A molybdenum trioxide single crystal ribbon and its preparation method
By introducing a structure-directing agent during the calcination process of the molybdenum source, the problems of large-scale production and morphological consistency of molybdenum trioxide single crystal ribbons were solved, realizing the preparation of high-performance molybdenum trioxide single crystal ribbons, simplifying the preparation process and improving the consistency and performance of the material.
Patent Information
- Application Number
- CN202511007581.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-22
- Publication Date
- 2025-10-28
- Estimated Expiration
- 2045-07-22
AI Technical Summary
Existing technologies struggle to mass-produce molybdenum trioxide single crystal ribbons with high consistency and performance. Traditional methods present challenges in terms of morphology and size, limiting their potential for high-performance applications.
During the calcination of the molybdenum source, it comes into contact with a structure-directing agent composed of alkali metal salts or alkaline earth metal salts and metals other than molybdenum in Group 6. After cooling, a single crystal zone of molybdenum trioxide is obtained. The growth of MoO3 is guided along a specific direction by using a heterogeneous nucleation substrate and localized stress to induce lattice distortion.
High crystallinity and directional growth of molybdenum trioxide single crystals were achieved, simplifying the preparation process and improving the consistency and performance of the material.
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Figure CN120505703B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of single crystal material preparation technology, specifically a molybdenum trioxide single crystal ribbon and its preparation method. Background Technology
[0002] Molybdenum and molybdenum alloys possess excellent high-temperature strength and hardness, as well as good electrical and thermal conductivity and corrosion resistance, making them widely used in chemical, metallurgical, mechanical, and aerospace industries. Molybdenum trioxide (MoO3) is not only a primary raw material for preparing molybdenum and molybdenum alloys, but it also exhibits electrochromic, photochromic, photocatalytic degradation, and gas-sensing properties, thus holding special applications in the synthesis of sensitive elements, catalysts, fast ion conductors, and potential battery electrodes. Due to the surface effects, small size effects, quantum size effects, and quantum tunneling effects exhibited by nanomaterials, nano-molybdenum trioxide shows broad application prospects in battery electrode materials, catalysts, flat panel displays, smoke inhibitors, sensors, and photoluminescent color-developing materials.
[0003] In the field of single-crystal materials, the preparation of molybdenum trioxide (MoO3) single-crystal ribbons typically requires complex template-guided or high-temperature catalytic processes, which present challenges in terms of large-scale production and cost control. Furthermore, the consistency of morphology and size of MoO3 obtained by conventional methods is difficult to guarantee, limiting its potential for high-performance applications.
[0004] Therefore, there is an urgent need for a method to prepare molybdenum trioxide single crystal ribbons. Summary of the Invention
[0005] To obtain molybdenum trioxide single-crystal ribbon materials with high added value and application potential, the present invention aims to provide a molybdenum trioxide single-crystal ribbon and its preparation method. The method involves contacting a structure-directing agent composed of alkali metal salts and metals other than molybdenum in Group 6 subgroup, or alkaline earth metal salts and metals other than molybdenum in Group 6 subgroup, during the calcination of a molybdenum source, followed by cooling to obtain the molybdenum trioxide single-crystal ribbon.
[0006] A method for preparing molybdenum trioxide single crystal ribbons includes the following steps:
[0007] S1. Obtain the molybdenum source;
[0008] S2. The molybdenum source is calcined at a temperature of 800~1100℃ for 5~10h. During the calcination process, the molybdenum source comes into contact with the structure directing agent. The mass ratio of the structure directing agent to the molybdenum source is 100:(1~6).
[0009] S3. Cooling yields molybdenum trioxide single crystal ribbons.
[0010] In a preferred embodiment of the method for preparing a single crystal zone of molybdenum trioxide according to the present invention, in step S2, the structure directing agent is composed of an alkali metal salt and a metal other than molybdenum in Group 6, or an alkaline earth metal salt and a metal other than molybdenum in Group 6.
[0011] In a preferred embodiment of the method for preparing a single crystal zone of molybdenum trioxide according to the present invention, in step S2, the mass ratio of alkali metal salts to metals other than molybdenum in Group 6 subgroup or alkaline earth metal salts to metals other than molybdenum in Group 6 subgroup is 1:(1~20).
