Release Agent for Integral Die Casting of Aluminum Alloy Automobiles

Abstract

The present invention relates to the technical field of mold release agents, and specifically discloses a mold release agent for the integrated die-casting of aluminum alloy automobiles, which comprises the following raw materials in parts by weight: 15-20 parts of fluorinated wax emulsion, 6-8 parts of sodium dodecylbenzenesulfonate, 3-6 parts of Tween 80, 3-5 parts of methylphenyl modified silicone oil, 4-6 parts of graphene regulator, 2-4 parts of nano-silica modifier, 2-4 parts of silane coupling agent, and 10-15 parts of water. The mold release agent of the present invention uses fluorinated wax emulsion in combination with sodium dodecylbenzenesulfonate, Tween 80, and methylphenyl modified silicone as the matrix materials, and through the addition of graphene regulator, nano-silica modifier, and silane coupling agent to coordinate with each other and work together synergistically, with the silane coupling agent as the interfacial agent to enhance the interfacial effect between the raw materials of the system.

Description

Technical Field

[0001] The present invention relates to the technical field of release agents, and specifically relates to a release agent for integrated die-casting of aluminum alloy automobiles. Background Art

[0002] The die-casting release agent, also known as the mold release agent, as the name implies, is an auxiliary agent that plays an isolating role between the mold and the casting during the casting forming process. It can effectively prevent or reduce mechanical damage when the formed casting is demolded, thus playing an indispensable role in improving the appearance quality of the casting and extending the service life of the mold. The release agent is required to be not easily decomposed and worn during use, not adhere to the surface of the casting, not affect subsequent processing such as bonding, printing, painting, and embossing of the casting, so as to maintain the integrity of the casting.

[0003] The existing release agents have poor adhesion strength to aluminum alloy products, which easily leads to insufficient adsorption strength of the metal during demolding, resulting in poor demolding performance. At the same time, in order to improve its adhesion performance, the friction coefficient of the product becomes worse, and it is difficult to achieve coordinated improvement of the adhesion and friction coefficient of the product, restricting the use efficiency of the product. Summary of the Invention

[0004] Aiming at the defects of the existing technology, the purpose of the present invention is to provide a release agent for integrated die-casting of aluminum alloy automobiles to solve the problems raised in the above background art.

[0005] The present invention solves the technical problems by adopting the following technical solutions:

[0006] The present invention provides a release agent for integrated die-casting of aluminum alloy automobiles, which comprises the following raw materials in parts by weight:

[0007] 15 - 20 parts of fluorinated wax emulsion, 6 - 8 parts of sodium dodecylbenzenesulfonate, 3 - 6 parts of Tween 80, 3 - 5 parts of methylphenyl modified silicone oil, 4 - 6 parts of graphene regulator,

[0008] 2 - 4 parts of nano-silica modifier, 2 - 4 parts of silane coupling agent,

[0009] 10 - 15 parts of water.

[0008] Preferably, the release agent for integrated die-casting of aluminum alloy automobiles comprises the following raw materials in parts by weight:

[0009] 17.5 parts of fluorinated wax emulsion, 7 parts of sodium dodecylbenzenesulfonate, 4.5 parts of Tween 80, 4 parts of methylphenyl modified silicone oil, 5 parts of graphene regulator, 3 parts of nano-silica modifier, 3 parts of silane coupling agent, 12.5 parts of water.

[0010] Preferably, the silane coupling agent is silane coupling agent KH560.

[0011] Preferably, the preparation method of the graphene regulator is:

[0012] S01: Add 2-5 parts by weight of lanthanum chloride solution and 1-3 parts of glycolic acid to 5-10 parts of sodium citrate solution, stir and mix evenly, and finally add 2-4 parts of a 5% chitosan solution by mass fraction, stir thoroughly to obtain a pre-modifier;

[0013] S02: First, place graphene in a pre-modifier that is 3-5 times the total amount of graphene and stir for modification treatment. After the modification is completed, a modified graphene agent is obtained;

[0014] S03: Ball-mill and lubricate the modified graphene agent and the lubricating fluid according to a weight ratio of 5:2. After the lubrication is completed, wash with water and dry to obtain a graphene regulator.

