Molybdenum trioxide single crystal belt and preparation method thereof
By using structural guide agent to prepare molybdenum trioxide single crystal belt during the calcination of molybdenum source, the problems of high cost and inconsistent morphology and size in traditional methods are solved, and efficient and low-cost preparation of molybdenum trioxide single crystal belt is achieved.
Patent Information
- Application Number
- CN202511007581.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-22
- Publication Date
- 2025-08-19
- Estimated Expiration
- 2045-07-22
AI Technical Summary
The prior art is difficult to produce highly consistent and high-performance molybdenum trioxide single crystal bands on a large scale, and the traditional methods are costly and difficult to control the morphology and size.
During the calcination process of the molybdenum source, contact with alkali metal salts or alkaline earth metal salts and the structural guide agent composed of metals other than molybdenum in the sixth subgroup, and after cooling, a single-crystal band of molybdenum trioxide was obtained.
The high crystallinity growth of the single crystal band of molybdenum trioxide is achieved, the preparation process is simplified, the cost is reduced, and the consistency of morphology and size is improved.
Smart Images

Figure CN120505703A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of single crystal material preparation, and specifically relates to a molybdenum trioxide single crystal ribbon and a preparation method thereof. Background Art
[0002] Molybdenum and molybdenum alloys not only possess excellent high-temperature strength and hardness, but also possess excellent electrical and thermal conductivity and corrosion resistance, making them widely used in industries such as chemistry, chemical engineering, metallurgy, machinery, and aerospace. Molybdenum trioxide (MoO3) is not only the primary raw material for the preparation of molybdenum and molybdenum alloys, but also possesses electrochromic, photochromic, photocatalytic degradation, and gas-sensing properties. Therefore, it has special applications in the synthesis of many functional materials, including sensors, 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 has broad application prospects in battery electrode materials, catalysts, flat-panel displays, smoke retardants, sensors, and photoluminescent colorants.
[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 pose challenges in scalable production and cost control. Furthermore, the morphological and dimensional consistency of MoO3 obtained by traditional methods is difficult to ensure, limiting its potential for high-performance applications.
[0004] Therefore, there is an urgent need for a method for preparing a molybdenum trioxide single crystal ribbon to obtain a molybdenum trioxide single crystal ribbon. Summary of the Invention
[0005] To obtain molybdenum trioxide single crystal ribbon materials with high added value and application potential, the present invention provides a molybdenum trioxide single crystal ribbon and a method for preparing the same. The method comprises contacting a molybdenum source with a structure-directing agent composed of an alkali metal salt and a metal of the sixth subgroup other than molybdenum, or an alkaline earth metal salt and a metal of the sixth subgroup other than molybdenum, during calcination, and then cooling the resulting molybdenum trioxide single crystal ribbon.
[0006] A method for preparing a molybdenum trioxide single crystal ribbon comprises the following steps: S1, obtaining a molybdenum source; S2, calcining the molybdenum source at a temperature of 800-1100° C. for 5-10 hours, wherein the molybdenum source is in contact with a structure directing agent during the calcination process, and the mass ratio of the structure directing agent to the molybdenum source is 100:(1-6); S3. Cooling to obtain a molybdenum trioxide single crystal ribbon.
[0007] As a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon described in the present invention, in step S2, the structure directing agent is composed of an alkali metal salt and a metal of the sixth subgroup other than molybdenum, or an alkaline earth metal salt and a metal of the sixth subgroup other than molybdenum.
[0008] As a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon according to the present invention, in step S2, the mass ratio of the alkali metal salt to the metal of the sixth subgroup other than molybdenum or the alkaline earth metal salt to the metal of the sixth subgroup other than molybdenum in the structure directing agent is 1:(1~20).
[0009] As a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon according to the present invention, step S3 further comprises: cooling to obtain an orthorhombic phase molybdenum trioxide single crystal ribbon.
[0010] As a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon according to the present invention, in step S2, the calcination is oxygen calcination.
[0011] As a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon according to the present invention, in step S1, the molybdenum purity of the molybdenum source is greater than 99%.