[0012] As a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon according to the present invention, step S3 further includes: cooling to obtain an orthorhombic molybdenum trioxide single crystal ribbon.
[0013] In a preferred embodiment of the method for preparing molybdenum trioxide single crystal ribbons according to the present invention, the calcination in step S2 is aerobic calcination.
[0014] In a preferred embodiment of the method for preparing a single crystal zone of molybdenum trioxide according to the present invention, in step S1, the molybdenum source has a molybdenum purity greater than 99%.
[0015] In a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon according to the present invention, step S3 further includes: the molybdenum trioxide single crystal ribbon obtained by cooling is in the form of flocculent clumps.
[0016] According to another aspect of the present invention, the present invention provides the following technical solution:
[0017] A molybdenum trioxide single crystal ribbon is obtained by the above-mentioned method for preparing a molybdenum trioxide single crystal ribbon.
[0018] As a preferred embodiment of the molybdenum trioxide single crystal ribbon described in this invention, the molybdenum trioxide single crystal ribbon is an orthorhombic molybdenum trioxide single crystal ribbon, and the average width of the orthorhombic molybdenum trioxide single crystal ribbon is 25~60μm.
[0019] The beneficial effects of this invention are as follows:
[0020] This invention provides a molybdenum trioxide single crystal ribbon and its preparation method. The method involves contacting a structure-directing agent composed of alkali metal salts and metals other than molybdenum in Group 6 subgroup, or alkaline earth metal salts and metals other than molybdenum in Group 6 subgroup, during the calcination of a molybdenum source. Cooling afterwards yields the molybdenum trioxide single crystal ribbon. This method eliminates the need for complex template guidance, utilizes readily available and simple structure-directing agents, and enables the molybdenum trioxide crystals to grow along a specific direction, resulting in highly crystalline molybdenum trioxide single crystal ribbons. Attached Figure Description
[0021] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.
[0022] Figure 1 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 1.
[0023] Figure 2 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 2.
[0024] Figure 3 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 3.
[0025] Figure 4 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 4.
[0026] Figure 5 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 5.
[0027] Figure 6 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 6.
[0028] Figure 7 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 7.
[0029] Figure 8 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 8.
[0030] Figure 9 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 9.
[0031] Figure 10 This is a SEM image of the molybdenum trioxide single crystal zone obtained in Example 10.
[0032] Figure 11 The image shows a SEM image of the blocky molybdenum trioxide prepared in Comparative Example 1.
[0033] Figure 12 The image shows a SEM image of molybdenum trioxide in a band-like shape obtained in Comparative Example 2.
[0034] Figure 13 SEM image of molybdenum trioxide bonded together as prepared in Comparative Example 3.
[0035] Figure 14 The image shows a SEM image of the layered molybdenum trioxide prepared in Comparative Example 4.
[0036] The realization of the objective, functional features and advantages of the present invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation
[0037] The technical solutions described below in conjunction with the embodiments will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0038] This invention proposes a molybdenum trioxide single crystal ribbon and its preparation method. The method involves contacting a structure-directing agent composed of alkali metal salts and metals other than molybdenum in Group 6 or alkaline earth metal salts and metals other than molybdenum in Group 6 during the calcination of a molybdenum source, followed by cooling to obtain the molybdenum trioxide single crystal ribbon.
[0039] According to one aspect of the present invention, the present invention proposes the following technical solution:
[0040] A method for preparing molybdenum trioxide single crystal ribbons includes the following steps:
[0041] S1. Obtain the molybdenum source;
[0042] S2. The molybdenum source is calcined at a temperature of 800~1100℃ for 5~10h. During the calcination process, the molybdenum source comes into contact with the structure directing agent. The mass ratio of the structure directing agent to the molybdenum source is 100:(1~6).
[0043] S3. Cooling yields molybdenum trioxide single crystal ribbons.
[0044] Preferably, in step S2, the mass ratio of the structure-directing agent to the molybdenum source is 100:(1~6). Specifically, the mass ratio can be, for example, but not limited to, any one of 100:1, 100:2, 100:3, 100:4, 100:6, or a range between two of them.
[0045] Preferably, in step S2, the structure directing agent is composed of alkali metal salts and metals other than molybdenum from Group 6, or alkaline earth metal salts and metals other than molybdenum from Group 6.
