A method for preparing gold-encapsulated nanomaterial

Through activation treatment and ball milling technology, graphene and metal are better dispersed, solving the problems of carbonization and agglomeration during the melting of graphene and metal, and improving the dispersion and performance of olefin nanomaterials.

CN118291805BActive Publication Date: 2024-12-10SHANGHAI QIANHUI GOLD MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202410544651.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-05-06
Publication Date
2024-12-10
Estimated Expiration
2044-05-06

AI Technical Summary

Technical Problem

Carbonization and agglomeration are easily generated during the mixing and melting of graphene and metal, resulting in poor performance and effect.

Method used

Using the method of activating the graphene oxide powder and aluminum powder, the graphene can be dispersed better through ball milling and sintering technology, and then evenly mixed with metal elements and other powders, cold-pressing molding and smelting, increasing potassium fluorotitanate and fluorine Sodium borate is used to improve the dispersion and smelting temperature of graphene.

Benefits of technology

It effectively reduces the aluminum oxidation reaction temperature, improves the dispersion and performance of graphene, avoids carbonization and agglomeration, and improves the catalytic and thermal conductivity of olefin nanomaterials.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation method of graphene nanomaterials. Dry graphene oxide powder and aluminum powder are activated to promote better dispersion of graphene, and activated graphene mixed powder is obtained. The activated graphene is further dispersed in the aluminum powder by the first ball milling. Metal elements are added for the second ball milling to promote the metal elements, graphene and aluminum powder to be evenly mixed. The pressed embryos are sintered to disperse the graphene again. After the sintering is completed, the sintered pressed embryos are crushed and filtered. Potassium fluorotitanate, sodium fluoroborate and aluminum particles are added and stirred evenly, and then pressed embryos are pressed for the second time and then melted together with aluminum blocks to increase the graphene burning temperature, reduce the reaction temperature and energy of aluminum oxidation, and the oxide layer floats on the surface. The dispersion of graphene in aluminum liquid is improved during the smelting process. The preparation of the highly concentrated catalytic module and the smelting of the pure aluminum block are firstly sintered for the second time and then heated and dissolved with the aluminum block as a whole, so that the pressed embryos are dissolved in the aluminum liquid, and the dispersion area of ​​the graphene is greatly diffused.
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Description

Technical Field

[0001] The invention belongs to the technical field of graphene metal materials, and in particular relates to a method for preparing graphene gold nanomaterials. Background Art

[0002] At present, it is difficult to manufacture products with graphene as a single material. It is mainly to use its outstanding characteristics to combine with other material systems to prepare new composite materials, so that graphene-based composite materials have many excellent properties. For example, using graphene as a carrier to load nanoparticles can improve the catalytic and conductive properties of these particles; adding it to polymers can improve the mechanical and thermal conductivity of materials.

[0003] In the prior art, graphene is used as a coating or surface coating method. In this process, it is very difficult to control the uniformity of graphene. The performance effect of using unprocessed graphene is not very obvious. Graphene is a two-dimensional nanomaterial. By synthesizing graphene with aluminum powder, ball milling, sintering and other powder metallurgy technologies have also become an important processing technology for graphene alloy materials. However, the problem of carbonization and agglomeration is easy to occur during the melting process of graphene and metal.

[0004] The above information disclosed in the background technology is only used to increase the understanding of the background technology of the present application, and therefore, it may include information that does not constitute the prior art known to ordinary technicians in the field. Summary of the invention

[0005] The invention provides a method for preparing graphene gold nanomaterials to solve the technical problem that carbonization and agglomeration are easily generated in the existing process of mixing and melting graphene and metal.

