An intelligent production process for magnesium deposition hydrogen storage materials

Abstract

The present application relates to the technical field of magnesium deposition hydrogen storage material production, and specifically to an intelligent production process for magnesium deposition hydrogen storage material, the process comprising: ultrasonically cleaning a porous copper mesh; injecting precious metal ions into the porous copper mesh; preparing copper oxide nanowires at high temperature; obtaining temperature field data at each acquisition moment during the high-temperature oxidation process of the copper oxide nanowires; determining a temperature adjustment coefficient based on the uniformity and stability of the distribution between different temperature data in the temperature field; adjusting the temperature during the high-temperature oxidation process of the copper oxide nanowires according to the real-time temperature adjustment coefficient; oxidizing titanium oxide-coated copper oxide nanowires; and depositing magnesium on the nanowires to obtain magnesium deposition hydrogen storage materials. The present application aims to solve the problem of poor growth quality of copper oxide nanowires due to excessively high or low high-temperature oxidation temperatures, improve the quality of the prepared materials, and thereby obtain magnesium deposition hydrogen storage materials with better hydrogen storage performance.

Description

Technical Field

[0001] The present application relates to the technical field of magnesium deposition hydrogen storage material production, and specifically to an intelligent production process for magnesium deposition hydrogen storage material. Background Art

[0002] With the growth of energy demand and the intensification of environmental pollution, the development and utilization of clean, renewable energy sources has become increasingly important. Hydrogen, as a clean and efficient energy carrier with high energy density, can be produced through various methods such as water electrolysis and biomass conversion, making it the key to achieving energy transformation. Since the storage and transportation of hydrogen are key technical challenges in realizing hydrogen energy applications, and hydrogen is flammable, explosive, and easily diffusible, the development of efficient and safe hydrogen storage materials is particularly important.

[0003] Nanostructured materials with high surface area and high hydrogen storage performance can be formed using high-temperature oxidation, ion implantation, sol-gel, and magnetic filtration deposition methods at low cost and with low activation energy. However, in the process of preparing hydrogen storage materials using these technologies, the high-temperature oxidation temperature must be strictly controlled. If the high-temperature oxidation temperature is too low, the growth of copper oxide nanowires may be insufficient, affecting the material's hydrogen storage performance. If the high-temperature oxidation temperature is too high, the copper oxide nanowires may not grow preferentially, reducing the specific surface area and affecting the material's hydrogen storage capacity. Summary of the Invention

[0004] In order to solve the above technical problems, the present application provides an intelligent production process for magnesium deposition hydrogen storage materials to solve the existing problems.

[0005] The intelligent production process of magnesium deposition hydrogen storage material in this application adopts the following technical solutions:

[0006] One embodiment of the present application provides an intelligent production process for magnesium deposition hydrogen storage materials, the process comprising the following steps:

[0007] S1, ultrasonic cleaning of porous copper mesh;

[0008] S2, implanting noble metal ions into the porous copper mesh;

[0009] S3, preparing copper oxide nanowires at high temperature; during the high-temperature oxidation process of preparing the copper oxide nanowires, the process of adjusting the high-temperature oxidation temperature is specifically as follows:

[0010] Obtain temperature field data at each acquisition moment during the high-temperature oxidation process of copper oxide nanowires;

[0011] Divide isotherms based on different temperature data in the temperature field, and determine the high-temperature oxidation uniformity coefficient based on the uniform distribution characteristics between different isotherms;

[0012] Determine the temperature adjustment coefficient based on the stability characteristics of the high-temperature oxidation uniformity coefficient in the high-temperature oxidation range;

[0013] Adjusting the temperature during the high-temperature oxidation process of copper oxide nanowires according to a real-time temperature adjustment coefficient;

[0014] S4, titanium dioxide film wrapped around copper oxide nanowires was prepared by sol-gel method;

[0015] S5, performing magnesium deposition on the nanowires to obtain a magnesium-deposited hydrogen storage material.

[0016] Preferably, the porous copper mesh used in S1 has a thickness of 0.5-1.5 mm and a mesh size of 800-1000 meshes.

[0017] Preferably, the ion beam current set in S2 is 0.4-0.8 mA, and the pulse width is 80-140 .