[0046] Preferably, the mass ratio of alkali metal salts to Group 6 sub-metals other than molybdenum, or alkaline earth metal salts to Group 6 sub-metals other than molybdenum, in the structure-directing agent is 1:(1~20). Specifically, the mass ratio can be, for example, but not limited to, any one of 1:1, 1:5, 1:10, 1:15, 1:20, or a range between two of them.
[0047] Furthermore, step S3 also includes: cooling to obtain orthorhombic molybdenum trioxide single crystal ribbons.
[0048] Furthermore, in step S2, the alkali metal salt or alkaline earth metal salt acts as an inducing agent, wherein the metal cations (such as K⁺, Na⁺) are embedded in the layered structure of MoO₃, generating localized stress and inducing lattice distortion or oxygen vacancy formation. This lattice distortion selectively inhibits the growth of certain crystal planes, guiding MoO₃ to extend along specific directions to form a banded structure.
[0049] Furthermore, the metals of the sixth subgroup other than molybdenum serve as heterogeneous nucleation substrates. The oxidation of the metal element into stable oxides can provide a large number of oxygen vacancies to provide anchoring sites for MoO3 molecules, reduce the nucleation energy, and induce MoO3 to grow along a specific crystal phase. This inhibits the aggregation of MoO3 grains. After the oxides formed by oxidation expand in volume, they are dispersed around the grains, reducing the aggregation between MoO3 grains through physical barriers.
[0050] Preferably, in step S2, the calcination is aerobic calcination, the calcination temperature is 800~1100℃, and the calcination time is 5~10h. Specifically, the calcination temperature can be, for example, but not limited to, any one of 800℃, 850℃, 900℃, 950℃, 1100℃ or a range between two of them; the calcination time can be, for example, but not limited to, any one of 5h, 6h, 7h, 8h, 9h, 10h or a range between two of them.
[0051] Furthermore, the calcination temperature needs to reach above the melting point of the molybdenum source oxide. If the temperature is too low, only a small amount of molybdenum trioxide in the form of bands can be obtained; if the temperature is too high, the molybdenum trioxide formed will clump together.
[0052] Preferably, in step S1, the molybdenum source has a molybdenum purity greater than 99%.
[0053] Furthermore, the molybdenum source can be commercially available molybdenum with a purity greater than 99% or recyclable molybdenum waste.
[0054] Furthermore, the molybdenum waste with a purity greater than 99% can be considered as scrap molybdenum boats. A scrap molybdenum boat is a molybdenum boat with a purity of 99.9% that has been scrapped after long-term use. Currently, the process for producing ultra-coarse tungsten powder involves placing tungsten oxide in a molybdenum boat and using a molybdenum wire furnace to reduce the tungsten oxide at high temperatures to obtain ultra-coarse tungsten powder. During long-term use, molybdenum boats may become thinner, deformed, or even cracked due to evaporation loss, physical wear, thermal stress fatigue, and gas permeation, rendering them unusable and requiring disposal as scrap, hence the term "scrap molybdenum boat."
[0055] Preferably, in step S3, the molybdenum trioxide single crystal ribbon obtained by cooling is in the form of flocculent clumps.
[0056] Preferably, the structure-directing agent is a powder; the molybdenum source can be small fragments or powder.
[0057] Furthermore, to achieve contact between the molybdenum source and the structure-directing agent, the structure-directing agent can be laid flat at the bottom of the container, and then small fragments of the molybdenum source can be placed on top of the structure-directing agent. During calcination, the small fragments of the molybdenum source melt and oxidize, and gradually spread onto the structure-directing agent below. Under the guidance of the structure-directing agent, the molten and oxidized molybdenum trioxide crystals grow into molybdenum trioxide single crystal bands; or the structure-directing agent and molybdenum source powder can be mixed, and during calcination, the molybdenum source powder melts and oxidizes, and the molten and oxidized molybdenum trioxide crystals grow into molybdenum trioxide single crystal bands under the guidance of the structure-directing agent.
[0058] According to another aspect of the present invention, the present invention provides the following technical solution:
[0059] A molybdenum trioxide single crystal ribbon is obtained by the above-mentioned method for preparing a molybdenum trioxide single crystal ribbon.
[0060] Preferably, the molybdenum trioxide single crystal band is an orthorhombic molybdenum trioxide single crystal band, and the average width of the orthorhombic molybdenum trioxide single crystal band is 25~60μm. Specifically, the average width can be, for example, but not limited to, any one or a range between 25μm, 35μm, 45μm, 55μm, and 60μm.
