 wt%, less than 3 wt%, less than 1 wt%, less than 0.7 wt%, less than 0.5 wt%, or less than 0.1 wt% binder. From a range perspective, the compact contains 0.1 wt% to 10 wt% binder, such as 0.1 wt% to 8 wt%, 0.5 wt% to 7 wt%, 1 wt% to 6 wt%, or 2 wt% to 5 wt%.

[0026]

[0026] Pelletizing binders are well known in the art. Exemplary binders include ceramic binders, cellulose, and hydroxyalkyl cellulose. An exemplary commercial product is Klucel™ hydroxypropyl cellulose from Ashland Chemical.

[0027]

[0027] The use of the powders of the present disclosure (which, if any, contain only a small amount of binder) has been found to unexpectedly provide improved heat transfer uniformity across individual compacts. Without being bound by theory, it is believed that the higher the density of the compact, the less air and / or impurities are present therein. As a result, the overall conductivity and heat transfer properties of the compact are improved. In some embodiments, the compact has a heat transfer uniformity of less than ±10%, such as less than ±8%, less than ±5%, less than ±3%, less than ±1%, less than ±0.5%, or less than ±0.1% across the individual compacts.

[0028]

[0028] The size of the compact may vary widely. In some cases, the compact may have an average across dimension, such as greater than 1 mm, such as greater than 3 mm, greater than 5 mm, greater than 7 mm, greater than 10 mm, greater than 12 mm, greater than 15 mm, greater than 17 mm, greater than 20 mm, greater than 24 mm, or greater than 30 mm.

[0029] powder

[0029] As shown above, the compact is formed from a specific powder. In some embodiments, molybdenum oxychloride powder (molybdenum oxychloride composition) contains molybdenum oxychloride and, if any, only a small amount of binder, such as less than 10% binder. The molybdenum oxychloride powder has a bulk density greater than 0.75 g / cc. The molybdenum oxychloride powder is pressed into a compact. Thus, many of the measurements of the characteristics, properties, and qualities of the aforementioned composition of the compact also apply to the powder, for example, to molybdenum oxychloride and binder concentration, crystal size, surface area, etc. However, in some cases, the powder may have low density characteristics, for example, the powder may not be as dense as the pellet. The same applies to the concentration of molybdenum oxychloride and binder, crystal size, surface area, etc. However, in some cases, the powder may have low density characteristics, for example, the powder may not be as dense as the pellet.

[0030]

[0030] In some embodiments, the bulk density of the powder exceeds 0.55 g / cc, for example, exceeds 0.65 g / cc, exceeds 0.75 g / cc, exceeds 0.8 g / cc, exceeds 0.85 g / cc, exceeds 0.9 g / cc, exceeds 1.0 g / cc, exceeds 1.2 g / cc, exceeds 1.5 g / cc, exceeds 2.0 g / cc, or exceeds 2.5 g / cc. From the perspective of the range, the bulk density of the powder is in the range of 0.55 g / cc to 3.31 g / cc, for example, 0.65 g / cc to 3.31 g / cc, 0.70 g / cc to 3.31 g / cc, 0.75 g / cc to 3.31 g / cc, 0.77 g / cc to 3.0 g / cc, 0.78 g / cc to 2.5 g / cc, 0.77 g / cc to 2.0 g / cc, 0.55 g / cc to 2.0 g / cc, 0.7 g / cc to 1.8 g / cc, 1.0 g / cc to 1.5 g / cc, 1.2 g / cc to 1.3 g / cc.

[0031]

[0031] The powder may have a high tap density in some cases. For example, the tap density of the powder exceeds 0.5 g / cc, for example, exceeds 0.6 g / cc, exceeds 0.7 g / cc, exceeds 0.8 g / cc, exceeds 0.85 g / cc, exceeds 0.9 g / cc, exceeds 1.0 g / cc, exceeds 1.2 g / cc, exceeds 1.5 g / cc, or exceeds 2.0 g / cc. From the perspective of the range, the tap density of the powder is in the range of 0.5 g / cc to 3.5 g / cc, for example, 0.5 g / cc to 2.0 g / cc, 0.6 g / cc to 1.8 g / cc, 0.7 g / cc to 1.5 g / cc, 0.8 g / cc to 1.3 g / cc, 0.9 g / cc to 1.1 g / cc or 0.95 g / cc to 1.05 g / cc. The tap density may be measured according to ASTM B527 - 2006.

[0032]

[0032] In some cases, the bulk density of the compact is at least 5% greater, at least 10% greater, at least 25% greater, at least 50% greater, at least 75% greater, or at least 100% greater than the bulk density of the powder.

