A ball milling process for ultra-coarse cemented carbide

By combining ultrasonic mixing with traditional ball milling, the problems of material breakage and uneven dispersion during the ultra-coarse tungsten carbide ball milling process are solved, efficient ultra-coarse tungsten carbide ball milling is achieved, and the uniformity and integrity of the material are ensured.

CN120170090BActive Publication Date: 2025-09-12CHONGYI ZHANGYUAN TUNGSTEN
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Patent Information

Application Number
CN202510645546.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-05-20
Publication Date
2025-09-12
Estimated Expiration
2045-05-20

AI Technical Summary

Technical Problem

In the ball milling process of ultra-coarse tungsten carbide, existing technologies make it difficult to reduce low ball milling efficiency and material breakage while ensuring particle size, and there are problems such as uneven component dispersion, coarse crystal aggregation, and cobalt aggregation.

Method used

The process combines ultrasonic mixing with traditional ball milling. Ultrasonic cavitation is used to fully disperse the ultra-coarse tungsten carbide powder and additives. The liquid-solid ratio and ball-to-material ratio are adjusted in the secondary ball milling to shorten the ball milling time and ensure uniform mixing.

Benefits of technology

The effective dispersion and uniform mixing of ultra-coarse tungsten carbide are achieved, which reduces breakage, improves ball milling efficiency, and avoids defects such as coarse crystal aggregation and cobalt aggregation.

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Abstract

The present invention belongs to the technical field of cemented carbide, and specifically relates to a ball milling process for ultra-coarse cemented carbide, comprising the following steps: S1, weighing ultra-coarse tungsten carbide powder, a binder, and an additive as raw materials according to the composition of the cemented carbide, and taking a forming agent for standby use; S2, adding the binder, additive, and forming agent to a ball mill, then adding oleic acid and anhydrous ethanol for a first ball milling, and after the ball milling is completed, taking out the slurry for standby use; S3, adding anhydrous ethanol, the slurry obtained in step S2, and ultra-coarse tungsten carbide powder to an ultrasonic mixer for ultrasonic mixing, and obtaining a mixed slurry after the mixing is completed; S4, adding the mixed slurry to a ball mill for a second ball milling, and obtaining a final slurry product after the ball milling is completed. The present invention combines ultrasonic mixing with a ball milling process, effectively reducing the breakage of ultra-coarse tungsten carbide particles through an extremely short ball milling time, while ensuring that the components are fully mixed and uniform.
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Description

Technical Field

[0001] The invention belongs to the technical field of cemented carbide, and in particular relates to a ball milling process for ultra-coarse cemented carbide. Background Art

[0002] Cemented carbide is a composite material composed of refractory metal compounds (such as WC, TaC, NbC, and TiC) and a binder metal (such as Co, Ni, and Fe). Produced through a powder metallurgy process, it combines hardness, strength, and toughness. Cemented carbide is widely used as a tool material for turning tools, milling cutters, and planing cutters. Cemented carbide exhibits a range of excellent properties, including high hardness, wear resistance, strength, toughness, heat resistance, and corrosion resistance.

[0003] With the rapid development of national industry, the demand for ultrafine and ultra-coarse particle tungsten carbide cemented carbide materials is gradually increasing. Ultra-coarse particle cemented carbide is in great demand for high impact load conditions in mining. Ultra-coarse particle tungsten carbide is broken by the impact of the grinding balls in the ball mill during the ball milling process. In the preparation of ultra-coarse particle cemented carbide, while ensuring that the raw materials have a certain Fsss particle size, a reasonable ball milling process is also required to reduce the breakage of tungsten carbide during the ball milling process.

[0004] Currently, the ultra-coarse particle milling process uses methods such as reducing the ball-to-material ratio and shortening the milling time to reduce milling efficiency in order to reduce the breakage of ultra-coarse tungsten carbide particles. However, reducing the milling time can easily lead to uneven dispersion of components, resulting in metallographic defects such as coarse crystal aggregation, additive segregation, and cobalt aggregation. Summary of the Invention

[0005] In order to solve the problems existing in the prior art, the main purpose of the present invention is to propose a ball milling process for ultra-coarse cemented carbide.