[0015] Preferably, the mass fraction of the lanthanum chloride solution is 2-5%; the mass fraction of the sodium citrate solution is 10-15%.

[0016] Preferably, the stirring temperature for the stirring modification treatment is 45-50 °C, the stirring time is 1-2 h, and the stirring speed is 450-500 r / min.

[0017] Preferably, the lubricating fluid includes the following raw materials in parts by weight:

[0018] 1-3 parts of urea, 2-5 parts of nano-silica sol, 3-5 parts of sodium lignosulfonate, 4-8 parts of deionized water, and 0.5-0.7 parts of nickel powder.

[0019] Preferably, the ball-milling speed for the ball-milling lubrication treatment is 1000-1500 r / min, and the ball-milling time is 1-2 h.

[0020] Preferably, the preparation method of the nano-silica modifier is as follows:

[0021] S101: Stir and mix nano-silica in a sufficient amount of 5% hydrochloric acid solution, then filter, and then stir thoroughly in a sufficient amount of 10% sodium alginate solution, and finally wash with water and dry;

[0022] S102: Perform stepwise thermal improvement treatment on the dried nano-silica. After the treatment is completed, the nano-silica modifier can be obtained.

[0023] Preferably, the steps of the stepwise thermal improvement treatment are as follows:

[0024] First, perform heat treatment at a temperature of 210-230 °C for 5-10 min, then cool at a rate of 1-3 °C / min to 150-155 °C, keep warm for 10-15 min, then cool at a rate of 2-5 °C / min to 85-95 °C, and finally cool with water to room temperature and dry.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The mold release agent of the present invention uses a fluorinated wax emulsion in combination with sodium dodecylbenzenesulfonate, Tween 80, and methylphenyl modified silicone as the matrix material. By adding graphene regulators, nano-silica modifiers, and silane coupling agents to coordinate with each other and work synergistically, with the silane coupling agent as the interfacial agent to enhance the interfacial effect between the raw materials of the system. At the same time, the graphene regulator is obtained by stirring and modifying graphene with a pre-modifier and then improving the lubrication by ball milling with a lubricating liquid, so that the graphene regulator can better cooperate in the system, enhance the strength of the attached metal body in the system, and improve the lubricity of the system. The nano-silica modifier is obtained by jointly treating nano-silica with hydrochloric acid solution and sodium alginate solution, and then through stepwise heat improvement treatment. The nano-silica modifier obtained can cooperate with the graphene regulator more significantly, thus better coordinating and improving the lubrication performance and adhesion strength performance of the product. Specific embodiments

[0027] The following combines specific embodiments to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0028] The mold release agent for the integrated die-casting of aluminum alloy automobiles in this embodiment includes the following raw materials in parts by weight:

[0029] 15 - 20 parts of fluorinated wax emulsion, 6 - 8 parts of sodium dodecylbenzenesulfonate, 3 - 6 parts of Tween 80, 3 - 5 parts of methylphenyl modified silicone oil, 4 - 6 parts of graphene regulator, 2 - 4 parts of nano-silica modifier, 2 - 4 parts of silane coupling agent, and 10 - 15 parts of water.

[0030] The mold release agent for the integrated die-casting of aluminum alloy automobiles in this embodiment includes the following raw materials in parts by weight:

[0031] 17.5 parts of fluorinated wax emulsion, 7 parts of sodium dodecylbenzenesulfonate, 4.5 parts of Tween 80, 4 parts of methylphenyl modified silicone oil, 5 parts of graphene regulator, 3 parts of nano-silica modifier, 3 parts of silane coupling agent, and 12.5 parts of water.

[0032] The silane coupling agent in this embodiment is silane coupling agent KH560.

[0033] The preparation method of the graphene regulator in this embodiment is as follows:

[0034] S01: Add 2 - 5 parts by weight of lanthanum chloride solution and 1 - 3 parts of glycolic acid into 5 - 10 parts of sodium citrate solution, stir and mix evenly. Finally, add 2 - 4 parts of 5% chitosan solution by mass fraction, and stir thoroughly to obtain a pre - modifier.

