Intelligent production process of magnesium deposition hydrogen storage material

Abstract

The invention relates to the technical field of magnesium deposition hydrogen storage material production, in particular to an intelligent production process of a magnesium deposition hydrogen storage material. Injecting noble metal ions into the porous copper net; preparing a copper oxide nanowire at high temperature; the method comprises the following steps: acquiring temperature field data at each acquisition moment in a high-temperature oxidation process of preparing a copper oxide nanowire; determining a temperature adjustment coefficient based on the distribution uniformity characteristic and stability of different temperature data in the temperature field; adjusting the temperature of the copper oxide nanowire in the high-temperature oxidation process according to the real-time temperature adjustment coefficient; oxidizing the copper oxide nanowire wrapped by the titanium oxide; and performing magnesium deposition on the nanowire to obtain the magnesium deposition hydrogen storage material. The invention aims to solve the problem of poor growth quality of the copper oxide nanowire due to too high or too low high-temperature oxidation temperature, improve the quality of the prepared material, and further obtain the magnesium deposition hydrogen storage material with better hydrogen storage performance.

Description

Technical Field

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

[0002] With the growth of energy demand and the intensification of environmental pollution problems, it has become particularly important to develop and utilize clean and renewable energy. As a clean and efficient energy carrier, hydrogen energy has a good energy density and can be produced through various methods such as water electrolysis and biomass conversion. It is the key to achieving energy transformation. Since the storage and transportation of hydrogen are key technical problems in the application of hydrogen energy, and hydrogen has the characteristics of being flammable, explosive, and easy to diffuse, it is particularly important to develop high-efficiency and safe hydrogen storage materials.

[0003] Based on high-temperature oxidation, ion implantation, sol-gel, and magnetic filtration deposition methods, nanostructured materials with high surface area and high hydrogen storage performance can be formed, and the cost is relatively low, and the activation energy is low. However, in the process of preparing hydrogen storage materials using the above technologies, the high-temperature oxidation temperature needs to be strictly controlled. When the high-temperature oxidation temperature is too low, the growth of copper oxide nanowires may be insufficient, affecting the hydrogen storage performance of the material; when the high-temperature oxidation temperature is too high, the copper oxide nanowires may not grow preferentially, reducing the specific surface area and affecting the hydrogen storage capacity of the material. Summary of the Invention

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

[0005] The intelligent production process for magnesium deposition hydrogen storage materials of this application adopts the following technical solutions: An embodiment of this application provides an intelligent production process for magnesium deposition hydrogen storage materials, and this process includes the following steps: S1, ultrasonically clean the porous copper mesh; S2, inject precious metal ions into the porous copper mesh; S3, prepare copper oxide nanowires at high temperature; in the high-temperature oxidation process of preparing copper oxide nanowires, the specific process of adjusting the high-temperature oxidation temperature is as follows: Obtain the 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 characteristics distributed between different isotherms; Determine the temperature adjustment coefficient based on the stable characteristics of the high-temperature oxidation uniformity coefficient within the high-temperature oxidation interval; Adjust the temperature during the high-temperature oxidation process of copper oxide nanowires according to the real-time temperature adjustment coefficient; S4. Prepare a titanium dioxide film coating copper oxide nanowires by sol-gel method to oxidize the copper oxide nanowires coated with titanium oxide. S5. Deposit magnesium on the nanowires to obtain a magnesium-deposited hydrogen storage material.

[0006] Preferably, the thickness of the porous copper mesh used in S1 is 0.5 - 1.5 mm, and the mesh number of the copper mesh is 800 - 1000 meshes.

[0007] Preferably, the ion beam current set in S2 is 0.4 - 0.8 mA, and the pulse width is 80 - 140 .