[0006] In order to achieve the above invention / design purpose, the present invention adopts the following technical solutions:

[0007] A method for preparing gold olefin nanomaterials comprises the following steps:

[0008] Step 1: Activate the dried graphene oxide powder and aluminum powder:

[0009] Mix 5-16 parts of graphene oxide with 25-35 parts of aluminum powder;

[0010] Add 25-45 parts of isobutanol and mix well;

[0011] Add 0.3-1.2 parts of polyvinylpyrrolidone and mix well;

[0012] Add 0.5-1.6 parts of isobutyl ether and mix well;

[0013] The mixture is allowed to stand, filtered and then dried to obtain an activated graphene mixed powder;

[0014] Step 2, mixing 45-80 parts of the dried aluminum powder and 5-6 parts of the activated graphene mixed powder, stirring evenly, and then performing the first ball milling;

[0015] Step 3, adding 0.2-1.5 parts of dried nickel powder, 0.3-2.5 parts of magnesium powder, 0.1-1.6 parts of silicon powder, 0.02-1 parts of chromium powder, 0.08-0.6 parts of manganese powder, 0.4-2.5 parts of copper powder, 1.5-7 parts of zinc powder, 0.09-0.18 parts of titanium powder, 0.01-0.05 parts of neodymium powder, 0.6-1.2 parts of sodium tetraborate and 0.4-0.9 parts of potassium tetraborate to the ball-milled aluminum powder and activated graphene mixed powder, stirring evenly and then performing a second ball milling;

[0016] Step 4, cold-pressing the graphene mixed powder after the second ball milling to obtain a pressed green sheet, and sintering the pressed green sheet under oxygen-free conditions; crushing and filtering the sintered pressed green sheet to obtain a graphene sintered mixed powder;

[0017] Step 5: Add 0.6-1.3 parts of potassium fluorotitanate and 0.9-1.4 parts of sodium fluoroborate to the graphene sintered mixed powder obtained by crushing and filtering, mix 15-30 parts of the graphene sintered mixed powder after adding potassium fluorotitanate and sodium fluoroborate with 30-70 parts of dried aluminum particles, stir evenly, and cold press to obtain a graphene aluminum particle pressed block;

[0018] Step 6: gradually heat and bake the graphene aluminum particle pressed block and the pure aluminum block in a ratio of 1:15-25, melt and stir, and cast them into graphene aluminum material ingots to form a highly concentrated catalytic module;

[0019] Step 7: Melt the high-concentration catalytic module and the pure aluminum block in a ratio of 1:5-9 and stir evenly, and then cast to obtain the gold nanomaterial.

[0020] Wherein, the parts are all parts by weight.

[0021] The preparation method of the gold-gold nanomaterial as described above, in the step 1, the method of drying the graphene oxide powder and the aluminum powder is: mixing 5-16 parts of the graphene oxide powder and 25-35 parts of the aluminum powder of 600-800 mesh; spreading to a thickness of 3-5 mm and drying at 85-110° C. for 2-4 hours; stirring the graphene oxide and isobutanol evenly and subjecting to ultrasonic vibration for 0.5h-1h; adding vinylpyrrolidone, stirring evenly and subjecting to ultrasonic vibration for 1h-2h; adding isobutyl ether, stirring evenly and subjecting to ultrasonic vibration for 1.5h-3h; standing for 2-4h, filtering through a 300-500 mesh filter sieve, and drying at 85° C.-110° C. for 2h-5h.

[0022] In the method for preparing the gold-backed nanomaterial as described above, in step 2, aluminum powder with a mesh size of not less than 300-500 is dried at 110-130° C.; during the first ball milling, the ball milling is performed for 3-6 hours under vacuum and at a ball milling speed of 250-600 rpm.

[0023] The preparation method of gold olefin nanomaterials as described above, in step 3, the added dried powder is dried at 110-130°C, stirred evenly and subjected to ultrasonic oscillation for 1h-2h, and during the second ball milling, the ball milling is carried out for 4-8h under vacuum and at a ball milling speed of 200-600 rpm, and the ball milling is stopped for the first time and the second time.

[0024] In the method for preparing gold-backed nanomaterials as described above, in step 3, one or more of the following powders may be added: 0.0001-0.005 parts of neodymium powder, 0.00.9-0.18 parts of titanium powder, 0.00002-0.00007 parts of cobalt powder, 0.000001-0.00004 parts of vanadium powder, 0.0005-0.009 parts of iron powder, 0.00006-0.0001 parts of molybdenum powder, 0.00003-0.00008 parts of niobium powder, and 0.005-0.01 parts of zirconium carbide powder.