[0012] As a preferred embodiment of the method for preparing a molybdenum trioxide single crystal ribbon according to the present invention, step S3 further comprises: cooling the molybdenum trioxide single crystal ribbon to form a flocculent mass.
[0013] According to another aspect of the present invention, the present invention provides the following technical solutions: A molybdenum trioxide single crystal ribbon is obtained by adopting the above-mentioned method for preparing the molybdenum trioxide single crystal ribbon.
[0014] As a preferred embodiment of the molybdenum trioxide single crystal ribbon described in the present invention, the molybdenum trioxide single crystal ribbon is an orthorhombic phase molybdenum trioxide single crystal ribbon, and the average width of the orthorhombic phase molybdenum trioxide single crystal ribbon is 25-60 μm.
[0015] The beneficial effects of the present invention are as follows: The present invention provides a molybdenum trioxide single crystal ribbon and a method for preparing the same. The method involves contacting a molybdenum source with a structure-directing agent composed of an alkali metal salt and a metal from Group VI other than molybdenum, or an alkaline earth metal salt and a metal from Group VI other than molybdenum, during calcination, followed by cooling to produce the molybdenum trioxide single crystal ribbon. This method eliminates the need for complex template guidance, utilizes a readily available structure-directing agent, and enables molybdenum trioxide crystals to grow in a specific direction, resulting in a high-crystallinity molybdenum trioxide single crystal ribbon. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying any creative work.
[0017] Figure 1 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 1.
[0018] Figure 2 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 2.
[0019] Figure 3 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 3.
[0020] Figure 4 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 4.
[0021] Figure 5 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 5.
[0022] Figure 6 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 6.
[0023] Figure 7 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 7.
[0024] Figure 8 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 8.
[0025] Figure 9 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 9.
[0026] Figure 10 This is the SEM image of the molybdenum trioxide single crystal ribbon prepared in Example 10.
[0027] Figure 11 This is the SEM image of the bulk molybdenum trioxide prepared in Comparative Example 1.
[0028] Figure 12 This is an SEM image of the partially strip-shaped molybdenum trioxide prepared in Comparative Example 2.
[0029] Figure 13 This is an SEM image of the molybdenum trioxide combined together obtained in Comparative Example 3.
[0030] Figure 14 This is the SEM image of the layered molybdenum trioxide prepared in Comparative Example 4.
[0031] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION
[0032] The following will be a clear and complete description of the technical solutions in the embodiments. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.
[0033] The present invention proposes a molybdenum trioxide single crystal ribbon and a preparation method thereof. The method comprises the following steps: during the calcination of a molybdenum source, the molybdenum source is contacted with a structure-directing agent composed of an alkali metal salt and a metal of the sixth subgroup other than molybdenum, or an alkaline earth metal salt and a metal of the sixth subgroup other than molybdenum, and then cooled to obtain the molybdenum trioxide single crystal ribbon.
[0034] According to one aspect of the present invention, the present invention proposes the following technical solution: A method for preparing a molybdenum trioxide single crystal ribbon comprises the following steps: S1, obtaining a molybdenum source; S2, calcining the molybdenum source at a temperature of 800-1100° C. for 5-10 hours, wherein the molybdenum source is in contact with a structure directing agent during the calcination process, and the mass ratio of the structure directing agent to the molybdenum source is 100:(1-6); S3. Cooling to obtain a molybdenum trioxide single crystal ribbon.
[0035] 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 therebetween.
[0036] Preferably, in step S2, the structure directing agent is composed of an alkali metal salt and a metal of the sixth subgroup excluding molybdenum, or an alkaline earth metal salt and a metal of the sixth subgroup excluding molybdenum.
[0037] Preferably, the mass ratio of the alkali metal salt to the metal of the sixth subgroup excluding molybdenum, or the alkaline earth metal salt to the metal of the sixth subgroup excluding 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 therebetween.
[0038] Furthermore, the step S3 further includes: cooling to obtain an orthorhombic phase molybdenum trioxide single crystal ribbon.