[0008] Preferably, the method for determining the high-temperature oxidation uniformity coefficient includes: Connect the data points with equal temperature values in the temperature field to obtain isotherms at each temperature; Mark the minimum temperature point closest to the center point of the temperature field as the thermal radiation end point; with the thermal radiation end point as the center, extend the connection line in the direction of its preset neighborhood, and mark the last intersection point between the connection lines in each direction and each isotherm as the thermal radiation start point in each direction; Based on the position and angle distribution of the thermal radiation start points of different isotherms in the same direction, determine the isothermal interval factor; Take the difference between the highest temperature and the lowest temperature in the temperature field as the temperature range; take the cumulative result of the information entropy of all the thermal radiation start point temperature values on all the isotherms as the isothermal distribution disorder; Based on the temperature range and the isothermal distribution disorder, determine the high-temperature oxidation sufficiency factor; where the high-temperature oxidation sufficiency factor at the t-th moment The calculation formula is: ; is the temperature range in the temperature field at the t-th moment; is the isothermal distribution disorder in the temperature field at the t-th moment; is a preset adjustment parameter; 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.

[0009] Preferably, the method for determining the isothermal interval factor includes: Take the cumulative result of the distances between the thermal radiation end point and the thermal radiation start points on all the isotherms in its preset neighborhood direction as the isothermal distance; Arrange the heat radiation starting points in each neighborhood direction into an isothermal interval sequence in ascending order of temperature values; in each neighborhood direction, record the cumulative result of the cosine similarity between the heat radiation end point and the lines connecting all heat radiation starting points in the isothermal interval sequence as the neighborhood similarity in each neighborhood direction, and take the reciprocal of the cumulative result of the neighborhood similarities in all neighborhood directions as the isothermal interval deviation. Take the product of the isothermal distance and the isothermal interval deviation as the isothermal interval factor.

[0010] Preferably, the method for determining the temperature adjustment coefficient includes: Set an interval with a preset duration as the high-temperature oxidation interval; form a high-temperature oxidation uniformity sequence with all high-temperature oxidation uniformity coefficients within the high-temperature oxidation interval. Use a clustering algorithm to obtain several clustering clusters and their clustering centers of the high-temperature oxidation uniformity sequence, and record the clustering centers as characteristic points respectively. Take the difference between the high-temperature oxidation uniformity coefficients of all characteristic points in the high-temperature oxidation uniformity sequence as the high-temperature oxidation difference of the characteristic points. Take the reciprocal of the difference between all characteristic points in the high-temperature oxidation uniformity sequence and the data mean in their corresponding clustering clusters as the interval uniformity steady-state factor. Based on the high-temperature oxidation difference of the characteristic points and the interval uniformity steady-state factor, determine the high-temperature oxidation stability factor; among them, the high-temperature oxidation stability factor of the nth high-temperature oxidation interval The calculation formula is: ; 、 Are respectively the interval uniformity steady-state factor and the high-temperature oxidation difference of the characteristic points in the nth high-temperature oxidation interval; Is a preset adjustment parameter; Take the mean value of the high-temperature oxidation uniformity coefficients at all times in the high-temperature oxidation interval as the high-temperature oxidation sufficiency. Take the normalized value of the product of the high-temperature oxidation stability factor and the high-temperature oxidation sufficiency as the temperature adjustment coefficient.

[0011] 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, raise the high-temperature oxidation temperature by a preset degree; otherwise, do not adjust the high-temperature oxidation temperature.

[0012] Preferably, the length of the copper oxide nanowires prepared and obtained in S3 is 40 - 80 , and the density is 20 - 40 .

[0013] Preferably, the solution prepared by the sol-gel method in S4 includes tetrabutyl titanate, absolute ethanol, nitric acid, and glacial acetic acid.

[0014] Preferably, during the magnesium deposition in S5, the arc starting current is set to 50 - 80 A, and the deposition time is 2 - 3 min.