[0025] In the preparation method of gold-backed nanomaterials as described above, in step 3, one or more of the following powders may be added: 0.00004-0.00009 parts of tantalum powder, 0.000005-0.000009 parts of palladium powder, 0.0000002-0.0000006 parts of indium powder, 0.00000006-0.0000001 parts of ruthenium powder, 0.000000003-0.000000007 parts of tungsten powder, 0.000000004-0.000000008 parts of cerium powder, and 0.0000000003-0.000000007 parts of yttrium powder.

[0026] According to the preparation method of gold-backed nanomaterials as described above, in step 4, the pressure of cold pressing is 60Mpa-300Mpa, and the sintering process is: sintering at a starting temperature of 450°C for 2h, heating for 1h to increase the temperature to 550°C and sintering for 2h, heating for 1h to increase the temperature to 620°C and sintering for 2h, heating for 1h to increase the temperature to 680°C and sintering for 1h, and crushing the sintered pressed green blocks to less than 500 mesh.

[0027] In the method for preparing the gold-backed nanomaterial as described above, in step 5, the aluminum particles of 100-200 mesh are dried at a drying temperature of 110-130° C. for 1-2 hours; mixed and stirred for 0.5-1.5 hours, and the pressure of cold pressing is 60-300 MPa.

[0028] The preparation method of graphene gold nanomaterials as described above, in step 6, the step of gradually heating up and baking to carry out the melting process is: baking the graphene aluminum particle pressed block and part of the pure aluminum block at 400°C for 1h, 450°C for 1h, 500°C for 1h, 550°C for 1h, 600°C for 1h, 650°C for 1h, and 700°C for 1h, starting to melt at 750°C, stirring for 0.2h to form a paste, adding the remaining pure aluminum block, continuing to stir for 0.2h after melting, then raising the temperature to 850°C, and completely melting after 0.5h, starting to stir with a stirrer, the stirring time is 0.2-0.5h, and the stirring cycle is repeated multiple times.

[0029] The method for preparing the gold-olefin nanomaterial as described above is to carry out smelting at 800-900°C.

[0030] Compared with the prior art, the advantages and positive effects of the present invention are:

[0031] The preparation method of the gold-gold nanomaterial of the present invention comprises the following steps: performing activation treatment on dried graphene oxide powder and aluminum powder, so as to promote better dispersion of graphene, obtain activated graphene mixed powder, further disperse the activated graphene in aluminum powder by first ball milling, add metal elements for second ball milling, promote uniform mixing of metal elements with graphene and aluminum powder, sinter the pressed embryo to disperse the graphene again, crush and filter the sintered pressed embryo after sintering, add potassium fluorotitanate, sodium fluoroborate and aluminum particles, stir evenly, perform second pressed embryo, and then melt with aluminum block, increase the graphene burning temperature, reduce the reaction temperature and energy of aluminum oxidation, and float the oxide layer on the surface. The dispersion of graphene in aluminum liquid is improved during the smelting process. The preparation of the highly concentrated catalytic module and the smelting of the pure aluminum block firstly sinter the pressed embryo for the second time and then heat it up and melt it with the aluminum block, so that the pressed embryo is dissolved in the aluminum liquid, and the graphene dispersion area is greatly diffused.

[0032] After reading the specific embodiments of the present invention in conjunction with the accompanying drawings, other features and advantages of the present invention will become more clear. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0034] Figure 1 It is the pressed green piece in step 4 of the specific embodiment of the present invention.

[0035] Figure 2 It is the pressed green body obtained by sintering in step 4 of the specific embodiment of the present invention.

[0036] Figure 3 This is the graphene aluminum particle pressed block obtained in step 5 of the specific embodiment of the present invention.

[0037] Figure 4 It is the highly concentrated catalytic module obtained in step 6 of the specific embodiment of the present invention.

[0038] Figure 5 It is the gold olefin nanomaterial obtained in step 7 of the specific embodiment of the present invention.

[0039] Figure 6 , 7 It is the transparent body in the melting process of step 7 of the specific embodiment of the present invention.