[0035] S02: First, place graphene in a pre - modifier that is 3 - 5 times the total amount of graphene and stir for modification treatment. After the modification is completed, obtain a modified graphene agent.

[0036] S03: Perform ball - milling lubrication treatment on the modified graphene agent and the lubricant according to a weight ratio of 5:2. After the lubrication is completed, wash with water and dry to obtain a graphene regulator.

[0037] In this example, the mass fraction of the lanthanum chloride solution is 2 - 5%; the mass fraction of the sodium citrate solution is 10 - 15%.

[0038] In this example, the stirring temperature for the stirring modification treatment is 45 - 50 °C, the stirring time is 1 - 2 h, and the stirring speed is 450 - 500 r / min.

[0039] The lubricant in this example includes the following raw materials in parts by weight:

[0040] 1 - 3 parts of urea, 2 - 5 parts of nano - silica sol, 3 - 5 parts of sodium lignosulfonate, 4 - 8 parts of deionized water, and 0.5 - 0.7 parts of nickel powder.

[0041] In this example, the ball - milling speed for the ball - milling lubrication treatment is 1000 - 1500 r / min, and the ball - milling time is 1 - 2 h.

[0042] The preparation method of the nano - silica modifier in this example is as follows:

[0043] S101: Stir and mix nano - silica in a sufficient amount of 5% hydrochloric acid solution, then filter, and then stir thoroughly in a sufficient amount of 10% sodium alginate solution. Finally, wash with water and dry.

[0044] S102: Perform stepped thermal improvement treatment on the dried nano - silica. After the treatment is completed, the nano - silica modifier can be obtained.

[0045] The steps of the stepped thermal improvement treatment in this example are as follows:

[0046] First, perform heat treatment at a temperature of 210 - 230 °C for 5 - 10 min, then cool at a rate of 1 - 3 °C / min to 150 - 155 °C, keep warm for 10 - 15 min, then cool at a rate of 2 - 5 °C / min to 85 - 95 °C, and finally cool with water to room temperature and dry.

[0047] Example 1.

[0048] The release agent for aluminum alloy automotive integrated die-casting of this embodiment includes the following raw materials in parts by weight:

[0049] 15 parts of fluorowax emulsion, 6 parts of sodium dodecylbenzenesulfonate, 3 parts of Tween 80, 3 parts of methylphenyl modified silicone oil, 4 parts of graphene regulator, 2 parts of nano-silica modifier, 2 parts of silane coupling agent, and 10 parts of water.

[0050] The silane coupling agent in this embodiment is silane coupling agent KH560.

[0051] The preparation method of the graphene regulator of this embodiment is:

[0052] S01: Add 2 parts by weight of lanthanum chloride solution and 1 part of glycolic acid to 5 parts of sodium citrate solution, stir and mix, and finally add 2 parts of 5% by mass chitosan solution and stir thoroughly to obtain a pre-modifier;

[0053] S02: Graphene is first placed in a pre-modifier with an amount three times the total amount of graphene and stirred for modification. After modification is completed, a modified graphene agent is obtained;

[0054] S03: ball milling and lubricating the modified graphene agent and lubricating liquid in a weight ratio of 5:2. After lubrication, washing with water and drying are completed to obtain a graphene regulator.

[0055] The mass fraction of the lanthanum chloride solution in this embodiment is 2%; the mass fraction of the sodium citrate solution is 10%.

[0056] The stirring temperature of the stirring modification treatment in this embodiment is 45° C., the stirring time is 1 h, and the stirring speed is 450 r / min.

[0057] The lubricating fluid of this embodiment includes the following raw materials in parts by weight:

[0058] 1 part urea, 2 parts nano-silica sol, 3 parts sodium lignin sulfonate, 4 parts deionized water and 0.5 parts nickel powder.

[0059] The ball milling speed of the ball milling lubrication treatment in this embodiment is 1000 r / min, and the ball milling time is 1 hour.

[0060] The preparation method of the nano-silica modifier of this embodiment is:

[0061] S101: Mix the nano-silica in a sufficient amount of 5% by mass hydrochloric acid solution, filter it, and then mix it thoroughly in a sufficient amount of 10% by mass sodium alginate solution, and finally wash it with water and dry it;

[0062] S102: The dried nano-silica is subjected to a stepwise thermal modification treatment. After the treatment is completed, a nano-silica modifier is obtained.