[0015] This application has at least the following beneficial effects: This application realizes the adjustment of the high-temperature oxidation temperature during the preparation of the hydrogen storage material. Compared with the prior art where the growth condition of copper oxide nanowires is not considered for the high-temperature oxidation temperature, there may be defects such as insufficient growth or failure to preferentially grow of copper oxide nanowires when the temperature is too high or too low, thus affecting the hydrogen storage capacity of the material. In this application, isotherms are divided based on the temperature field data during the high-temperature oxidation of copper oxide nanowires, and the high-temperature oxidation uniformity coefficient is obtained according to the uniform characteristics of the isotherms. The distance and difference characteristics between the isotherms formed during the high-temperature oxidation of copper oxide nanowires are comprehensively considered, which more accurately reflects the high-temperature oxidation uniformity of copper oxide nanowires at the moment level; the temperature adjustment coefficient is obtained based on the stable characteristics of the high-temperature oxidation uniformity coefficient within the high-temperature oxidation range. On the basis of the uniform growth of copper oxide nanowires, the growth stability of copper oxide nanowires is further analyzed, and the high-temperature oxidation temperature can be adjusted according to the growth condition of copper oxide nanowires, solving the problem that the growth quality of copper oxide nanowires is poor 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. Description of the Drawings

[0016] In order to more clearly illustrate the technical solutions and advantages in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0017] Figure 1 It is a flowchart of an intelligent production process of a magnesium deposition hydrogen storage material provided by an embodiment of the present application; Figure 2 It is a flowchart of the steps of the high-temperature oxidation temperature adjustment process provided by an embodiment of the present application; Figure 3 It is a partial schematic diagram of the two-dimensional network of thermocouples of the sample rack in a vacuum molybdenum rod furnace provided by an embodiment of the present application; Figure 4 It is a flowchart of the index construction of the high-temperature oxidation uniformity coefficient provided by an embodiment of the present application; Figure 5Flowchart for constructing the index of the temperature adjustment coefficient provided by an embodiment of the present application. Detailed implementation manners

[0018] In order to further elaborate on the technical means and effects adopted by the present application to achieve the intended invention purpose, the following combines the drawings and preferred embodiments to specifically describe a smart production process of a magnesium deposition hydrogen storage material proposed according to the present application, including its specific implementation manners, structures, features and effects in detail. In the following description, different "one embodiment" or "another embodiment" do not necessarily refer to the same embodiment. In addition, the specific features, structures or characteristics in one or more embodiments can be combined in any suitable form.

[0019] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field to which this application belongs.

[0020] The following specifically describes the specific solution of a smart production process of a magnesium deposition hydrogen storage material provided by the present application with reference to the drawings.

[0021] A smart production process of a magnesium deposition hydrogen storage material provided by an embodiment of the present application.

[0022] Specifically, a smart production process of a magnesium deposition hydrogen storage material is provided as follows. Please refer to Figure 1 , and the process includes the following steps: S1, ultrasonically clean the porous copper mesh. The thickness of the porous copper mesh used in the present application is 0.5 - 1.5 mm, and the mesh number of the copper mesh is 800 - 1000. Using a porous copper mesh with a mesh number in the range of 800 - 1000 can more stably achieve the growth of nanowires during the high-temperature oxidation stage and simultaneously achieve the storage of hydrogen with different volumes.

[0023] In the first embodiment of the present application, the thickness of the porous copper mesh used is 0.5 mm, and the mesh number of the copper mesh is 1000.

[0024] In the second embodiment of the present application, the thickness of the porous copper mesh used is 1.5 mm, and the mesh number of the copper mesh is 900.

[0025] In the third embodiment of the present application, the thickness of the porous copper mesh used is 1.2 mm, and the mesh number of the copper mesh is 800.

[0026] S2, inject noble metal ions into the porous copper mesh. When injecting the metal ion source into the porous copper mesh in the present application, the ion beam current is set to 0.4 - 0.8 mA, the pulse width is 80 - 140 , the injected metals are Ag, Au, Pt, etc., the injection energy is 2 - 4.5 KeV, and the dose is 1.0 1.0 / , the adoption of noble metal injection is conducive to forming defects, i.e., regions with high surface energy, on the surface of the porous copper mesh, enabling the preferential growth of copper oxide nanowires during high-temperature oxidation and capable of adjusting the size and length of the grown nanowires.

[0027] In the first embodiment of this application, the ion beam current is set to 0.8 mA and the pulse width is 100 .

[0028] In the second embodiment of this application, the ion beam current is set to 0.4 mA and the pulse width is 80 .

[0029] In the third embodiment of this application, the ion beam current is set to 0.6 mA and the pulse width is 140 .