[0040] Figure 8 It is a force-displacement curve diagram of the gold-olefin nanomaterial obtained in a specific embodiment of the present invention. DETAILED DESCRIPTION

[0041] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0042] In the description of the present invention, it should be understood that the terms "center", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore, should not be understood as a limitation on the present invention.

[0043] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected" and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. In the description of the implementation method, specific features, structures, materials or characteristics can be combined in any one or more embodiments or examples in a suitable manner.

[0044] The terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features.

[0045] In the description of the present invention, unless otherwise specified, "plurality" means two or more.

[0046] A method for preparing gold olefin nanomaterials comprises the following steps:

[0047] Step 1, drying graphene oxide powder and aluminum powder: 5-16 parts of graphene oxide powder and 25-35 parts of 600-800 mesh aluminum powder are mixed; spread to a thickness of 3-5 mm and dry at 85-110° C. for 2-4 hours.

[0048] Activation treatment of aluminum powder and dried graphene oxide powder:

[0049] 25-45 parts of isobutanol are added to the dried graphene oxide powder and aluminum powder and mixed evenly; specifically, the graphene oxide, aluminum powder and isobutanol are stirred evenly and subjected to ultrasonic vibration for 0.5h-1h to perform the first activation.

[0050] Add 0.3-1.2 parts of polyvinylpyrrolidone and mix evenly; specifically, add vinylpyrrolidone, stir evenly and vibrate ultrasonically for 1h-2h to perform the second activation.

[0051] Add 0.5-1.6 parts of isobutyl ether and mix evenly; specifically, add isobutyl ether, stir evenly and vibrate ultrasonically for 1.5h-3h to perform the third activation.

[0052] The mixture was allowed to stand for 2-4 hours, filtered and then dried to obtain an activated graphene mixed powder. Specifically, the mixture was filtered through a 300-500 mesh filter sieve and dried at 85° C.-110° C. for 2 hours-5 hours.

[0053] Step 2, drying aluminum powder with a mesh size of not less than 300-500 at 110-130° C.; mixing 45-80 parts of the dried aluminum powder with 5-6 parts of the activated graphene mixed powder and stirring them evenly, and then performing the first ball milling; during the first ball milling, the ball milling is performed for 3-6 hours under vacuum and at a ball milling speed of 250-600 rpm.

[0054] Step 3, add 0.2-1.5 parts of dried nickel powder, 0.3-2.5 parts of magnesium powder, 0.1-1.6 parts of silicon powder, 0.02-1 parts of chromium powder, 0.08-0.6 parts of manganese powder, 0.4-2.5 parts of copper powder, 1.5-7 parts of zinc powder, 0.09-0.18 parts of titanium powder, 0.01-0.05 parts of neodymium powder, 0.6-1.2 parts of sodium tetraborate and 0.4-0.9 parts of potassium tetraborate to the ball-milled aluminum powder and activated graphene mixed powder, stir evenly and then perform a second ball milling. During the second ball milling, ball milling is performed for 4-8 hours under vacuum and a ball milling speed of 200-600 rpm. The ball milling is stopped for the first time and the second time to prevent the temperature from rising.

[0055] The added dried powder is dried at 110-130° C., stirred evenly and subjected to ultrasonic oscillation for 1 h-2 h.

[0056] In some embodiments, one or more of the following powders may also be added: 0.0001-0.005 parts of neodymium powder, 0.9-0.18 parts of titanium powder, 0.00002-0.00007 parts of cobalt powder, 0.000001-0.00004 parts of vanadium powder, 0.0005-0.009 parts of iron powder, 0.00006-0.0001 parts of molybdenum powder, 0.00003-0.00008 parts of niobium powder, and 0.005-0.01 parts of zirconium carbide powder.

[0057] In some embodiments, one or more of the following powders may also be added: 0.00004-0.00009 parts of tantalum powder, 0.000005-0.000009 parts of palladium powder, 0.0000002-0.0000006 parts of indium powder, 0.00000006-0.0000001 parts of ruthenium powder, 0.000000003-0.000000007 parts of tungsten powder, 0.000000004-0.000000008 parts of cerium powder, and 0.0000000003-0.000000007 parts of yttrium powder.