[0063] The steps of the step-by-step thermal improvement treatment of this embodiment are:

[0064] First, heat treat at 210℃ for 5 minutes, then cool to 150℃ at a rate of 1℃ / min, keep warm for 10 minutes, then cool to 85℃ at a rate of 2℃ / min, finally water-cool to room temperature and dry.

[0065] Example 2.

[0066] The release agent for aluminum alloy automotive integrated die-casting of this embodiment includes the following raw materials in parts by weight:

[0067] 20 parts of fluorowax emulsion, 8 parts of sodium dodecylbenzenesulfonate, 6 parts of Tween 80, 5 parts of methylphenyl modified silicone oil, 6 parts of graphene regulator, 4 parts of nano-silica modifier, 4 parts of silane coupling agent, and 15 parts of water.

[0068] The silane coupling agent in this embodiment is silane coupling agent KH560.

[0069] The preparation method of the graphene regulator of this embodiment is:

[0070] S01: Add 5 parts by weight of lanthanum chloride solution and 3 parts of glycolic acid to 10 parts of sodium citrate solution, stir and mix, and finally add 4 parts of 5% by mass chitosan solution and stir thoroughly to obtain a pre-modifier;

[0071] S02: Graphene is first placed in a pre-modifier with a volume 5 times the total volume of graphene and stirred for modification. After modification, a modified graphene agent is obtained;

[0072] S03: ball milling and lubricating the modified graphene agent and lubricating liquid in a weight ratio of 5:2. After lubrication, washing with water and drying are completed to obtain a graphene regulator.

[0073] The mass fraction of the lanthanum chloride solution in this embodiment is 5%; the mass fraction of the sodium citrate solution is 15%.

[0074] The stirring temperature of the stirring modification treatment in this embodiment is 50° C., the stirring time is 2 h, and the stirring speed is 500 r / min.

[0075] The lubricating fluid of this embodiment includes the following raw materials in parts by weight:

[0076] 3 parts of urea, 5 parts of nano-silica sol, 5 parts of sodium lignin sulfonate, 8 parts of deionized water and 0.7 parts of nickel powder.

[0077] The ball milling speed of the ball milling lubrication treatment in this embodiment is 1500 r / min, and the ball milling time is 2 h.

[0078] The preparation method of the nano-silica modifier in this embodiment is as follows:

[0079] S101: Stir and mix nano-silica in a sufficient amount of 5% hydrochloric acid solution by mass fraction, then filter, and then stir thoroughly in a sufficient amount of 10% sodium alginate solution by mass fraction. Finally, wash with water and dry.

[0080] S102: Perform stepped thermal improvement treatment on the dried nano-silica. After the treatment is completed, the nano-silica modifier can be obtained.

[0081] The steps of the stepped thermal improvement treatment in this embodiment are as follows:

[0082] First, perform heat treatment at a temperature of 230 °C for 10 min, then cool to 155 °C at a rate of 3 °C / min, keep warm for 15 min, then cool to 95 °C at a rate of 5 °C / min, and finally cool to room temperature with water and dry.

[0083] Example 3.

[0084] The release agent for the integrated die-casting of aluminum alloy automobiles in this embodiment includes the following raw materials in parts by weight:

[0085] 17.5 parts of fluorinated wax emulsion, 7 parts of sodium dodecylbenzenesulfonate, 4.5 parts of Tween 80, 4 parts of methylphenyl modified silicone oil, 5 parts of graphene regulator, 3 parts of nano-silica modifier, 3 parts of silane coupling agent, and 12.5 parts of water.

[0086] The silane coupling agent in this embodiment is silane coupling agent KH560.

[0087] The preparation method of the graphene regulator in this embodiment is as follows:

[0088] S01: Add 3.5 parts by weight of lanthanum chloride solution and 2 parts of glycolic acid to 7.5 parts of sodium citrate solution, stir and mix evenly, and finally add 3 parts of 5% chitosan solution by mass fraction and stir thoroughly to obtain a pre-modifier.