[0030] S3. Prepare copper oxide nanowires at high temperature. Use a VHSgr-20 / 20 / 30-2000 vacuum molybdenum bar furnace to prepare copper oxide nanowires under the conditions of a temperature of 500 - 700 °C, a pressure of 10 Pa, and an oxygen atmosphere. The length of the prepared copper oxide nanowires is 40 - 80 , and the density is 20 - 40 .

[0031] To prevent the problem of insufficient growth of copper oxide nanowires caused by too high or too low high-temperature oxidation temperature, this application adjusts the temperature during the high-temperature oxidation process of copper oxide nanowires. The step flowchart of the high-temperature oxidation temperature adjustment process is as shown in the appendix Figure 2 , specifically: The first step is to obtain the temperature field data at each acquisition moment during the high-temperature oxidation process of copper oxide nanowires.

[0032] Evenly place the thermocouples on the sample rack of the VHSgr-20 / 20 / 30-2000 vacuum molybdenum bar furnace to form a two-dimensional network with the same side length, and connect the connecting segments of the thermocouples to the data acquisition module of the vacuum molybdenum bar furnace. After calibrating the thermocouples, start the technological process of preparing copper oxide nanowires at high temperature and obtain the temperature field T(x, y, a, t) of the copper oxide nanowires. Among them, x and y are the horizontal and vertical coordinates of the material respectively, t is the moment, and a is the temperature at the coordinate (x, y) at moment t. In this embodiment, the temperature field data acquisition time interval is set to 2 s, and the implementer can set the acquisition time interval according to the actual situation.

[0033] To prevent the occurrence of missing temperature data caused by sensor transmission failures, 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 elaborated too much.

[0034] In this embodiment, a schematic diagram of the two-dimensional network part of the thermocouple of the vacuum molybdenum rod furnace sample holder is shown in the appendix Figure 3 as shown. Figure 3 In , the label 1 is the thermocouple, and 2 is the two-dimensional network of thermocouples.

[0035] So far, the temperature field data at each acquisition moment during the high-temperature oxidation process of copper oxide nanowires can be obtained in real time.

[0036] The second step is to divide the isotherms based on different temperature data in the temperature field, and determine the high-temperature oxidation uniformity coefficient based on the uniform characteristics distributed between different isotherms.

[0037] In the intelligent production process of magnesium-deposited 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 sufficient and uniform, the local overcooling and local overheating phenomena that cause structural defects in copper oxide nanowires are milder; secondly, when the stability of the temperature field is higher, the growth rate of copper oxide nanowires is more uniform, and 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.

[0038] Now, taking the temperature field data at the t-th moment during the preparation process of copper oxide nanowires as an example for analysis, the data points with equal temperature values at the t-th moment are connected to obtain the isotherms at each temperature.

[0039] The minimum temperature point closest to the center point of the temperature field of the thermocouple is recorded as the heat radiation end point. Taking the heat radiation end point as the center, extend the connection lines in the eight neighborhood directions of the heat radiation end point. The last intersection point between the connection lines in each direction and each isotherm is recorded as the heat radiation start point in each direction, and the direction from the heat radiation start point to the heat radiation end point is recorded as the heat radiation direction.

[0040] For the isothermal interval factor of copper oxide nanowires at any moment, it can be determined by the isothermal distance and the isothermal interval deviation. Specifically, in an embodiment of the present application, the isothermal interval factor is the product of the isothermal distance and the isothermal interval deviation.

[0041] For the isothermal distance of copper oxide nanowires at any moment, it can be obtained according to the cumulative result of the distances between the heat radiation end point and the heat radiation start points on all isotherms in its eight neighborhood directions. Among them, in this embodiment, the distance is calculated using the Euclidean distance. In other embodiments of the present application, the Manhattan distance, Chebyshev distance, etc. can also be used to determine the distance between the heat radiation end point and the heat radiation start point.

[0042] It should be understood that when the high-temperature oxidation growth condition of copper oxide nanowires is better, the heat radiation rate in the temperature field is faster, the isothermal distance is shorter, and the distance between the heat radiation end point and each heat radiation start point in the temperature field is smaller.