[0061] In the embodiments of the present invention, the heteronucleation substrate is tungsten of group 6. In other embodiments, chromium of group 6 can also be used. Using chromium as a heteronucleation substrate can also achieve the technical solution of the present invention.
[0062] In the embodiments of the present invention, the molybdenum source is a pretreated waste molybdenum boat. The pretreatment involves grinding the waste molybdenum boat to remove impurities adhering to its surface, crushing it to obtain small fragments or powder of the waste molybdenum boat, soaking it in acetone solution for a period of time, washing it clean with pure water, and then drying it in an oven.
[0063] The technical solution of the present invention will be further described below with reference to specific embodiments.
[0064] Example 1
[0065] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0066] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of NaCl powder to W powder in the structure guiding agent is 1:1.
[0067] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0068] S3. After shutting down the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain orthorhombic molybdenum trioxide single crystal bands as shown. Figure 1 As shown, the average bandwidth is 41.48 μm.
[0069] Example 2
[0070] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0071] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:3, and the mass ratio of NaNO3 powder to W powder in the structure guiding agent is 1:1.
[0072] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 900℃ for 7 hours.
[0073] S3. After shutting down the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain orthorhombic molybdenum trioxide single crystal bands as shown. Figure 2 As shown, the average bandwidth is 54.76 μm.
[0074] Example 3
[0075] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0076] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:5, and the mass ratio of KCl powder to W powder in the structure guiding agent is 1:1.
[0077] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 1100℃ for 10 hours.
[0078] S3. After shutting down the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain orthorhombic molybdenum trioxide single crystal bands as shown. Figure 3 As shown, the average bandwidth is 55.85μm.
[0079] Example 4
[0080] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0081] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of MgCl2 powder to W powder in the structure guiding agent is 1:10.
[0082] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0083] S3. After shutting down the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain orthorhombic molybdenum trioxide single crystal bands as shown. Figure 4 As shown, the average bandwidth is 35.21 μm.
[0084] Example 5
[0085] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0086] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of KCl powder to W powder in the structure guiding agent is 1:20.
[0087] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0088] S3. After shutting down the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain orthorhombic molybdenum trioxide single crystal bands as shown. Figure 5 As shown, the average bandwidth is 28.39 μm.
[0089] Example 6
[0090] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0091] S1. Spread the structure-directing agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure-directing agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of KCl powder to W powder in the structure-directing agent is 1:49.
[0092] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0093] S3. After turning off the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain thin strip-shaped molybdenum trioxide single crystal ribbons, as shown. Figure 6 As shown.
[0094] Example 7
[0095] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0096] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of NaCl powder to W powder in the structure guiding agent is 49:1.
[0097] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0098] S3. After shutting down the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain partially bonded molybdenum trioxide single crystal bands, such as... Figure 7 As shown.
[0099] Example 8
[0100] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0101] S1. Spread the structure-directing agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure-directing agent to the small pieces of waste molybdenum boat is 100:6, and the mass ratio of KCl powder to W powder in the structure-directing agent is 1:1.
[0102] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0103] S3. After turning off the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain thin strip-shaped molybdenum trioxide single crystal ribbons, as shown. Figure 8 As shown.
[0104] Example 9
[0105] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0106] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:1. The structure guiding agent is pure tungsten powder.
[0107] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0108] S3. After turning off the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain thin strip-shaped molybdenum trioxide single crystal ribbons, as shown. Figure 9 As shown.
[0109] Example 10
[0110] A molybdenum trioxide single crystal ribbon and its preparation method, comprising the following steps:
[0111] S1. Mix the structure-directing agent and waste molybdenum boat powder evenly and spread it on the bottom of the corundum boat dish. The mass ratio of the structure-directing agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of NaCl powder to W powder in the structure-directing agent is 1:1.
[0112] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0113] S3. After shutting down the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain an orthorhombic molybdenum trioxide single crystal band, as shown. Figure 10 As shown, the average bandwidth is 41.78 μm.
[0114] Comparative Example 1
[0115] A method for preparing molybdenum trioxide includes the following steps:
[0116] S1. Spread the structure-directing agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure-directing agent to the small pieces of waste molybdenum boat is 2:1, and the mass ratio of NaCl powder to W powder in the structure-directing agent is 1:1.