[0058] Metal elements have the effect of changing physical properties and can be added as needed.

[0059] Step 4, cold press the graphene mixed powder after the second ball milling, the pressure of cold pressing is 60Mpa-300Mpa, and a pressed green block is obtained. The pressed green block is sintered under oxygen-free conditions. The sintering process is: sintering at a starting temperature of 450°C for 2h, heating for 1h to increase the temperature to 550°C and sintering for 2h, heating for 1h to increase the temperature to 620°C and sintering for 2h, heating for 1h to increase the temperature to 680°C and sintering for 1h. The sintered pressed green block is crushed and filtered to obtain graphene sintered mixed powder; the sintered pressed green block is crushed to less than 500 mesh.

[0060] Among them, the anaerobic condition can be achieved by using a vacuum pump to evacuate the working chamber to a negative pressure of 0.2-2Pa, and then filling it with inert gas to replace oxygen.

[0061] Step 5, drying the 100-200 mesh aluminum particles at a drying temperature of 110-130° C. for 1-2 hours; adding 0.6-1.3 parts of potassium fluorotitanate and 0.9-1.4 parts of sodium fluoroborate to the graphene sintering mixed powder obtained by crushing and filtering, and mixing 15-30 parts of the graphene sintering mixed powder after adding potassium fluorotitanate and sodium fluoroborate with 30-70 parts of the dried aluminum particles, stirring for 0.5-1.5 hours, and cold pressing to obtain graphene aluminum particle pressed blocks. The pressure of cold pressing is 60-300Mpa.

[0062] Step 6: gradually heat and bake the graphene aluminum particle pressed block and the pure aluminum block in a ratio of 1:15-25, melt and stir, and cast them into graphene aluminum material ingots to form a highly concentrated catalytic module.

[0063] The gradual heating and baking and melting process is as follows: the graphene aluminum particle pressed block and part of the pure aluminum block are baked at 400°C for 1h, 450°C for 1h, 500°C for 1h, 550°C for 1h, 600°C for 1h, 650°C for 1h, and 700°C for 1h, and start to melt at 750°C. Stir for 0.2h to form a paste, add the remaining pure aluminum block, continue stirring for 0.2h after melting, then raise the temperature to 850°C, and melt all of it after 0.5h. Start stirring with a stirrer for 0.2-0.5h, and repeat several times.

[0064] First add some aluminum blocks, and then add aluminum blocks in proportion when the aluminum blocks melt into liquid according to the melting conditions of the aluminum blocks.

[0065] The purpose of gradually increasing the temperature at different temperatures is to first sinter the graphene aluminum particle pressed block and then increase the temperature to melt it together with the aluminum block. This greatly increases the carbonization temperature of the graphene and ensures that the graphene can be melted into the aluminum liquid and dispersed.

[0066] Step 7: Smelt the high-concentration catalytic module and the pure aluminum block at a ratio of 1:5-9 at 800-900° C., remove hydrogen with inert gas, refine, and cast to obtain the gold nanomaterial.

[0067] Wherein, parts are parts by weight.

[0068] In a specific example:

[0069] A method for preparing gold olefin nanomaterials comprises the following steps:

[0070] Step 1, drying graphene oxide powder and aluminum powder: 10 parts of graphene oxide powder and 30 parts of 700 mesh aluminum powder were mixed and spread to a thickness of 4 mm and dried for 3 hours.

[0071] Activation treatment of aluminum powder and dried graphene oxide powder:

[0072] 30 parts of isobutanol were added to the dried graphene oxide powder and aluminum powder and mixed evenly; specifically, the graphene oxide, aluminum powder and isobutanol were stirred evenly and subjected to ultrasonic vibration for 0.7 hours to perform the first activation.

[0073] 0.8 parts of polyvinylpyrrolidone was added and mixed evenly; specifically, vinylpyrrolidone was added, stirred evenly and subjected to ultrasonic vibration for 1.5 hours to perform a second activation.