[0043] Arrange the thermal radiation starting points in each neighborhood direction in the temperature field in ascending order of temperature values to form an isothermal interval sequence in each neighborhood direction.

[0044] For the isothermal interval deviation of copper oxide nanowires at any moment, in each neighborhood direction, the cumulative result of the cosine similarity between the thermal radiation end point and the lines connecting all thermal radiation starting points in the isothermal interval sequence is denoted as the neighborhood similarity in each neighborhood direction. The reciprocal of the cumulative result of the neighborhood similarities in all neighborhood directions is used as the isothermal interval deviation.

[0045] 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 thermal radiation end point and the lines connecting all thermal radiation starting points in the isothermal interval sequence in all neighborhood directions is larger.

[0046] For the high-temperature oxidation uniformity coefficient of copper oxide nanowires at any moment, it can be determined by calculating the normalized value of the ratio of the high-temperature oxidation sufficiency factor to the isothermal interval factor. When the isothermal interval factor is 0, the ratio of the high-temperature oxidation sufficiency factor to the adjustment parameter is used as the high-temperature oxidation uniformity coefficient. In this embodiment, the adjustment parameter is taken as 0.1.

[0047] For the high-temperature oxidation sufficiency factor at any moment, it can be obtained through the following calculation method. Taking the high-temperature oxidation sufficiency factor at the t-th moment as an example: ; where is the high-temperature oxidation sufficiency factor at the t-th moment; is the temperature range in the temperature field at the t-th moment; is the isothermal distribution chaos in the temperature field at the t-th moment; is a preset adjustment parameter, which is taken as 1 in this embodiment to prevent the denominator from being 0.

[0048] Among them, the temperature range is obtained from the difference between the highest temperature and the lowest temperature in the temperature field; the isothermal distribution chaos is the cumulative result of the information entropy of all thermal radiation starting points on all isothermal lines.

[0049] It should be understood that when the growth condition of copper oxide nanowires is more sufficient and uniform, the high-temperature oxidation uniformity coefficient is larger, the isothermal interval factor is smaller, the high-temperature oxidation sufficiency factor is larger, and further, the phenomenon of non-uniform temperature gradient during the high-temperature oxidation of copper oxide nanowires due to inappropriate high-temperature oxidation temperature is less obvious. At this time, it is less necessary to adjust the high-temperature oxidation temperature of copper oxide nanowires.

[0050] So far, the high-temperature oxidation uniformity coefficient of copper oxide nanowires can be obtained in real time according to the above method.

[0051] In this application, the flow chart for constructing the index of the high-temperature oxidation uniformity coefficient is as attached Figure 4 as shown.

[0052] The third step is to determine the temperature adjustment coefficient based on the stable characteristics of the high-temperature oxidation uniformity coefficient within the high-temperature oxidation interval.

[0053] Set every 10 minutes as a high-temperature oxidation interval. For any high-temperature oxidation interval, the sequence formed by arranging the high-temperature oxidation uniformity coefficients of all copper oxide nanowires in chronological order is denoted as the high-temperature oxidation uniformity sequence of the high-temperature oxidation interval.

[0054] Taking the high-temperature oxidation uniformity sequence as the input, use the K-means clustering algorithm to obtain each clustering cluster and clustering center of the high-temperature oxidation uniformity sequence, and denote the clustering centers as feature points respectively. Among them, the number of clustering centers K is set to 10, , the larger K is, the more accurate the monitoring of the high-temperature oxidation reaction of copper oxide nanowires is. The implementer can set the value of the number of clustering centers according to the actual situation. 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 for clustering.

[0055] It should be understood that the beneficial effect of using the K-means clustering algorithm to obtain feature points and clustering clusters is to avoid uniformly analyzing the data within the entire high-temperature oxidation interval when analyzing the high-temperature oxidation stability of copper oxide nanowires later, ignoring that the change of the high-temperature oxidation uniformity coefficient of copper oxide nanowires within the high-temperature oxidation interval is a process, resulting in misjudgment of the high-temperature oxidation stability of copper oxide nanowires later.