[0018] Preferably, the method for determining the high-temperature oxidation uniformity coefficient includes:

[0019] Connect all data points with equal temperature values ​​in the temperature field to obtain isotherms at various temperatures;

[0020] The minimum temperature point closest to the center point of the temperature field is recorded as the end point of the thermal radiation; with the thermal radiation end point as the center, a line is extended through the thermal radiation end point in the direction of its preset neighborhood, and the last intersection point between the line in each direction and each isotherm is recorded as the starting point of the thermal radiation in each direction;

[0021] Determine the isothermal interval factor based on the position and angle distribution of the thermal radiation starting points of different isotherms in the same direction;

[0022] The difference between the highest temperature and the lowest temperature in the temperature field is taken as the temperature range; the cumulative information entropy of all thermal radiation starting point temperature values ​​on all isotherms is taken as the isothermal distribution disorder;

[0023] Based on the temperature extreme difference and the isothermal distribution disorder, the high-temperature oxidation sufficiency factor is determined; wherein the high-temperature oxidation sufficiency factor at time t is The calculation formula is: ; is the temperature extreme difference in the temperature field at moment t; is the isothermal distribution chaos in the temperature field at time t; Adjust parameters for presets;

[0024] The normalized value of the ratio of the high-temperature oxidation sufficiency factor to the isothermal interval factor is calculated as the high-temperature oxidation uniformity coefficient.

[0025] Preferably, the method for determining the isothermal interval factor includes:

[0026] The cumulative result of the distances between the heat radiation end point and the heat radiation starting points on all isothermal lines in the preset neighborhood direction is taken as the isothermal distance;

[0027] The heat radiation starting points in each neighborhood direction are arranged in ascending order of temperature value to form an isothermal interval sequence in each neighborhood direction; in each neighborhood direction, the cosine similarity between the heat radiation end point and the connecting line of all heat radiation starting points in the isothermal interval sequence is accumulated and recorded as the neighborhood similarity in each neighborhood direction, and the reciprocal of the accumulated result of the neighborhood similarity in all neighborhood directions is used as the isothermal interval deviation;

[0028] The product of the isothermal distance and the isothermal interval deviation is used as the isothermal interval factor.

[0029] Preferably, the method for determining the temperature adjustment coefficient includes:

[0030] Setting a preset time interval as a high-temperature oxidation interval; forming a high-temperature oxidation uniformity sequence with all high-temperature oxidation uniformity coefficients within the high-temperature oxidation interval;

[0031] Clustering algorithm is used to obtain several clusters and their cluster centers of high-temperature oxidation uniform sequence, and the cluster centers are recorded as feature points.

[0032] taking the difference between the high-temperature oxidation uniformity coefficients of all characteristic points in the high-temperature oxidation uniformity sequence as the characteristic point high-temperature oxidation difference;

[0033] The reciprocal of the difference between all characteristic points in the high-temperature oxidation uniform sequence and the data mean in the corresponding cluster is used as the interval uniform steady-state factor;

[0034] Based on the high-temperature oxidation difference of the characteristic point and the uniform steady-state factor of the interval, the high-temperature oxidation stability factor is determined; among them, the high-temperature oxidation stability factor of the nth high-temperature oxidation interval is The calculation formula is: ; 、 are the interval uniform steady-state factor of the nth high-temperature oxidation interval and the high-temperature oxidation difference of the characteristic point; Adjust parameters for presets;

[0035] The average value of the high-temperature oxidation uniformity coefficient at all times in the high-temperature oxidation interval is regarded as the high-temperature oxidation sufficiency state;

[0036] The normalized value of the product of the high-temperature oxidation stability factor and the high-temperature oxidation sufficiency condition is used as the temperature adjustment coefficient.

[0037] Preferably, the temperature adjustment process during the high-temperature oxidation of the copper oxide nanowires includes: setting a temperature adjustment threshold; when the real-time temperature adjustment coefficient is greater than or equal to the temperature adjustment threshold, increasing the high-temperature oxidation temperature by a preset degree; otherwise, not adjusting the high-temperature oxidation temperature.

[0038] Preferably, the length of the copper oxide nanowires prepared in S3 is 40-80 , density is 20-40 .

[0039] Preferably, the solution prepared by the sol-gel method in S4 comprises tetrabutyl titanate, anhydrous ethanol, nitric acid, and glacial acetic acid.

[0040] Preferably, during the magnesium deposition process in S5, the arc starting current is set to 50-80 A and the deposition time is set to 2-3 minutes.