[0074] 1.2 parts of isobutyl ether were added and mixed evenly; specifically, isobutyl ether was added, stirred evenly and subjected to ultrasonic vibration for 2 hours to perform the third activation.

[0075] The mixture was allowed to stand for 3 hours, filtered and dried to obtain an activated graphene mixed powder. Specifically, the mixed powder was filtered through a 400-mesh filter sieve and dried at 90° C. for 3 hours.

[0076] Step 2, drying aluminum powder with a mesh size of not less than 400 at 120° C.; mixing 60 parts of the dried aluminum powder with 5.5 parts of the activated graphene mixed powder and stirring them evenly, and then performing the first ball milling; during the first ball milling, the ball milling was performed for 4 hours under vacuum and at a ball milling speed of 400 rpm.

[0077] Step 3, add 0.8 parts of dried nickel powder, 1.5 parts of magnesium powder, 1.2 parts of silicon powder, 0.2 parts of chromium powder, 0.3 parts of manganese powder, 1.2 parts of copper powder, 3 parts of zinc powder, 0.1 parts of titanium powder, 0.03 parts of neodymium powder, 0.9 parts of sodium tetraborate and 0.7 parts of potassium tetraborate to the mixed powder of aluminum powder and activated graphene after ball milling, stir evenly and then perform a second ball milling. During the second ball milling, ball milling is carried out for 6 hours under vacuum and at a ball milling speed of 400 rpm. After 2 hours of ball milling, stop for 15 minutes to prevent temperature increase.

[0078] The added dried powder was dried at 120° C., stirred evenly and subjected to ultrasonic oscillation for 1.5 hours.

[0079] In some embodiments, one or more of the following powders can be added as needed: 0.0001-0.005 parts of neodymium powder, 0.9-0.18 parts of titanium powder, 0.00002-0.00007 parts of cobalt powder, 0.000001-0.00004 parts of vanadium powder, 0.0005-0.009 parts of iron powder, 0.00006-0.0001 parts of molybdenum powder, 0.00003-0.00008 parts of niobium powder, and 0.005-0.01 parts of zirconium carbide powder.

[0080] In some embodiments, one or more of the following powders may be further added as needed: 0.00004-0.00009 parts of tantalum powder, 0.000005-0.000009 parts of palladium powder, 0.0000002-0.0000006 parts of indium powder, 0.00000006-0.0000001 parts of ruthenium powder, 0.000000003-0.000000007 parts of tungsten powder, 0.000000004-0.000000008 parts of cerium powder, and 0.0000000003-0.000000007 parts of yttrium powder.

[0081] The type and amount of added powder can be determined according to the properties of the material to be prepared.

[0082] Step 4: cold-press the graphene mixed powder after the second ball milling at a pressure of 150 MPa to obtain a pressed green block, such as Figure 1 The pressed green body is sintered under oxygen-free conditions. Figure 2 As shown. The sintering process is: sintering at a starting temperature of 450°C for 2h, heating up to 550°C for 1h and sintering for 2h, heating up to 620°C for 1h and sintering for 2h, heating up to 680°C for 1h and sintering for 1h. The sintered pressed green block is crushed and filtered to obtain graphene sintered mixed powder; the sintered pressed green block is crushed to 300 mesh.

[0083] Step 5, drying the 100-200 mesh aluminum particles at a drying temperature of 120° C. for 1.5 h; adding 0.8 parts of potassium fluorotitanate and 1.1 parts of sodium fluoroborate to the graphene sintered mixed powder obtained by crushing and filtering, and mixing 20 parts of the graphene sintered mixed powder after adding potassium fluorotitanate and sodium fluoroborate with 50 parts of the dried aluminum particles, stirring evenly, stirring for 1 h, and cold pressing to obtain a graphene aluminum particle pressed block, such as Figure 3 As shown in the figure, the pressure of cold pressing is 100Mpa.

[0084] Step 6: gradually heat and bake the graphene aluminum particle pressed block and the pure aluminum block in a ratio of 1:20, melt and stir, and cast them into graphene aluminum material ingots to form a highly concentrated catalytic module, such as Figure 4 shown.