[0056] For any high-temperature oxidation interval, the high-temperature oxidation stability factor can be determined by the high-temperature oxidation difference of the feature points and the interval uniform steady-state factor. Specifically, in this embodiment, it can be calculated in the following way. Taking the high-temperature oxidation stability factor of the nth high-temperature oxidation interval as an example: ; where is the high-temperature oxidation stability factor of the nth high-temperature oxidation interval; , are respectively the interval uniform steady-state factor and the high-temperature oxidation difference of the feature points of the nth high-temperature oxidation interval; is a preset adjustment parameter, and its value in this embodiment is 0.1 to prevent the denominator from being 0.

[0057] For any high-temperature oxidation interval, the high-temperature oxidation difference of the characteristic points is determined by the difference between the high-temperature oxidation uniformity coefficients of all the characteristic points in the high-temperature oxidation uniformity sequence corresponding to the high-temperature oxidation interval.

[0058] In an embodiment of the present application, the difference between the high-temperature oxidation uniformity coefficients of all the characteristic points is set as: the accumulated result of the absolute values of the differences between the high-temperature oxidation uniformity coefficients of all the characteristic points. In other embodiments of the present application, other suitable difference calculation methods can also be used to obtain it.

[0059] It should be understood that when the growth process of the copper oxide nanowires in the high-temperature oxidation interval is more stable, the high-temperature oxidation stability factor is larger, and the high-temperature oxidation difference of the characteristic points is smaller.

[0060] For any high-temperature oxidation interval, the interval uniformity steady-state factor is the reciprocal of the difference between all the characteristic points and the mean value of the data in their corresponding clustering clusters.

[0061] 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 uniformity steady-state factor is larger, and further, the accumulated result of the mean value differences between all the characteristic points and all the data in their corresponding clustering clusters is smaller.

[0062] For any high-temperature oxidation interval, the temperature adjustment coefficient can be determined according to 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.

[0063] It should be understood that when the growth quality of the copper oxide nanowires is higher and the growth rate is more stable, the high-temperature oxidation stability factor is larger, the high-temperature oxidation difference of the characteristic points is smaller, the interval uniformity steady-state factor is larger, and at this time, it is less necessary to adjust the high-temperature oxidation temperature of the copper oxide nanowires.

[0064] The high-temperature oxidation sufficiency condition of the high-temperature oxidation interval is the mean value of the high-temperature oxidation uniformity coefficients at all times in the high-temperature oxidation interval. It should be understood that when the growth quality of the copper oxide nanowires in the high-temperature oxidation interval is higher, the high-temperature oxidation sufficiency condition is more significant, that is, the mean value of the high-temperature oxidation uniformity coefficients at all times in the high-temperature oxidation interval is larger, and at this time, it is less necessary to adjust the high-temperature oxidation temperature of the copper oxide nanowires.

[0065] So far, the temperature adjustment coefficient of the copper oxide nanowires in each high-temperature oxidation interval can be obtained in real time according to the above method.

[0066] In the present application, the flow chart for constructing the index of the temperature adjustment coefficient is as shown in the appendix Figure 5 as follows.

[0067] The fourth step is to adjust the temperature during the high-temperature oxidation of copper oxide nanowires according to the real-time temperature adjustment coefficient.

[0068] Set the temperature adjustment threshold W. When the real-time obtained temperature adjustment coefficient 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 relatively low at this time, and 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 real-time obtained temperature adjustment coefficient 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.

[0069] Among them, the value range of the temperature adjustment threshold W is [0, 1]. The higher the value of W, the more strict the requirements for the high-temperature oxidation process of copper oxide nanowires. In an embodiment of the present application, the value of W is 0.6, and the value of A is 20. The implementer can set the values of the temperature adjustment threshold W and the adjustment amplitude A according to the actual situation.

[0070] Thus, the temperature adjustment during the high-temperature oxidation of copper oxide nanowires can be realized according to the above method, and copper oxide nanowires with better quality can be obtained for the subsequent preparation of magnesium-deposited hydrogen storage materials.