[0039] Furthermore, in step S2, the alkali metal salt or alkaline earth metal salt acts as an inducer, wherein metal cations (such as K⁺ and Na⁺) are embedded in the layered structure of MoO⁺, generating localized stress and inducing lattice distortion or oxygen vacancy formation. This lattice distortion selectively inhibits the growth of certain crystal planes, guiding the MoO⁺ to extend along specific directions, forming a ribbon structure.
[0040] Furthermore, the metals of the sixth subgroup other than molybdenum serve as heterogeneous nucleation substrates. The oxidation of metal elements into stable oxides can provide a large number of oxygen vacancies as anchoring points for MoO3 molecules, reduce nucleation energy, and induce MoO3 to grow along a specific crystal phase; inhibit the agglomeration of MoO3 grains, and the oxides formed by oxidation expand in volume and disperse around, thereby reducing the agglomeration between MoO3 grains through physical barriers.
[0041] Preferably, in step S2, the calcination is oxygen calcination, the calcination temperature is 800-1100° C., and the calcination time is 5-10 hours. Specifically, the calcination temperature can be, for example, but not limited to, any one of 800° C., 850° C., 900° C., 950° C., and 1100° C., or a range therebetween; the calcination time can be, for example, but not limited to, any one of 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, and 10 hours, or a range therebetween.
[0042] Furthermore, the calcination temperature must be above the melting point of the molybdenum source oxide. If the temperature is too low, only a small amount of ribbon-shaped molybdenum trioxide can be obtained. If the temperature is too high, the formed molybdenum trioxide will agglomerate into a mass.
[0043] Preferably, in step S1, the molybdenum purity of the molybdenum source is greater than 99%.
[0044] Furthermore, the molybdenum source can be molybdenum purchased on the market with a purity greater than 99% or recyclable molybdenum waste.
[0045] Furthermore, the molybdenum waste with a molybdenum purity greater than 99% can be a scrap molybdenum boat, which is a molybdenum boat with a molybdenum purity of 99.9% that has been discarded after long-term use. The current process for producing ultra-coarse tungsten powder involves placing tungsten oxide in a molybdenum boat and then subjecting it to high-temperature reduction in a molybdenum wire furnace to produce the ultra-coarse tungsten powder. Over long-term use, molybdenum boats can become thinner, deformed, or even cracked due to evaporation loss, physical wear, thermal fatigue, gas permeation, and other factors, rendering them unusable and requiring disposal as scrap, thus becoming a scrap molybdenum boat.
[0046] Preferably, in step S3, the molybdenum trioxide single crystal ribbon obtained by cooling is in a flocculent form.
[0047] Preferably, the structure directing agent is in the form of powder; and the molybdenum source can be in the form of small pieces or powder.
[0048] Furthermore, in order to achieve contact between the molybdenum source and the structure directing agent, the structure directing agent can be spread flat on the bottom of the container, and then small pieces of molybdenum source are placed above the structure directing agent. During the calcination process, the small pieces of molybdenum source are melted and oxidized, and gradually spread on the structure directing agent below. Under the guidance of the structure directing agent, the melted and oxidized molybdenum trioxide crystals grow into molybdenum trioxide single crystal ribbons; or the structure directing agent and molybdenum source powder can be mixed, and during the calcination process, the molybdenum source powder is melted and oxidized, and the melted and oxidized molybdenum trioxide crystals grow into molybdenum trioxide single crystal ribbons under the guidance of the structure directing agent.
[0049] According to another aspect of the present invention, the present invention provides the following technical solutions: A molybdenum trioxide single crystal ribbon is obtained by adopting the above-mentioned method for preparing the molybdenum trioxide single crystal ribbon.
[0050] Preferably, 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 to 60 μm. Specifically, the average width can be, for example, but not limited to, any one of 25 μm, 35 μm, 45 μm, 55 μm, and 60 μm, or a range therebetween.
[0051] In the embodiments of the present invention, the heterogeneous nucleation substrate is implemented by tungsten of the sixth subgroup. In other embodiments, chromium of the sixth subgroup can also be used. Using chromium as the heterogeneous nucleation substrate can also realize the technical solution of the present invention.