[0085] The gradual heating and baking and melting process is as follows: bake the graphene aluminum particle pressed block and 2 / 3 pure aluminum block at 400°C for 1h, 450°C for 1h, 500°C for 1h, 550°C for 1h, 600°C for 1h, 650°C for 1h, and 700°C for 1h, start to melt at 750°C, start stirring for 0.2h to form a paste, add the remaining 1 / 3 pure aluminum block, continue stirring for 0.2h after melting, then raise the temperature to 850°C, and melt all of it after 0.5h. Start stirring with a stirrer for 0.4h, and repeat 5 times.

[0086] Step 7: Smelt the high-concentration catalyst module and the pure aluminum block at a ratio of 1:7 at 850°C, and cast to obtain the gold-enriched nanomaterial, such as Figure 5 shown.

[0087] Pure aluminum is silver at room temperature. The melting temperature during smelting is 680 degrees, the liquid flow temperature is 730 degrees, and the normal melting temperature is 760-780 degrees. If the temperature is higher, a large amount of evaporation will occur, producing hydrogen. The evaporation rate is 1.5-2%. The color of aluminum during smelting is red.

[0088] In step 7, the melting temperature of graphene and aluminum block is 750 degrees, the flow temperature is 800 degrees, the normal melting temperature is 850-900 degrees, the melting temperature is increased, the melting temperature of graphene nanomaterials is 12-18% higher than that of pure aluminum, the evaporation rate is 0.3-5%, the consumption rate is also significantly reduced, the liquid fluidity is obviously different, the normal aluminum liquid is opaque, while the graphene nanomaterial liquid fluidity is as transparent as water, the casting temperature is 830-870 degrees, the color of the liquid changes under the action of graphene during the melting process, the liquid is dehydrogenated by inert gas, and the liquid surface is visually transparent, such as Figure 6 and Figure 7 As shown, the fluidity during melting is superior to that of pure aluminum, and the liquid is transparent during melting, which is a manifestation of uniform dispersion of graphene.

[0089] The performance test of the obtained gold-olefin nanomaterial is shown in the following table:

[0090]

[0091]

[0092] The force-displacement curve of the obtained gold nanoparticles is shown in Figure 8 shown.

[0093] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for a person skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to replace some of the technical features therein by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions claimed to be protected by the present invention.

Claims

1. A method for preparing gold olefin nanomaterials, characterized in that: The steps include: Step 1: Activate the dried graphene oxide powder and aluminum powder: Mix 5-16 parts of graphene oxide with 25-35 parts of aluminum powder; Add 25-45 parts of isobutanol and mix well; Add 0.3-1.2 parts of polyvinylpyrrolidone and mix well; Add 0.5-1.6 parts of isobutyl ether and mix well; The mixture is allowed to stand, filtered and then dried to obtain an activated graphene mixed powder; Step 2, mixing 45-80 parts of the dried aluminum powder and 5-6 parts of the activated graphene mixed powder, stirring evenly, and then performing the first ball milling; Step 3, adding 0.2-1.5 parts of dried nickel powder, 0.3-2.5 parts of magnesium powder, 0.1-1.6 parts of silicon powder, 0.02-1 parts of chromium powder, 0.08-0.6 parts of manganese powder, 0.4-2.5 parts of copper powder, 1.5-7 parts of zinc powder, 0.09-0.18 parts of titanium powder, 0.01-0.05 parts of neodymium powder, 0.6-1.2 parts of sodium tetraborate and 0.4-0.9 parts of potassium tetraborate to the ball-milled aluminum powder and activated graphene mixed powder, stirring evenly and then performing a second ball milling; Step 4, cold-pressing the graphene mixed powder after the second ball milling to obtain a pressed green sheet, and sintering the pressed green sheet under oxygen-free conditions; crushing and filtering the sintered pressed green sheet to obtain a graphene sintered mixed powder; Step 5: Add 0.6-1.3 parts of potassium fluorotitanate and 0.9-1.4 parts of sodium fluoroborate to the graphene sintered mixed powder obtained by crushing and filtering, mix 15-30 parts of the graphene sintered mixed powder after adding potassium fluorotitanate and sodium fluoroborate with 30-70 parts of dried aluminum particles, stir evenly, and cold press to obtain a graphene aluminum particle pressed block; Step 6: gradually heat and bake the graphene aluminum particle pressed block and the pure aluminum block in a ratio of 1:15-25, melt and stir, and cast them into graphene aluminum material ingots to form a highly concentrated catalytic module; Step 7, melting the high-concentration catalytic module and the pure aluminum block in a ratio of 1:5-9 and stirring them evenly, and then casting to obtain the gold nanomaterial; Wherein, the parts are all parts by weight.