[0071] S4. Prepare a titanium dioxide film wrapping the copper oxide nanowires by the sol-gel method to oxidize the copper oxide nanowires wrapped with titanium oxide. The solution prepared by the sol-gel method in the present application includes tetrabutyl titanate, absolute ethanol, nitric acid, and glacial acetic acid, and the thickness of the wrapping film layer is 0.2 - 0.8 . The copper oxide nanowires can either serve as the support of the high-surface-area nanomaterials; or form a composite semiconductor with titanium dioxide later to improve the hydrogen absorption efficiency.

[0072] S5. Perform magnesium deposition on the nanowires to obtain a magnesium-deposited hydrogen storage material. During the process of depositing magnesium on the nanowires by the magnetic filtration technology to obtain a magnesium-deposited hydrogen storage material, in the present application, the arc starting current is set to 50 - 80 A, the oxygen flow rate is 0 - 80 sccm, the vacuum degree is 2 6 Pa, the deposition time is 2 - 3 min, and the deposition thickness does not exceed 4 nm; the voltage of the high-power pulsed bias is set to 1 - 5 KV, the pulse width is 2 - 4 , the pulse frequency is 1 - 180 Hz, the duty cycle is 1 / 8500 - 1 / 5500, and the peak power is 2 - 5 MW. Using nano-metallic magnesium as the nano-decoration on the surface of titanium dioxide can greatly improve the hydrogen absorption efficiency, and at the same time reduce the hydrogen release temperature and decomposition activation energy.

[0073] In the first embodiment of the present application, the arc starting current is set to 80 A and the deposition time is 2 min.

[0074] In the second embodiment of the present application, the arc starting current is set to 70 A and the deposition time is 2.5 min.

[0075] In the third embodiment of the present application, the arc starting current is set to 50 A and the deposition time is 3 min.

[0076] The magnesium deposition hydrogen storage material prepared in the present application is tested, and the test results are as follows: the hydrogen release temperature is 63.8 °C and the decomposition activation energy is 63.4 KJ / mol.

[0077] Thus, an intelligent production process of a magnesium deposition hydrogen storage material can be realized according to the above method, and a magnesium deposition hydrogen storage material with better quality can be prepared.

[0078] Each embodiment in this specification is described in a progressive manner. The same or similar parts among the embodiments can be referred to each other, and the differences between each embodiment and other embodiments are emphasized.

[0079] It should be noted that unless otherwise specified and limited, terms such as "including", "comprising" or any other variant thereof are intended to cover non-exclusive inclusion, so that a circuit structure, article or device including a series of elements not only includes those elements, but also includes other elements not explicitly listed, or also includes elements inherent to such article or device. Without further limitation, an element defined by the statement "including one..." does not exclude the existence of another identical element 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 of the related listed items.

[0080] Those skilled in the art will readily think of other embodiments of the present application after considering the specification and practicing the invention herein. The present application is intended to cover any variations, uses or adaptations of the present application, which follow the general principles of the present application and include common general knowledge or conventional technical means in the technical field not invented by the present application.

[0081] It should be understood that the present application is not limited to the exact structure described above and shown in the drawings, and various modifications and changes can be made without departing from its scope.

Claims

1. An intelligent production process for a magnesium deposition hydrogen storage material, characterized in that The process includes the following steps: S1, ultrasonically clean the porous copper mesh; S2, inject noble metal ions into the porous copper mesh; S3, prepare copper oxide nanowires at high temperature; during the high-temperature oxidation process of preparing copper oxide nanowires, the specific process of adjusting the high-temperature oxidation temperature is as follows: Obtain the 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 characteristics distributed between different isotherms; Determine the temperature adjustment coefficient based on the stable characteristics of the high-temperature oxidation uniformity coefficient within the high-temperature oxidation interval; Adjust the temperature during the high-temperature oxidation process of copper oxide nanowires according to the real-time temperature adjustment coefficient; S4, prepare a titanium dioxide film coating the copper oxide nanowires by sol-gel method to oxidize the copper oxide nanowires coated with titanium oxide; S5, deposit magnesium on the nanowires to obtain a magnesium-deposited hydrogen storage material.