[0052] In the embodiments of the present invention, the molybdenum source is pretreated waste molybdenum boat, which is polished to remove impurities adhering to the surface, crushed to obtain small fragments of the waste molybdenum boat or waste molybdenum boat powder, soaked in acetone solution for a period of time, and then cleaned with pure water and placed in an oven for drying.
[0053] The technical solution of the present invention is further described below with reference to specific embodiments.
[0054] Example 1 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. 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. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, the corundum boat is taken out to obtain an orthorhombic molybdenum trioxide single crystal ribbon. Figure 1 As shown, the average bandwidth is 41.48 μm.
[0055] Example 2 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. The mass ratio of the structure-directing 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-directing agent is 1:1. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at 900°C for 7 hours. S3. After closing the muffle furnace and cooling to room temperature, the corundum boat is taken out to obtain an orthorhombic molybdenum trioxide single crystal ribbon. Figure 2 As shown, the average bandwidth is 54.76 μm.
[0056] Example 3 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. The mass ratio of the structure-directing 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-directing agent is 1:1. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 1100°C for 10 hours; S3. After closing the muffle furnace and cooling to room temperature, the corundum boat is taken out to obtain an orthorhombic molybdenum trioxide single crystal ribbon. Figure 3 As shown, the average bandwidth is 55.85 μm.
[0057] Example 4 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. The mass ratio of the structure-directing 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-directing agent is 1:10. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, the corundum boat is taken out to obtain an orthorhombic molybdenum trioxide single crystal ribbon. Figure 4 As shown, the average bandwidth is 35.21 μm.
[0058] Example 5 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. 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 1:20. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, the corundum boat is taken out to obtain an orthorhombic molybdenum trioxide single crystal ribbon. Figure 5 As shown, the average bandwidth is 28.39 μm.
[0059] Example 6 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. 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. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, take out the corundum boat to obtain a thin strip of molybdenum trioxide single crystal ribbon, such as Figure 6 shown.
[0060] Example 7 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. 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 49:1. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, the corundum boat is taken out to obtain a partially bonded molybdenum trioxide single crystal ribbon, such as Figure 7 shown.
[0061] Example 8 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. 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. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, take out the corundum boat to obtain a thin strip of molybdenum trioxide single crystal ribbon, such as Figure 8 shown.
[0062] Example 9 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. The mass ratio of the structure-directing agent to the small pieces of waste molybdenum boat is 100:1. The structure-directing agent is pure tungsten powder. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, take out the corundum boat to obtain a thin strip of molybdenum trioxide single crystal ribbon, such as Figure 9 shown.
[0063] Example 10 A molybdenum trioxide single crystal ribbon and a preparation method thereof, comprising the following steps: S1. Evenly mix the structure-directing agent and the waste molybdenum boat powder, and spread them on the bottom of the corundum 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 NaCl powder to W powder in the structure-directing agent is 1:1. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, the corundum boat is taken out to obtain an orthorhombic molybdenum trioxide single crystal ribbon, such as Figure 10 As shown, the average bandwidth is 41.78 μm.
[0064] Comparative Example 1 A molybdenum trioxide and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. 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. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, take out the corundum boat to obtain bulk molybdenum trioxide, such as Figure 11 shown.
[0065] Comparative Example 2 A molybdenum trioxide and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. The mass ratio of the structure-directing 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-directing agent is 1:1. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at 700°C for 10 hours. S3. After closing the muffle furnace and cooling to room temperature, the corundum boat was taken out to obtain molybdenum trioxide in a partial ribbon shape, such as Figure 12As shown, the dark part is molybdenum trioxide that has not been generated in a banded shape, and the light part is molybdenum trioxide that has been generated in a banded shape.
[0066] Comparative Example 3 A molybdenum trioxide and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. The mass ratio of the structure-directing 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-directing agent is 1:1. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 1200°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, take out the corundum boat to obtain the molybdenum trioxide combined together, such as Figure 13 shown.