2. The method for preparing the gold-olefin nanomaterial according to claim 1, characterized in that: In step 1, the method of drying graphene oxide powder and aluminum powder is: Mix 5-16 parts of graphene oxide powder and 25-35 parts of 600-800 mesh aluminum powder; spread to a thickness of 3-5 mm and dry at 85-110° C. for 2-4 hours; Add isobutanol, stir evenly and vibrate ultrasonically for 0.5h-1h; Add vinylpyrrolidone, stir evenly and vibrate ultrasonically for 1h-2h; Add isobutyl ether, stir evenly and vibrate ultrasonically for 1.5h-3h; let stand for 2-4h, filter through a 300-500 mesh filter sieve, and dry at 85℃-110℃ for 2h-5h.

3. The method for preparing the gold-olefin nanomaterial according to claim 1, characterized in that: In the step 2, the aluminum powder with a mesh size of not less than 300-500 is dried at 110-130° C.; during the first ball milling, the ball milling is performed for 3-6 hours under vacuum and at a ball milling speed of 250-600 rpm.

4. The method for preparing the gold-olefin nanomaterial according to claim 1, characterized in that: In the step 3, the mixture is stirred evenly and subjected to ultrasonic oscillation for 1 h to 2 h. During the second ball milling, the mixture is ball milled for 4 to 8 h under vacuum at a ball milling speed of 200 to 600 rpm.

5. The method for preparing the gold-olefin nanomaterial according to claim 1, characterized in that: In step 3, one or more of the following powders may be added: 0.00002-0.00007 parts of cobalt powder, 0.000001-0.00004 parts of vanadium powder, 0.0005-0.009 parts of iron powder, 0.00006-0.0001 parts of molybdenum powder, 0.00003-0.00008 parts of niobium powder, and 0.005-0.01 parts of zirconium carbide powder.

6. The method for preparing the gold-olefin nanomaterial according to claim 1, characterized in that: In step 4, the cold pressing pressure is 60Mpa-300Mpa, and the sintering process is: starting temperature 450°C for sintering for 2h, heating for 1h to increase the temperature to 550°C for sintering for 2h, heating for 1h to increase the temperature to 620°C for sintering for 2h, heating for 1h to increase the temperature to 680°C for sintering for 1h, and crushing the sintered pressed green blocks to less than 500 mesh.

7. The method for preparing gold olefin nanomaterials according to claim 1, characterized in that: In the step 5, the aluminum particles of 100-200 mesh are dried at a drying temperature of 110-130° C. for 1-2 hours; mixed and stirred for 0.5-1.5 hours, and the pressure of cold pressing is 60-300 MPa.

8. The method for preparing gold olefin nanomaterials according to claim 1, characterized in that: In step 6, the step of gradually increasing the temperature for baking and melting is as follows: baking the graphene aluminum particle pressed block and part of the pure aluminum block at 400°C for 1h, 450°C for 1h, 500°C for 1h, 550°C for 1h, 600°C for 1h, 650°C for 1h, and 700°C for 1h, starting to melt at 750°C, stirring for 0.2h to form a paste, adding the remaining pure aluminum block, continuing to stir for 0.2h after melting, then raising the temperature to 850°C, and completely melting after 0.5h, starting to stir with a stirrer for 0.2-0.5h, and repeating the stirring cycle for multiple times.

9. The method for preparing gold olefin nanomaterial according to claim 1, characterized in that: The melting is carried out at 800-900°C.