[0033] Method for manufacturing a compact

[0033] The present disclosure also relates to a method for manufacturing a consolidated body. The method includes a step of preparing molybdenum oxychloride powder and a step of pressing the powder to form a consolidated body. The consolidated body has the properties discussed herein.

[0034]

[0034] In some cases, the pressing step may include a step of filling the powder into a mold and a step of pressurizing the shaped powder to form a consolidated body. The inventors have found that the specific powders disclosed herein provide benefits in processing. For example, if the powder completely fills the mold, there is less powder left as air pockets and / or other impurities that can affect pellet composition, density, and / or conductivity. Without being bound by theory, it is assumed that smaller-sized crystals assist in this improved packing of the mold. As a result, a high-density and high-performance consolidated body is formed.

[0035]

[0035] In some cases, the pressurization of the shaped powder can be performed at a lower pressure than that used when conventional powders are used. The smaller crystals and larger surface area of the powder are considered to advantageously contribute to the adhesion between crystals, enabling the formation of a consolidated body under a lower pressure.

[0036]

[0036] In some embodiments, the pressurization is performed at a pressure of less than 1000 MPa, for example, less than 800 MPa, less than 750 MPa, less than 700 MPa, less than 650 MPa, less than 600 MPa. From a range perspective, the pressurization may be performed at a pressure in the range of 50 MPa to 1000 MPa, for example, 100 MPa to 1000 MPa, 50 MPa to 500 MPa, 50 MPa to 400 MPa, 50 MPa to 300 MPa, 75 MPa to 400 MPa, 100 MPa to 300 MPa, 100 MPa to 200 MPa, 200 MPa to 900 MPa, 300 MPa to 800 MPa, 400 MPa to 700 MPa, or 400 MPa to 650 MPa. Advantageously, the low pressure improves work efficiency and also contributes to the improvement of equipment consumption.

[0037]

[0037] In other embodiments, the preparation of the powder includes synthesizing an intermediate molybdenum oxychloride composition (powder) comprising molybdenum oxychloride and less than 10% binder. The intermediate molybdenum oxychloride composition contains crystals and has a bulk density of less than 0.75 g / cc. The method further includes separating the intermediate molybdenum oxychloride composition to form a molybdenum oxychloride composition. In this step, the bulk density of the intermediate molybdenum oxychloride powder increases to obtain the aforementioned molybdenum oxychloride powder. In some cases, larger crystals may be removed from the intermediate molybdenum oxychloride powder, for example, via sieving or other size-related separation methods.

Examples

[0038]

[0038] The following examples are provided to illustrate the compositions and methods of the present disclosure. The examples are merely illustrative and are not intended to limit the present disclosure to the materials, conditions, or process parameters described herein.

[0039]

[0039] As described herein, molybdenum oxychloride powders of Examples 1 and 2 having a smaller crystal size, e.g., less than 5 mm, e.g., approximately 0.8 mm to 2 mm, were prepared. The powder was loaded into a graduated glass container with a volume of approximately 870 cc. Advantageously, due to the minimal (if any) binder content, burn-out of the powder was not performed. A conventional powder of Comparative Example A having a larger crystal size was loaded into a similar graduated glass container. The loaded container was weighed, thereby calculating the bulk density. The results are shown in Table 1.

[0040]

Table 1

[0041] As shown, the powders of Examples 1 and 2 exhibit significantly higher tap densities, for example, exceeding 1.4 g / cc. This high density beneficially enables more highly dense compacts, for example, more highly dense powders. Advantageously, the more highly dense powders contain more molybdenum oxychloride and, in use, can significantly reduce the need to reload molybdenum oxychloride pellets in a semiconductor processing chamber.

[0042] The molybdenum oxychloride powders of Examples 3 and 4 having smaller crystal sizes as described herein were prepared and tablets were formed as shown in Table 2. Advantageously, due to the minimal binder content (if any), burnout of the powder was not performed. Conventional powders of Comparative Examples B and C having larger crystal sizes were similarly prepared and tablets were formed as shown in Table 2. The relative density was calculated by comparing the maximum theoretical density of 3.31 with the tablet density.

[0043]

Table 2

[0044] As shown in Table 2, the tablets of Examples 3 and 4 exhibit significantly higher tablet densities and relative densities compared to the conventional tablets of Comparative Examples B and C. Advantageously, the tablets of Examples 3 and 4 contain more molybdenum oxychloride and, in use, can significantly reduce the need to reload molybdenum oxychloride pellets in a semiconductor processing chamber.