[0041] This application has at least the following beneficial effects:

[0042] The present application realizes the adjustment of the high-temperature oxidation temperature during the preparation of hydrogen storage materials. Compared with the prior art, the high-temperature oxidation temperature does not take into account the growth of copper oxide nanowires. When the temperature is too high or too low, the copper oxide nanowires may not grow sufficiently or cannot grow preferentially, thereby affecting the hydrogen storage capacity of the material. The present application divides isotherms by temperature field data during the high-temperature oxidation of copper oxide nanowires, obtains a high-temperature oxidation uniformity coefficient based on the uniform characteristics of the isotherms, and comprehensively considers the distance and difference characteristics between the isotherms formed during the high-temperature oxidation of copper oxide nanowires, more accurately reflecting the high-temperature oxidation uniformity of copper oxide nanowires based on the moment level; obtains a temperature adjustment coefficient based on the stable characteristics of the high-temperature oxidation uniformity coefficient within the high-temperature oxidation range, further analyzes the growth stability of copper oxide nanowires on the basis of the uniform growth of copper oxide nanowires, and can adjust the high-temperature oxidation temperature according to the growth status of copper oxide nanowires, thereby solving the problem of poor growth quality of copper oxide nanowires due to too high or too low high-temperature oxidation temperature, improving the quality of the prepared material, and thus obtaining a magnesium deposition hydrogen storage material with better hydrogen storage performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] In order to more clearly illustrate the technical solutions and advantages of the embodiments of the present application or the prior art, the following is a brief introduction to 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 application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0044] Figure 1A flow chart of an intelligent production process for magnesium deposition hydrogen storage materials provided in one embodiment of the present application;

[0045] Figure 2 A flowchart of the steps of the high-temperature oxidation temperature adjustment process provided in one embodiment of the present application;

[0046] Figure 3 A schematic diagram of a two-dimensional thermocouple network of a vacuum molybdenum rod furnace sample holder according to one embodiment of the present application;

[0047] Figure 4 A flowchart for constructing an indicator of a high-temperature oxidation uniformity coefficient provided in one embodiment of the present application;

[0048] Figure 5 A flowchart for constructing an indicator of a temperature adjustment coefficient provided in one embodiment of the present application. DETAILED DESCRIPTION

[0049] To further illustrate the technical means and effectiveness of this application's implementation of the intended invention, the following, in conjunction with the accompanying drawings and preferred embodiments, details the specific implementation, structure, features, and effectiveness of an intelligent production process for magnesium-deposited hydrogen storage materials proposed in this application. In the following description, references to "one embodiment" or "another embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.

[0050] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.

[0051] The specific solution of the intelligent production process of magnesium deposition hydrogen storage material provided by the present application is described in detail below with reference to the accompanying drawings.

[0052] One embodiment of the present application provides an intelligent production process for magnesium deposition hydrogen storage materials.

[0053] Specifically, the following intelligent production process of magnesium deposition hydrogen storage material is provided, please refer to Figure 1 , the process comprises the following steps:

[0054] S1. Ultrasonic cleaning of the porous copper mesh. The porous copper mesh used in this application has a thickness of 0.5-1.5 mm and a mesh size of 800-1000. Using a porous copper mesh with a mesh size range of 800-1000 can more stably achieve nanowire growth during the high-temperature oxidation stage and simultaneously achieve storage of different volumes of hydrogen.

[0055] In the first embodiment of the present application, the porous copper mesh used has a thickness of 0.5 mm and a mesh size of 1000.

[0056] In the second embodiment of the present application, the porous copper mesh used has a thickness of 1.5 mm and a mesh size of 900.

[0057] In the third embodiment of the present application, the porous copper mesh used has a thickness of 1.2 mm and a mesh size of 800.

[0058] S2, injecting precious metal ions into the porous copper mesh. In this application, when injecting the metal ion source into the porous copper mesh, the ion beam current is set to 0.4-0.8mA and the pulse width is 80-140 , the injected metal is Ag, Au, Pt, etc., the injection energy is 2-4.5KeV, and the dose is 1.0 1.0 / The use of precious metal injection is conducive to the formation of defects on the surface of the porous copper mesh, that is, areas with high surface energy, which enable copper oxide nanowires to grow preferentially during high-temperature oxidation and can adjust the size and length of the growing nanowires.

[0059] In the first embodiment of the present application, the ion beam current is set to 0.8 mA and the pulse width is 100 .

[0060] In the second embodiment of the present application, the ion beam current is set to 0.4 mA and the pulse width is 80 .

[0061] In the third embodiment of the present application, the ion beam current is set to 0.6 mA and the pulse width is 140 .