[0067] Comparative Example 4 A molybdenum trioxide and a preparation method thereof, comprising the following steps: S1. Evenly spread the structure-directing agent on the bottom of the corundum boat, and then put the small pieces of waste molybdenum boat into it. The mass ratio of the structure-directing 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-directing agent is 1:1. S2. Place the corundum boat in a muffle furnace and calcine it with oxygen at a temperature of 800°C for 5 hours; S3. After closing the muffle furnace and cooling to room temperature, take out the corundum boat to obtain layered molybdenum trioxide, such as Figure 14 shown.
[0068] The present invention provides a molybdenum trioxide single crystal ribbon and a method for preparing the same. This method involves contacting a molybdenum source with a structure-directing agent composed of an alkali metal salt and a metal from Group VI other than molybdenum, or an alkaline earth metal salt and a metal from Group VI other than molybdenum, during calcination, followed by cooling to produce the molybdenum trioxide single crystal ribbon. This method eliminates the need for complex template guidance, and the structure-directing agent is readily available. It enables the molybdenum trioxide crystals to grow in a specific direction, resulting in a highly crystalline molybdenum trioxide single crystal ribbon.
[0069] The above description is only a preferred embodiment of the present invention and does not limit the patent scope of the present invention. All equivalent structural transformations made by using the contents of the present invention specification under the inventive concept of the present invention, or direct / indirect application in other related technical fields are included in the patent protection scope of the present invention.
Claims
1. A method for preparing a molybdenum trioxide single crystal ribbon, characterized in that: The steps include: S1, obtaining a molybdenum source; S2, calcining the molybdenum source at a temperature of 800-1100° C. for 5-10 hours, wherein the molybdenum source is in contact with a structure directing agent during the calcination process, and the mass ratio of the structure directing agent to the molybdenum source is 100:(1-6); S3. Cooling to obtain a molybdenum trioxide single crystal ribbon.
2. The method for preparing a molybdenum trioxide single crystal ribbon according to claim 1, wherein: In step S2, the structure directing agent is composed of an alkali metal salt and a metal of the sixth subgroup excluding molybdenum, or an alkaline earth metal salt and a metal of the sixth subgroup excluding molybdenum.
3. The method for preparing a molybdenum trioxide single crystal ribbon according to claim 2, wherein: The mass ratio of the alkali metal salt to the metal of the sixth subgroup excluding molybdenum or the alkaline earth metal salt to the metal of the sixth subgroup excluding molybdenum in the structure directing agent is 1:(1-20).
4. The method for preparing a molybdenum trioxide single crystal ribbon according to claim 3, wherein: The step S3 further includes: cooling to obtain an orthorhombic phase molybdenum trioxide single crystal ribbon.
5. The method for preparing a molybdenum trioxide single crystal ribbon according to claim 1, wherein: In the step S2, the calcination is oxygen calcination.
6. The method for preparing a molybdenum trioxide single crystal ribbon according to claim 1, wherein: In step S1, the molybdenum purity of the molybdenum source is greater than 99%.
7. The method for preparing a molybdenum trioxide single crystal ribbon according to claim 1, wherein: The step S3 further includes: cooling the obtained molybdenum trioxide single crystal ribbon to be in a flocculent shape.
8. A molybdenum trioxide single crystal ribbon, characterized in that The molybdenum trioxide single crystal ribbon is produced by the method for preparing a molybdenum trioxide single crystal ribbon according to any one of claims 1 to 7.
9. The molybdenum trioxide single crystal ribbon according to claim 8, characterized in that: The molybdenum trioxide single crystal ribbon is an orthorhombic phase molybdenum trioxide single crystal ribbon.
10. The molybdenum trioxide single crystal ribbon according to claim 9, characterized in that: The average width of the orthorhombic molybdenum trioxide single crystal ribbon is 25-60 μm.
Citation Information
Patent Citations
Preparation method for centimeter-scale single crystal molybdenum trioxide nano-tape
CN106629850A
JMZ-5 and JMZ-6, zeolites having SZR-type crystal structure, and methods of their preparation and use
CN109843803A
Preparation method of centimeter-level molybdenum trioxide single crystal
CN113186590A
Organic-inorganic hybrid thin film and its manufacturing method
JP2005179115A
P-type semiconductor material, and photoelectric conversion device manufacture method
JP2013211397A