[0045] The molybdenum oxychloride powders of Examples 5 - 12 having smaller crystal sizes as described herein were prepared. The powders were measured for tap density as measured by ASTM B527 - 2006. A conventional powder of Comparative Example D having a larger crystal size was similarly measured for tap density. The results are shown in Table 3.

[0046]

Table 3

[0047]

[0044] As shown in Table 3, the tablets of Examples 5 - 12 exhibit a tap density that is well above 0.5 g / cc, for example, greater than 0.80 g / cc. In fact, in most cases, the tap density was greater than 1.0 g / cc. As shown, Comparative Example D exhibited a tap density of 0.80 g / cc, which was even 12% lower than that of the smallest working example (Example 10) ((0.91 - 0.8) → 0.11 / 0.91 = 12%). The tap density of Comparative Example A was also lower than that of Examples 5 - 12. Advantageously, in use, powders with the higher tap densities disclosed provide excellent packing and do not require as much compression as powders with lower tap densities.

[0048] Embodiment

[0045] In particular, the following embodiments are disclosed.

[0049]

[0046] Embodiment 1: A molybdenum oxychloride compaction product comprising molybdenum oxychloride; and a binder of less than 10% by weight. The compaction product has a bulk density exceeding 0.85 g / cc, for example, exceeding 1.4 g / cc.

[0050]

[0047] Embodiment 2: The embodiment of Embodiment 1, wherein the molybdenum oxychloride contains crystals, and at least 90% of the crystals have an average across - dimension of less than 5 mm.

[0048] Embodiment 3: The embodiment of Embodiment 1 or 2, wherein the compaction product contains more than 95% by weight of molybdenum oxychloride.

[0051]

[0049] Embodiment 4: The embodiment according to any one of Embodiments 1 - 3, wherein the compaction product has a relative density exceeding 75%.

[0050] Embodiment 5: The embodiment according to any one of Embodiments 1 - 4, wherein the compaction product has a heat transfer uniformity of less than ±10% across the entire individual compaction product.

[0052]

[0051] Embodiment 6: The embodiment according to any one of Embodiments 1-5, wherein molybdenum oxychloride contains crystals, and the crystals have a surface area exceeding 0.0005 cm 2 / g.

[0052] Embodiment 7: The embodiment according to any one of Embodiments 1-6, wherein the consolidated product has an average across dimension exceeding 1 mm.

[0053]

[0053] Embodiment 8: The embodiment according to any one of Embodiments 1-7, which contains a ceramic binder, cellulose or hydroxyalkyl cellulose or a mixture thereof, and contains a binder of less than 5% by weight.

[0054]

[0054] Embodiment 9: A molybdenum oxychloride composition containing molybdenum oxychloride and a binder of less than 10%. The molybdenum oxychloride composition has a bulk density exceeding 0.75 g / cc.

[0055]

[0055] Embodiment 10: The embodiment according to Embodiment 9, wherein molybdenum oxychloride contains crystals, and at least 90% of the crystals have an average across dimension of less than 1 mm.

[0056] Embodiment 11: The embodiment according to Embodiment 9 or 10, wherein the molybdenum oxychloride composition contains more than 95% by weight of molybdenum oxychloride.

[0056]

[0057] Embodiment 12: The embodiment according to any one of Embodiments 9-11, wherein the molybdenum oxychloride composition has a tap density exceeding 0.5 g / cc, for example exceeding 1 g / cc, as measured by ASTM B527-2006.

[0057]

[0058] Embodiment 13: The embodiment according to any one of Embodiments 9-12, wherein molybdenum oxychloride contains crystals, and the crystals have a surface area exceeding 0.0005 cm 2 / g.

[0059] Embodiment 14: A method for manufacturing a molybdenum oxychloride compact, comprising the steps of preparing a molybdenum oxychloride composition having a bulk density exceeding 0.75 g / cc and containing molybdenum oxychloride and a binder of less than 10%, and pressing the molybdenum oxychloride composition to form a compact. The compact has a bulk density exceeding 1.4 g / cc.

[0058]

[0060] Embodiment 15: The embodiment according to Embodiment 14, wherein the pressing step includes the steps of filling the molybdenum oxychloride composition into a mold and pressing the formed molybdenum oxychloride composition to form a compact.

[0059]

[0061] Embodiment 16: The embodiment according to Embodiment 14 or 15, wherein the pressing step is performed at a pressure of less than 1000 MPa.