[0062] S3, high temperature preparation of copper oxide nanowires. Copper oxide nanowires were prepared using a VHSgr-20 / 20 / 30-2000 vacuum molybdenum rod furnace at a temperature of 500-700°C, a pressure of 10 Pa, and an oxygen atmosphere. The length of the prepared copper oxide nanowires was 40-80 mm. , density is 20-40 .

[0063] In order to prevent the problem of insufficient growth of copper oxide nanowires caused by excessively high or low high temperature oxidation temperature, the present application adjusts the temperature during the high temperature oxidation process of copper oxide nanowires. The flow chart of the high temperature oxidation temperature adjustment process is shown in the attached figure. Figure 2 As shown, specifically:

[0064] The first step is to obtain the temperature field data at each acquisition moment during the high-temperature oxidation process of the copper oxide nanowires.

[0065] Thermocouples are evenly placed on the sample rack of the VHSgr-20 / 20 / 30-2000 vacuum molybdenum rod furnace to form a two-dimensional network with the same side length, and the connecting segments of the thermocouples are connected to the data acquisition module of the vacuum molybdenum rod furnace. After the thermocouples are calibrated, the high-temperature preparation process of copper oxide nanowires is started and the temperature field T (x, y, a, t) of the copper oxide nanowires is obtained, where x and y are the horizontal and vertical coordinates of the material, t is the time, and a is the temperature at the coordinate (x, y) at time t. In this embodiment, the temperature field data acquisition time interval is set to 2s, and the implementer can set the acquisition time interval according to the actual situation.

[0066] In order to prevent the temperature data from being missing due to sensor transmission failure, the mean filling method is used to fill the temperature data in the temperature field data. Since the mean filling method is a well-known technology, the specific acquisition process will not be described in detail.

[0067] In this embodiment, the schematic diagram of the two-dimensional thermocouple network of the vacuum molybdenum rod furnace sample holder is shown in the attached figure. Figure 3 shown. Figure 3 The number 1 is a thermocouple, and the number 2 is a two-dimensional thermocouple network.

[0068] At this point, the temperature field data at each acquisition moment during the high-temperature oxidation process of copper oxide nanowires can be obtained in real time.

[0069] In the second step, isotherms are divided based on different temperature data in the temperature field, and the high-temperature oxidation uniformity coefficient is determined based on the uniform distribution characteristics between different isotherms.

[0070] In the intelligent production process of magnesium deposition hydrogen storage materials, the uniformity of the temperature field is one of the key factors to ensure the quality of copper oxide nanowires. When the high-temperature oxidation growth of copper oxide nanowires is more uniform, the local overcooling and local overheating phenomena that cause structural defects of copper oxide nanowires are more minor; secondly, when the stability of the temperature field is higher, the growth rate of copper oxide nanowires is more uniform. The uniform temperature gradient can also improve the growth quality of copper oxide nanowires, which helps to improve the adsorption capacity and cycle stability of subsequent hydrogen storage materials.

[0071] The temperature field data at time t during the preparation of copper oxide nanowires are taken as an example for analysis. All data points with equal temperature values ​​at time t are connected to obtain isotherms at various temperatures.

[0072] The minimum temperature point of the temperature field closest to the thermocouple is recorded as the thermal radiation end point. With the thermal radiation end point as the center, a line is extended through the thermal radiation end point in the eight neighborhood directions. The last intersection between the line in each direction and each isotherm is recorded as the thermal radiation starting point in each direction, and the direction from the thermal radiation starting point to the thermal radiation end point is recorded as the thermal radiation direction.

[0073] The isothermal interval factor of the copper oxide nanowires at any time can be determined by the isothermal distance and the isothermal interval deviation. Specifically, in one embodiment of the present application, the isothermal interval factor is the product of the isothermal distance and the isothermal interval deviation.

[0074] The isothermal distance of the copper oxide nanowire at any time can be calculated by summing the distances between the thermal radiation endpoint and the thermal radiation starting point on all isothermal lines in its eight-neighborhood direction. In this embodiment, the distance is calculated using Euclidean distance. In other embodiments of the present application, the distance between the thermal radiation endpoint and the thermal radiation starting point can also be determined using Manhattan distance, Chebyshev distance, or other methods.

[0075] It should be understood that when the high-temperature oxidation growth condition of copper oxide nanowires is better, the thermal radiation rate in the temperature field is faster, the isothermal distance is shorter, and the distance between the thermal radiation end point and each thermal radiation starting point in the temperature field is smaller.