[0006] To solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:

[0007] A ball milling process for ultra-coarse cemented carbide, comprising the following steps:

[0008] S1. Ingredients: According to the composition of cemented carbide, weigh ultra-coarse tungsten carbide powder, binder, additives as raw materials for batching, and take the forming agent for standby;

[0009] S2, primary ball milling: Add the binder, additives, and forming agent into the ball mill, then add oleic acid and anhydrous ethanol for primary ball milling. After the ball milling is completed, the slurry is taken out for later use;

[0010] S3, ultrasonic mixing: adding anhydrous ethanol, the slurry obtained in step S2, and the ultra-coarse tungsten carbide powder into an ultrasonic mixer for ultrasonic mixing, and obtaining a mixed slurry after the mixing is completed;

[0011] S4. Secondary ball milling: Add the mixed slurry into a ball mill for secondary ball milling. After the ball milling is completed, the final slurry product is obtained.

[0012] As a preferred solution of the ball milling process of an ultra-coarse cemented carbide described in the present invention, wherein: in the step S1, the raw materials are, by weight percentage: 93.5-94wt% of ultra-coarse tungsten carbide powder, 5.5-6.5wt% of binder, and 0-0.5wt% of additives; the forming agent is added separately at 2wt% of the total weight of the raw materials.

[0013] As a preferred solution of the ball milling process of an ultra-coarse cemented carbide described in the present invention, wherein: in the step S1, the average Fsss particle size of the ultra-coarse tungsten carbide powder is 17~23μm, the average Fsss particle size of the binder is 80~120nm, and the average Fsss particle size of the additive is 0.8~1.2μm.

[0014] As a preferred solution of the ball milling process of an ultra-coarse cemented carbide described in the present invention, wherein: in the step S1, the additive is a metal carbide other than tungsten, including at least one of chromium carbide, tantalum carbide, titanium carbide, and niobium carbide, the binder is cobalt powder, and the molding agent is paraffin.

[0015] As a preferred embodiment of the ball milling process for ultra-coarse cemented carbide according to the present invention, in step S2, during the first ball milling process, oleic acid is added at a liquid-solid ratio of 1.4-1.6 mL / kg, anhydrous ethanol is added at a liquid-solid ratio of 0.26-0.28 L / kg, the ball-to-material ratio is (1.5-3):1, the ball milling time is 5-6 h, and the ball mill speed is 36-38 r / min.

[0016] As a preferred solution of the ball milling process for ultra-coarse cemented carbide described in the present invention, wherein: in the step S3, anhydrous ethanol is added at a liquid-solid ratio of 0.6-0.8 L / kg, and the ultrasonic power is 3.0-5.0 kW.

[0017] As a preferred embodiment of the ball milling process of an ultra-coarse cemented carbide according to the present invention, in step S3, the ultra-coarse tungsten carbide powder and the slurry obtained in step S2 are simultaneously added to the ultrasonic mixer, wherein the feeding rate of the ultra-coarse tungsten carbide powder is 1.8-2.2 kg / min, and the feeding rate of the slurry is 0.18-0.22 kg / min.

[0018] As a preferred embodiment of the ball milling process for ultra-coarse cemented carbide according to the present invention, in step S4, during the secondary ball milling process, the liquid-solid ratio is 0.25-0.30 L / kg, the ball-to-material ratio is (1.0-2.0):1, the ball milling time is 2-6 h, and the ball mill speed is 36-38 r / min.

[0019] The beneficial effects of the present invention are as follows:

[0020] 1. The present invention utilizes ultrasonic cavitation to fully disperse and evenly mix the ultra-coarse tungsten carbide powder with the forming agent, binder, additives, etc.; at the same time, ultrasonic driving is utilized to increase the collision between the tungsten carbide particles and activate the tungsten carbide particles. In addition, the nano-scale cobalt powder is selected, which is easier to disperse under the action of ultrasound and has a strong wrapping effect on the ultra-coarse tungsten carbide.