[0062] Embodiment 17: The step of preparing is a step of synthesizing an intermediate molybdenum oxychloride composition containing molybdenum oxychloride and a binder of less than 10%, the intermediate molybdenum oxychloride composition containing crystals and having a bulk density of less than 0.75 g / cc, and separating the intermediate molybdenum oxychloride composition to form a molybdenum oxychloride composition. The embodiment according to any one of Embodiments 14 - 16.

[0060]

[0063] Although the present invention has been described in detail, modifications within the spirit and scope of the invention will be readily apparent to those skilled in the art. Considering the foregoing discussion, all knowledge related to the art relevant to the background art and the detailed description, as well as the disclosures of the references discussed above, are hereby incorporated by reference into this specification. Further, it should be understood that the aspects of the present invention and parts of various embodiments, as well as the various features described hereinafter and / or in the appended claims, may be combined well or may be exchanged either in whole or in part. In the foregoing description of the various embodiments, embodiments referring to another embodiment can be appropriately combined with other embodiments as recognized by those skilled in the art. Further, those skilled in the art will recognize that the foregoing description is merely an example and is not intended to be limiting.

Claims

1. A molybdenum oxychloride compact, comprising: molybdenum oxychloride, and a binder of less than 10% by weight and having a bulk density exceeding 0.85 g / cc. A compact having a bulk density exceeding 0.85 g / cc.

2. The compact according to claim 1, wherein the molybdenum oxychloride contains crystals, and at least 90% of the crystals have an average across dimension of less than 5 mm.

3. The compact according to claim 1, comprising more than 95% by weight of molybdenum oxychloride.

4. The compact according to claim 1, having a relative density exceeding 75%.

5. The compact according to claim 1, having a heat transfer uniformity of less than ±10% across the entire individual compact.

6. The molybdenum oxychloride contains crystals, and the crystals have a surface area exceeding 0.0005 cm ２ / g, and the consolidated product according to claim 1.

7. The compact according to claim 1, having an average across dimension exceeding 1 mm.

8. The compact according to claim 1, comprising a binder of less than 5% by weight, the binder comprising a ceramic binder, cellulose, or hydroxyalkyl cellulose, or a mixture thereof.

9. A molybdenum oxychloride composition, comprising: molybdenum oxychloride and a binder of less than 10% and having a bulk density exceeding 0.75 g / cc. A composition having a bulk density exceeding 0.75 g / cc.

10. The composition according to claim 9, wherein the molybdenum oxychloride contains crystals, and at least 90% of the crystals have an average across dimension of less than 1 mm.

11. The composition according to claim 9, comprising more than 95% by weight of molybdenum oxychloride.

12. The composition according to claim 9, having a tap density exceeding 0.5 g / cc as measured by ASTM B527-2006.

13. The molybdenum oxychloride contains crystals, and the crystals have a surface area exceeding 0.0005 cm ２ / g, the composition according to claim 9.

14. A method for producing a molybdenum oxychloride compact, comprising: preparing a molybdenum oxychloride composition having a bulk density exceeding 0.75 g / cc and comprising molybdenum oxychloride and a binder of less than 10%; pressing the molybdenum oxychloride composition to form the compact having a bulk density exceeding 1.4 g / cc. A method comprising the steps of preparing a molybdenum oxychloride composition having a bulk density exceeding 0.75 g / cc and comprising molybdenum oxychloride and a binder of less than 10%, and pressing the molybdenum oxychloride composition to form the compact having a bulk density exceeding 1.4 g / cc. A method comprising the steps of preparing a molybdenum oxychloride composition having a bulk density exceeding 0.75 g / cc and comprising molybdenum oxychloride and a binder of less than 10%, and pressing the molybdenum oxychloride composition to form the compact having a bulk density exceeding 1.4 g / cc.

15. The pressing step comprises: filling the molybdenum oxychloride composition into a mold; pressing the formed molybdenum oxychloride composition to form the compact. The method according to claim 14, comprising the steps of filling the molybdenum oxychloride composition into a mold and pressing the formed molybdenum oxychloride composition to form the compact.

16. The method according to claim 15, wherein the step of applying pressure is carried out at a pressure of less than 1000 MPa. **Claim 17** The step of preparing is synthesizing an intermediate molybdenum oxychloride composition comprising molybdenum oxychloride and a binder of less than 10% wherein the intermediate molybdenum oxychloride composition contains crystals and has a bulk density of less than 0.75 g / cc; and separating the intermediate molybdenum oxychloride composition to form the molybdenum oxychloride composition The method according to claim 14, comprising:

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