[0076] The starting points of thermal radiation in each neighborhood direction in the temperature field are arranged in ascending order of temperature values ​​to form an isothermal interval sequence in each neighborhood direction.

[0077] For the isothermal interval deviation of copper oxide nanowires at any time, the cosine similarity between the end point of thermal radiation and the connection line of all thermal radiation starting points in the isothermal interval sequence is accumulated in each neighborhood direction, which is recorded as the neighborhood similarity in each neighborhood direction. The reciprocal of the accumulated result of the neighborhood similarity in all neighborhood directions is taken as the isothermal interval deviation.

[0078] It should be understood that when the high-temperature oxidation growth quality of copper oxide nanowires is higher, the phenomenon of uniform temperature gradient in the temperature field is more significant, the isothermal interval deviation is smaller, and further, the cosine similarity between the connection lines of all thermal radiation starting points in the corresponding isothermal interval sequence in all neighborhood directions is greater.

[0079] For the high-temperature oxidation uniformity coefficient of copper oxide nanowires at any time, the normalized value of the ratio of the high-temperature oxidation sufficient factor to the isothermal interval factor can be determined. When the isothermal interval factor is 0, the high-temperature oxidation sufficient factor is divided by the adjustment parameter The ratio of is used as the high temperature oxidation uniformity coefficient. In this embodiment, the adjustment parameters The value is 0.1.

[0080] The high temperature oxidation sufficient factor at any time can be obtained by the following calculation method: For example: ;in, is the high temperature oxidation sufficient factor at time t; is the temperature extreme difference in the temperature field at moment t; is the isothermal distribution chaos in the temperature field at time t; It is a preset adjustment parameter, and in this embodiment, the value is 1 to prevent the denominator from being 0.

[0081] The temperature extreme difference is obtained by the difference between the highest temperature and the lowest temperature in the temperature field; and the isothermal distribution disorder is obtained by the accumulation of the information entropy of all thermal radiation starting points on all isotherms.

[0082] It should be understood that when the growth condition of the copper oxide nanowires is more fully and uniformly, the high-temperature oxidation uniformity coefficient is greater, the isothermal interval factor is smaller, and the high-temperature oxidation sufficiency factor is greater. Furthermore, the phenomenon of uneven temperature gradient during the high-temperature oxidation of the copper oxide nanowires due to improper high-temperature oxidation temperature is less obvious. At this time, there is no need to adjust the high-temperature oxidation temperature of the copper oxide nanowires.

[0083] At this point, the high-temperature oxidation uniformity coefficient of the copper oxide nanowires can be obtained in real time according to the above method.

[0084] In this application, the high temperature oxidation uniformity coefficient index construction flow chart is as shown in the attached Figure 4 shown.

[0085] The third step is to determine the temperature adjustment coefficient based on the stable characteristics of the high-temperature oxidation uniformity coefficient in the high-temperature oxidation range.

[0086] Set every 10 minutes as a high-temperature oxidation interval. For any high-temperature oxidation interval, the sequence of the high-temperature oxidation uniformity coefficients of all copper oxide nanowires in chronological order is recorded as the high-temperature oxidation uniformity sequence of the high-temperature oxidation interval.

[0087] The high-temperature oxidation uniform sequence is used as input, and the K-means clustering algorithm is used to obtain the clusters and cluster centers of the high-temperature oxidation uniform sequence. The cluster centers are recorded as feature points, where the number of cluster centers K is set to 10. A larger K value provides more accurate monitoring of the high-temperature oxidation reaction of copper oxide nanowires. The number of cluster centers can be set by the user based on actual conditions. In this embodiment, the K-means clustering algorithm is used for clustering. In other embodiments, the DBSCAN clustering algorithm or other suitable clustering algorithms can also be used.

[0088] It should be understood that the beneficial effect of using the K-means clustering algorithm to obtain feature points and clusters is to avoid the subsequent analysis of the high-temperature oxidation stability of copper oxide nanowires, where the data in the entire high-temperature oxidation range are analyzed uniformly, and the change in the high-temperature oxidation uniformity coefficient of the copper oxide nanowires in the high-temperature oxidation range is ignored as a process, which leads to subsequent misjudgment of the high-temperature oxidation stability of the copper oxide nanowires.