[0117] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0118] S3. After turning off the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain blocky molybdenum trioxide, as shown below. Figure 11 As shown.
[0119] Comparative Example 2
[0120] A method for preparing molybdenum trioxide includes the following steps:
[0121] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of MgCl2 powder to W powder in the structure guiding agent is 1:1.
[0122] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 700℃ for 10 hours.
[0123] S3. After turning off the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain some banded molybdenum trioxide, such as... Figure 12 As shown, the dark part is the unformed banded molybdenum trioxide, and the light part is the formed banded molybdenum trioxide.
[0124] Comparative Example 3
[0125] A method for preparing molybdenum trioxide includes the following steps:
[0126] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:1, and the mass ratio of MgCl2 powder to W powder in the structure guiding agent is 1:1.
[0127] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 1200℃ for 5 hours.
[0128] S3. After turning off the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain molybdenum trioxide bonded together, as shown below. Figure 13 As shown.
[0129] Comparative Example 4
[0130] A method for preparing molybdenum trioxide includes the following steps:
[0131] S1. Spread the structure guiding agent evenly on the bottom of the corundum boat dish, and then put in small pieces of waste molybdenum boat. The mass ratio of the structure guiding agent to the small pieces of waste molybdenum boat is 100:7, and the mass ratio of NaCl powder to W powder in the structure guiding agent is 1:1.
[0132] S2. Place the corundum boat dish in a muffle furnace and calcine it with oxygen at a temperature of 800℃ for 5 hours.
[0133] S3. After turning off the muffle furnace and cooling to room temperature, remove the corundum boat dish to obtain layered molybdenum trioxide, as shown below. Figure 14 As shown.
[0134] This invention proposes a molybdenum trioxide single crystal ribbon and its preparation method. The method involves contacting a structure-directing agent composed of alkali metal salts and group 6 subgroup metals other than molybdenum, or alkaline earth metal salts and group 6 subgroup metals other than molybdenum, during the calcination of a molybdenum source. After cooling, the molybdenum trioxide single crystal ribbon is obtained. This method eliminates the need for complex template guidance, utilizes readily available and simple structure-directing agents, and enables molybdenum trioxide crystals to grow along a specific direction, resulting in highly crystalline molybdenum trioxide single crystal ribbons.
[0135] The above description is merely a preferred embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the contents of the present invention under the inventive concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.
Claims
1. A method for preparing molybdenum trioxide single crystal ribbons, characterized in that, Includes the following steps: S1. Obtain the molybdenum source; S2. The molybdenum source is calcined at a temperature of 800~1100℃ for 5~10h. During the calcination process, the molybdenum source comes into contact with the structure directing agent. The mass ratio of the structure directing agent to the molybdenum source is 100:(1~6). S3. Cooling yields molybdenum trioxide single crystal ribbons; In step S2, the structure directing agent is composed of alkali metal salts and metals other than molybdenum from Group 6, or alkaline earth metal salts and metals other than molybdenum from Group 6.
2. The method for preparing a single-crystal molybdenum trioxide ribbon according to claim 1, characterized in that, The mass ratio of alkali metal salts to Group 6 metals other than molybdenum or alkaline earth metal salts to Group 6 metals other than molybdenum in the structure-directing agent is 1:(1~20).
3. The method for preparing a single-crystal molybdenum trioxide ribbon according to claim 2, characterized in that, Step S3 further includes: cooling to obtain orthorhombic molybdenum trioxide single crystal ribbons.
4. The method for preparing a single-crystal molybdenum trioxide ribbon according to claim 1, characterized in that, In step S2, the calcination is aerobic calcination.
5. The method for preparing a single-crystal molybdenum trioxide ribbon according to claim 1, characterized in that, In step S1, the molybdenum source has a molybdenum purity greater than 99%.
6. The method for preparing a single-crystal molybdenum trioxide ribbon according to claim 1, characterized in that, Step S3 further includes: the molybdenum trioxide single crystal ribbon obtained by cooling is in the form of flocculent clumps.
Citation Information
Patent Citations
Preparation method for centimeter-scale single crystal molybdenum trioxide nano-tape
CN106629850A
Cited By
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