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

3. The intelligent production process of a magnesium-deposited 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 a magnesium-deposited hydrogen storage material as described in claim 1, wherein, The method for determining the high-temperature oxidation uniformity coefficient includes: Connect the data points with equal temperature values in the temperature field to obtain the isotherms at each temperature; Denote the minimum temperature point closest to the center point of the temperature field as the heat radiation end point; with the heat radiation end point as the center, extend the connection line in its preset neighborhood direction, and denote the last intersection point between the connection lines in each direction and each isotherm as the heat radiation start point in each direction; Determine the isothermal interval factor based on the position and angle distribution of the heat radiation start points of different isotherms in the same direction; Take the difference between the highest temperature and the lowest temperature in the temperature field as the temperature range; take the cumulative result of the information entropy of the temperature values of all heat radiation start points on all isotherms as the isothermal distribution chaos; Determine a high-temperature oxidation sufficiency factor based on the temperature range difference and the isothermal distribution chaos; wherein, the high-temperature oxidation sufficiency factor at the t-th moment is calculated by the formula: ; is the temperature range difference in the temperature field at the t-th moment; is the isothermal distribution chaos in the temperature field at the t-th moment; is a preset adjustment parameter; 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.

5. The intelligent production process of a magnesium-deposited hydrogen storage material according to claim 4, characterized in that, The method for determining the isothermal interval factor includes: Take the cumulative result of the distances between the heat radiation end point and the heat radiation start points on all isotherms in its preset neighborhood direction as the isothermal distance; Arrange the heat radiation start points in each neighborhood direction in ascending order of temperature values to form an isothermal interval sequence in each neighborhood direction; in each neighborhood direction, denote the cumulative result of the cosine similarity between the heat radiation end point and the connection lines between all heat radiation start points in the isothermal interval sequence as the neighborhood similarity in each neighborhood direction, and take the reciprocal of the cumulative result of the neighborhood similarities in all neighborhood directions as the isothermal interval deviation; Take the product of the isothermal distance and the isothermal interval deviation as the isothermal interval factor.

6. The intelligent production process of a magnesium-deposited hydrogen storage material according to claim 4, characterized in that, The method for determining the temperature adjustment coefficient includes: Set an interval with a preset duration as the high-temperature oxidation interval; form a high-temperature oxidation uniformity sequence with all the high-temperature oxidation uniformity coefficients within the high-temperature oxidation interval; Use a clustering algorithm to obtain several clustering clusters and their clustering centers of the high-temperature oxidation uniformity sequence, and denote the clustering centers as characteristic points; Take 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; Take the reciprocal of the difference between all feature points in the high-temperature oxidation uniform sequence and the data mean in their corresponding clustering clusters as the interval uniform steady-state factor; Determine the high-temperature oxidation stability factor based on the high-temperature oxidation difference of feature points and the interval uniform steady-state factor; among them, the high-temperature oxidation stability factor of the nth high-temperature oxidation interval The calculation formula is as follows: ; , are respectively the interval uniform steady-state factor and the feature point high-temperature oxidation difference of the nth high-temperature oxidation interval; is a preset adjustment parameter; Take the mean of the high-temperature oxidation uniform coefficients at all times in the high-temperature oxidation interval as the high-temperature oxidation sufficiency; Take the normalized value of the product of the high-temperature oxidation stability factor and the high-temperature oxidation sufficiency as the temperature adjustment coefficient.

7. The intelligent production process of a magnesium-deposited hydrogen storage material according to claim 6, characterized in that 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, raise the high-temperature oxidation temperature by a preset number of degrees; otherwise, do not adjust the high-temperature oxidation temperature.

8. The intelligent production process of a magnesium-deposited hydrogen storage material as described in claim 1, characterized in that, The length of the copper oxide nanowires prepared and obtained in S3 is 40 - 80 , and the density is 20 - 40 .

9. The intelligent production process of a magnesium-deposited hydrogen storage material as claimed in claim 1, wherein, The solution prepared by the sol-gel method in S4 includes tetrabutyl titanate, absolute ethanol, nitric acid, and glacial acetic acid.

10. The intelligent production process of a magnesium-deposited hydrogen storage material as described in claim 1, characterized in that, In S5, during the magnesium deposition process, set the arc starting current to 50 - 80 A and the deposition time to 2 - 3 min.

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