[0089] For any high-temperature oxidation interval, the high-temperature oxidation stability factor can be determined by the high-temperature oxidation difference of the characteristic point and the interval uniform steady-state factor. Specifically, in this embodiment, it can be calculated as follows, taking the high-temperature oxidation stability factor of the nth high-temperature oxidation interval as an example: ;in, is the high temperature oxidation stability factor of the nth high temperature oxidation interval; 、 are the interval uniform steady-state factor of the nth high-temperature oxidation interval and the high-temperature oxidation difference of the characteristic point; This is a preset adjustment parameter, and in this embodiment, the value is 0.1 to prevent the denominator from being 0.

[0090] For any high-temperature oxidation interval, the high-temperature oxidation difference of the characteristic point is determined by the difference between the high-temperature oxidation uniformity coefficients of all characteristic points in the high-temperature oxidation uniformity sequence corresponding to the high-temperature oxidation interval.

[0091] In one embodiment of the present application, the difference between the high temperature oxidation uniformity coefficients of all characteristic points is set to: the cumulative result of the absolute value of the difference between the high temperature oxidation uniformity coefficients of all characteristic points. In other embodiments of the present application, other suitable difference calculation methods can also be used to obtain the result.

[0092] It should be understood that when the growth process of the copper oxide nanowires in the high temperature oxidation zone is more stable, the high temperature oxidation stability factor is larger and the high temperature oxidation difference of the characteristic points is smaller.

[0093] For any high-temperature oxidation interval, the interval uniform steady-state factor is the inverse of the difference between all characteristic points and the data mean in their corresponding clusters.

[0094] It should be understood that when the growth process of the copper oxide nanowires in the high-temperature oxidation interval is more uniform and stable, the high-temperature oxidation stability factor is larger, the interval uniform steady-state factor is larger, and further, the cumulative difference between the mean values ​​of all feature points and all data in their corresponding clusters is smaller.

[0095] For any high-temperature oxidation interval, the temperature adjustment coefficient can be determined based on the high-temperature oxidation stability factor and the high-temperature oxidation sufficiency condition. Specifically, in this embodiment, the temperature adjustment coefficient is the normalized value of the product of the high-temperature oxidation stability factor and the high-temperature oxidation sufficiency condition.

[0096] It should be understood that when the growth quality of copper oxide nanowires is higher and the growth rate is more stable, the high-temperature oxidation stability factor is larger, the difference in high-temperature oxidation of characteristic points is smaller, and the interval uniform steady-state factor is larger, then there is no need to adjust the high-temperature oxidation temperature of the copper oxide nanowires.

[0097] The high-temperature oxidation sufficiency in the high-temperature oxidation interval is the average of the high-temperature oxidation uniformity coefficients at all times within the high-temperature oxidation interval. It should be understood that, as the growth quality of the copper oxide nanowires in the high-temperature oxidation interval increases, the high-temperature oxidation sufficiency becomes more pronounced, i.e., the average of the high-temperature oxidation uniformity coefficients at all times within the high-temperature oxidation interval increases, and in this case, there is less need to adjust the high-temperature oxidation temperature of the copper oxide nanowires.

[0098] At this point, the temperature adjustment coefficient of the copper oxide nanowires in each high-temperature oxidation zone can be obtained in real time according to the above method.

[0099] In this application, the indicator construction flow chart of the temperature adjustment coefficient is as shown in the attached Figure 5 shown.

[0100] The fourth step is to adjust the temperature of the copper oxide nanowires during the high-temperature oxidation process according to the real-time temperature adjustment coefficient.

[0101] A temperature adjustment threshold W is set. When the temperature adjustment coefficient obtained in real time is greater than or equal to the temperature adjustment threshold W, it is considered that the high-temperature oxidation temperature of the copper oxide nanowires is low at this time, the growth of the copper oxide nanowires in the high-temperature oxidation vacuum environment is insufficient, and the high-temperature oxidation temperature needs to be increased by A°C; when the temperature adjustment coefficient obtained in real time is less than the temperature adjustment threshold W, it is considered that the high-temperature oxidation temperature of the copper oxide nanowires is appropriate at this time, and there is no need to adjust the high-temperature oxidation temperature.

[0102] Among them, the temperature adjustment threshold W ranges from [0, 1]. The higher the value of W, the stricter the requirements for the high-temperature oxidation process of copper oxide nanowires. In one embodiment of the present application, W is 0.6 and A is 20. The implementer can set the values ​​of the temperature adjustment threshold W and the adjustment amplitude A according to actual conditions.

[0103] Thus, the temperature adjustment during the high-temperature oxidation process of copper oxide nanowires can be achieved according to the above method, and copper oxide nanowires with good quality can be obtained for the subsequent preparation of magnesium deposition hydrogen storage materials.