[0089] S02: First, place graphene in 4 times the total amount of graphene of the pre-modifier and stir for modification treatment. After the modification is completed, the modified graphene agent is obtained.

[0090] S03: Perform ball milling lubrication treatment on the modified graphene agent and the lubricating fluid according to a weight ratio of 5:2. After the lubrication is completed, wash with water and dry to obtain the graphene regulator.

[0091] The mass fraction of the lanthanum chloride solution in this embodiment is 3.5%; the mass fraction of the sodium citrate solution is 12.5%.

[0092] The stirring temperature for the stirring modification treatment in this embodiment is 47.5 °C, the stirring time is 1.5 h, and the stirring speed is 470 r / min.

[0093] The lubricating fluid in this embodiment comprises the following raw materials in parts by weight:

[0094] 2 parts of urea, 3.5 parts of nano-silica sol, 4 parts of sodium lignosulfonate, 6 parts of deionized water, and 0.6 part of nickel powder.

[0095] The ball milling speed for the ball milling lubrication treatment in this embodiment is 1000 - 1500 r / min, and the ball milling time is 1 - 2 h.

[0096] The preparation method of the nano-silica modifier in this embodiment is as follows:

[0097] S101: Stir and mix nano-silica in a sufficient amount of 5% hydrochloric acid solution by mass fraction, then filter, and then stir thoroughly in a sufficient amount of 10% sodium alginate solution by mass fraction. Finally, wash with water and dry.

[0098] S102: Perform stepwise thermal improvement treatment on the dried nano-silica. After the treatment is completed, the nano-silica modifier can be obtained.

[0099] The steps of the stepwise thermal improvement treatment in this embodiment are as follows:

[0100] First, perform heat treatment at a temperature of 220 °C for 7.5 min, then cool at a rate of 2 °C / min to 152 °C, keep warm for 12.5 min, then cool at a rate of 3.5 °C / min to 90 °C, and finally cool with water to room temperature and dry.

[0101] Comparative Example 1.

[0102] The difference from Example 3 is that no graphene regulator is added.

[0103] Comparative Example 2.

[0104] The difference from Example 3 is that no pre-modifier treatment is used in the preparation of the graphene regulator.

[0105] Comparative Example 3.

[0106] The difference from Example 3 is that no treatment with lanthanum chloride solution and glycolic acid is used in the preparation of the pre-modifier.

[0107] Comparative Example 4.

[0108] The difference from Example 3 is that no lubricating fluid treatment is used.

[0109] Comparative Example 5.

[0110] The difference from Example 3 is that the components for preparing the lubricating fluid are different; urea and nano-silica sol are not added.

[0111] Comparative Example 6

[0112] It is different from Example 3 in that the components for preparing the lubricating fluid are different; sodium lignosulfonate and nickel powder are not added.

[0113] Comparative Example 7

[0114] It is different from Example 3 in that the nano-silica modifier is not added.

[0115] Comparative Example 8

[0116] It is different from Example 3 in that the stepped thermal improvement treatment is not adopted in the preparation of the nano-silica modifier.

[0117] The raw materials of the products of Examples 1-3 and Comparative Examples 1-8 can be mixed evenly to obtain the products, and then under conventional conditions and placed in a 2% hydrochloric acid mist condition for 12 h, the performance measurement results are as follows

[0118]

[0119] It can be concluded from Examples 1-3 and Comparative Examples 1-8 that the products of Example 3 of the present invention have excellent friction coefficient and adhesion performance. The performance of the prepared products can achieve a coordinated and significant improvement in the friction coefficient and adhesion performance, and the acid corrosion resistance and stability effect of the products are remarkable;

[0120] If one of the graphene regulator and the nano-silica modifier is not added in the present invention, the performance effect of the product is significantly reduced. By using the two in coordination and synergistically, the performance effect of the product is significantly enhanced;

[0121] If the pre-modifier treatment is not adopted in the preparation of the graphene regulator of the present invention, lanthanum chloride solution and glycolic acid treatment are not adopted in the preparation of the pre-modifier, the lubricating fluid treatment is not adopted, and the components for preparing the lubricating fluid are different; urea and nano-silica sol are not added, and the components for preparing the lubricating fluid are different; sodium lignosulfonate and nickel powder are not added, the performance of the product shows a deteriorating trend. At the same time, if the stepped thermal improvement treatment is not adopted in the preparation of the nano-silica modifier, the performance of the product shows a deteriorating trend. Only by using the graphene regulator and nano-silica modifier prepared by the method of the present invention, the performance effect of the product is the most remarkable, and using other methods to replace it is not as obvious as the effect of the present invention.