[0104] S4, using a sol-gel method to prepare a titanium dioxide film wrapped around the copper oxide nanowires. The solution prepared by the sol-gel method in this application includes tetrabutyl titanate, anhydrous ethanol, nitric acid, and glacial acetic acid. The thickness of the wrapping film layer is 0.2-0.8 Copper oxide nanowires can serve as a scaffold for high-surface-area nanomaterials and can also subsequently form a composite semiconductor with titanium dioxide to improve hydrogen absorption efficiency.

[0105] S5, magnesium deposition is performed on the nanowires to obtain magnesium deposition hydrogen storage material. In the process of obtaining magnesium deposition hydrogen storage material by magnetic filtration technology, the present application sets the arc starting current to 50-80A, the oxygen flow rate to 0-80sccm, and the vacuum degree to 2 6 Pa, the deposition time is 2-3min, and the deposition thickness does not exceed 4nm; the voltage of the high power pulse bias is set to 1-5KV, the pulse width is 2-4 The pulse frequency is 1-180Hz, the duty cycle is 1 / 8500-1 / 5500, and the peak power is 2-5MW. Using nano-magnesium as a nano-dot on the surface of titanium dioxide can greatly improve the hydrogen absorption efficiency while reducing the hydrogen release temperature and decomposition activation energy.

[0106] In the first embodiment of the present application, the arc starting current is set to 80A and the deposition time is set to 2 minutes.

[0107] In the second embodiment of the present application, the arc starting current is set to 70A and the deposition time is set to 2.5 minutes.

[0108] In the third embodiment of the present application, the arc starting current is set to 50A and the deposition time is set to 3 minutes.

[0109] The magnesium deposited hydrogen storage material prepared in this application was tested, and the test results showed that the hydrogen release temperature was 63.8° C. and the decomposition activation energy was 63.4 KJ / mol.

[0110] Thus, an intelligent production process of magnesium deposition hydrogen storage material can be realized according to the above method, and magnesium deposition hydrogen storage material with better quality can be prepared.

[0111] The various embodiments in this specification are described in a progressive manner, and the same or similar parts between the various embodiments can be referred to each other. Each embodiment focuses on the differences from other embodiments.

[0112] It should be noted that, unless otherwise specified and limited, terms such as "include", "comprising" or any other variations thereof are intended to cover non-exclusive inclusion, so that a circuit structure, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such article or device. In the absence of further restrictions, the phrase "including a ..." defines an element, does not exclude the presence of other identical elements in the article or device including the element. In addition, the term "and\or" used herein includes any and all combinations of one or more related listed items.

[0113] Those skilled in the art will readily appreciate other embodiments of the present application after considering the specification and practicing the invention herein. This application is intended to cover any variations, uses, or adaptations of the present application that follow the general principles of the present application and include common knowledge or customary techniques in the art not invented herein.

[0114] It will be understood that the present application is not limited to the exact construction that has been described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof.