[0122] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above-described exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention. Therefore, in any aspect, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be embraced within the present invention.

[0123] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative manner of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A mold release agent for integrated die-casting of aluminum alloy automobiles, characterized in that, It includes the following raw materials in parts by weight: 15-20 parts of fluorowax emulsion, 6-8 parts of sodium dodecylbenzenesulfonate, 3-6 parts of Tween 80, 3-5 parts of methylphenyl modified silicone oil, 4-6 parts of graphene regulator, 2-4 parts of nano-silica modifier, 2-4 parts of silane coupling agent, and 10-15 parts of water; the preparation method of the graphene regulator is as follows: S01: Add 2-5 parts by weight of lanthanum chloride solution and 1-3 parts of glycolic acid to 5-10 parts of sodium citrate solution, stir and mix, and finally add 2-4 parts of 5% by weight chitosan solution and stir thoroughly to obtain a pre-modifier; S02: Graphene is first placed in a pre-modifier that is 3-5 times the total amount of graphene and stirred for modification. After the modification is completed, a modified graphene agent is obtained; S03: ball milling the modified graphene agent and lubricating liquid in a weight ratio of 5:2, washing with water, and drying to obtain a graphene conditioning agent; The lubricating fluid comprises the following raw materials in parts by weight: 1-3 parts of urea, 2-5 parts of nano-silica sol, 3-5 parts of sodium lignin sulfonate, 4-8 parts of deionized water and 0.5-0.7 parts of nickel powder; the preparation method of the nano-silica modifier is: S101: Mix the nano-silica in a sufficient amount of 5% by mass hydrochloric acid solution, filter it, and then mix it thoroughly in a sufficient amount of 10% by mass sodium alginate solution, and finally wash it with water and dry it; S102: subjecting the dried nano-silica to a stepwise thermal improvement treatment, and upon completion of the treatment, a nano-silica modifier is obtained; the steps of the stepwise thermal improvement treatment are as follows: First, heat treat at 210-230℃ for 5-10min, then cool to 150-155℃ at a rate of 1-3℃ / min, keep warm for 10-15min, then cool to 85-95℃ at a rate of 2-5℃ / min, finally water-cool to room temperature and dry.

2. The mold release agent for integral die-casting of aluminum alloy automobiles according to claim 1, wherein, The release agent for aluminum alloy automobile integrated die casting comprises the following raw materials in parts by weight: 17.5 parts of fluorowax emulsion, 7 parts of sodium dodecylbenzenesulfonate, 4.5 parts of Tween 80, 4 parts of methylphenyl modified silicone oil, 5 parts of graphene regulator, 3 parts of nano-silica modifier, 3 parts of silane coupling agent, and 12.5 parts of water.

3. The mold release agent for integrated die-casting of aluminum alloy automobiles according to claim 1, wherein, The silane coupling agent is silane coupling agent KH560.

4. The mold release agent for integrated die-casting of aluminum alloy automobiles according to claim 1, characterized in that, The mass fraction of the lanthanum chloride solution is 2-5%; the mass fraction of the sodium citrate solution is 10-15%.

5. The mold release agent for integrated die-casting of aluminum alloy automobiles according to claim 1, characterized in that, The stirring temperature of the stirring modification treatment is 45-50° C., the stirring time is 1-2 hours, and the stirring speed is 450-500 r / min.

6. The mold release agent for integrated die-casting of aluminum alloy automobiles according to claim 1, wherein, The ball milling speed of the ball milling lubrication treatment is 1000-1500 r / min, and the ball milling time is 1-2 hours.

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