Claims

1. An intelligent production process for magnesium deposition hydrogen storage materials, characterized in that: The process includes the following steps: S1, ultrasonic cleaning of porous copper mesh; S2, implanting noble metal ions into the porous copper mesh; S3, preparing copper oxide nanowires at high temperature; during the high-temperature oxidation process of preparing the copper oxide nanowires, the process of adjusting the high-temperature oxidation temperature is specifically as follows: Obtain temperature field data at each acquisition moment during the high-temperature oxidation process of copper oxide nanowires; Divide isotherms based on different temperature data in the temperature field, and determine the high-temperature oxidation uniformity coefficient based on the uniform distribution characteristics between different isotherms; Determine the temperature adjustment coefficient based on the stability characteristics of the high-temperature oxidation uniformity coefficient in the high-temperature oxidation range; Adjusting the temperature during the high-temperature oxidation process of copper oxide nanowires according to a real-time temperature adjustment coefficient; S4, titanium dioxide film wrapped around copper oxide nanowires was prepared by sol-gel method; S5, depositing magnesium on the nanowires to obtain a magnesium-deposited hydrogen storage material; The method for determining the high-temperature oxidation uniformity coefficient includes: Connect all data points with equal temperature values ​​in the temperature field to obtain isotherms at various temperatures; The minimum temperature point closest to the center point of the temperature field is recorded as the end point of the thermal radiation; with the thermal radiation end point as the center, a line is extended through the thermal radiation end point in the direction of its preset neighborhood, and the last intersection point between the line in each direction and each isotherm is recorded as the starting point of the thermal radiation in each direction; Determine the isothermal interval factor based on the position and angle distribution of the thermal radiation starting points of different isotherms in the same direction; The difference between the highest temperature and the lowest temperature in the temperature field is taken as the temperature range; the cumulative information entropy of all thermal radiation starting point temperature values ​​on all isotherms is taken as the isothermal distribution disorder; Based on the temperature extreme difference and the isothermal distribution disorder, the high-temperature oxidation sufficiency factor is determined; wherein the high-temperature oxidation sufficiency factor at time t is The calculation formula is: ; is the temperature extreme difference in the temperature field at moment t; is the isothermal distribution chaos in the temperature field at time t; Adjust parameters for presets; Calculate the normalized value of the ratio of the high-temperature oxidation sufficiency factor to the isothermal interval factor as the high-temperature oxidation uniformity coefficient; The method for determining the temperature adjustment coefficient includes: Setting a preset time interval as a high-temperature oxidation interval; forming a high-temperature oxidation uniformity sequence with all high-temperature oxidation uniformity coefficients within the high-temperature oxidation interval; Clustering algorithm is used to obtain several clusters and their cluster centers of high-temperature oxidation uniform sequence, and the cluster centers are recorded as feature points. taking the difference between the high-temperature oxidation uniformity coefficients of all characteristic points in the high-temperature oxidation uniformity sequence as the characteristic point high-temperature oxidation difference; The reciprocal of the difference between all characteristic points in the high-temperature oxidation uniform sequence and the data mean in the corresponding cluster is used as the interval uniform steady-state factor; Based on the high-temperature oxidation difference of the characteristic point and the uniform steady-state factor of the interval, the high-temperature oxidation stability factor is determined; among them, the high-temperature oxidation stability factor of the nth high-temperature oxidation interval is The calculation formula is: ; 、 are the interval uniform steady-state factor of the nth high-temperature oxidation interval and the high-temperature oxidation difference of the characteristic point; Adjust parameters for presets; The average value of the high-temperature oxidation uniformity coefficient at all times in the high-temperature oxidation interval is regarded as the high-temperature oxidation sufficiency state; The normalized value of the product of the high-temperature oxidation stability factor and the high-temperature oxidation sufficiency condition is used as the temperature adjustment coefficient; Wherein, the method for determining the isothermal interval factor includes: The cumulative result of the distances between the heat radiation end point and the heat radiation starting points on all isothermal lines in the preset neighborhood direction is taken as the isothermal distance; The heat radiation starting points in each neighborhood direction are arranged in ascending order of temperature value to form an isothermal interval sequence in each neighborhood direction; in each neighborhood direction, the cosine similarity between the heat radiation end point and the connecting line of all heat radiation starting points in the isothermal interval sequence is accumulated and recorded as the neighborhood similarity in each neighborhood direction, and the reciprocal of the accumulated result of the neighborhood similarity in all neighborhood directions is used as the isothermal interval deviation; The product of the isothermal distance and the isothermal interval deviation is used as the isothermal interval factor.

2. The intelligent production process of magnesium deposited hydrogen storage material according to claim 1, characterized in that: The porous copper mesh used in S1 has a thickness of 0.5-1.5 mm and a mesh size of 800-1000 meshes.

3. The intelligent production process of magnesium deposition hydrogen storage material according to claim 1, characterized in that: The ion beam current set in S2 is 0.4-0.8 mA, and the pulse width is 80-140 .

4. The intelligent production process of magnesium deposition hydrogen storage material according to claim 1, characterized in that: The temperature adjustment process during the high-temperature oxidation of copper oxide nanowires includes: setting a temperature adjustment threshold; when the real-time temperature adjustment coefficient is greater than or equal to the temperature adjustment threshold, increasing the high-temperature oxidation temperature by a preset degree; otherwise, not adjusting the high-temperature oxidation temperature.

5. The intelligent production process of magnesium deposition hydrogen storage material according to claim 1, characterized in that: The length of the copper oxide nanowires prepared in S3 is 40-80 , density is 20-40 .

6. The intelligent production process of magnesium deposition hydrogen storage material according to claim 1, characterized in that: The solution prepared by the sol-gel method in S4 includes tetrabutyl titanate, anhydrous ethanol, nitric acid, and glacial acetic acid.

7. The intelligent production process of magnesium deposition hydrogen storage material according to claim 1, characterized in that: In the process of magnesium deposition in S5, the arc starting current is set to 50-80A and the deposition time is set to 2-3 minutes.

Images