[0021] 2. The two-time ball milling process of the present invention has a shorter grinding time than the traditional ball milling process, which not only ensures the uniform dispersion of the material, but also effectively reduces the breakage of the ultra-coarse tungsten carbide. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying any creative work.

[0023] Figure 1 This is a metallographic photograph of the cemented carbide prepared in Example 1 of the present invention.

[0024] Figure 2 This is a metallographic photograph of the cemented carbide prepared in Example 2 of the present invention.

[0025] Figure 3 This is a metallographic photograph of the cemented carbide prepared in Example 3 of the present invention.

[0026] Figure 4 This is a metallographic photograph of the cemented carbide prepared in Comparative Example 1 of the present invention.

[0027] Figure 5 This is a metallographic photograph of the cemented carbide prepared in Comparative Example 2 of the present invention.

[0028] Figure 6 This is a metallographic photograph of the cemented carbide prepared in Comparative Example 3 of the present invention.

[0029] Figure 7 This is a metallographic photograph of the cemented carbide prepared in Comparative Example 4 of the present invention.

[0030] Figure 8 This is a metallographic photograph of the cemented carbide prepared in Comparative Example 5 of the present invention.

[0031] Figure 9 This is a metallographic photograph of the cemented carbide prepared in Comparative Example 6 of the present invention.

[0032] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION

[0033] The following will be a clear and complete description of the technical solutions in the embodiments. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0034] According to one aspect of the present invention, the present invention provides the following technical solutions:

[0035] A ball milling process for ultra-coarse cemented carbide, comprising the following steps:

[0036] S1. Ingredients: According to the composition of cemented carbide, weigh ultra-coarse tungsten carbide powder, binder, additives as raw materials for batching, and take the forming agent for standby;

[0037] S2, primary ball milling: Add the binder, additives, and forming agent into the ball mill, then add oleic acid and anhydrous ethanol for primary ball milling. After the ball milling is completed, the slurry is taken out for later use;

[0038] S3, ultrasonic mixing: adding anhydrous ethanol, the slurry obtained in step S2, and the ultra-coarse tungsten carbide powder into an ultrasonic mixer for ultrasonic mixing, and obtaining a mixed slurry after the mixing is completed;

[0039] S4. Secondary ball milling: Add the mixed slurry into a ball mill for secondary ball milling. After the ball milling is completed, the final slurry product is obtained.

[0040] The final slurry product obtained by the ball milling process of the present invention can be used for pressing after spray drying. The present invention combines ultrasonic mixing with traditional ball milling technology. Through extremely short ball milling time, the breakage of ultra-coarse tungsten carbide particles is effectively reduced, and at the same time, the components can be fully mixed and uniform.

[0041] Specifically, the present invention utilizes ultrasonic cavitation to fully disperse and evenly mix ultra-coarse tungsten carbide powder, a forming agent, a binder, and additives. Furthermore, ultrasonic waves are used to increase collisions between tungsten carbide particles, activating them. The use of a nanoscale binder facilitates dispersion under the action of ultrasound, providing strong coating for the ultra-coarse tungsten carbide. Compared to traditional ball milling processes, the present invention's double-milling process shortens the milling time, ensuring uniform material dispersion while effectively reducing breakage of the ultra-coarse tungsten carbide.

[0042] Preferably, in step S1, the raw materials are, by weight percentage: 93.5-94 wt% of ultra-coarse tungsten carbide powder, 5.5-6.5 wt% of binder, and 0-0.5 wt% of additive; and the forming agent is added separately at 2 wt% of the total weight of the raw materials.

[0043] Preferably, in step S1, the average Fsss particle size of the ultra-coarse tungsten carbide powder is 17-23 μm, the average Fsss particle size of the binder is 80-120 nm, and the average Fsss particle size of the additive is 0.8-1.2 μm.

[0044] Preferably, in step S1, the additive is a metal carbide other than tungsten, including at least one of chromium carbide, tantalum carbide, titanium carbide, and niobium carbide, the binder is cobalt powder, and the molding agent is paraffin.

[0045] Preferably, in step S2, during the first ball milling process, oleic acid is used to promote the dispersion of paraffin wax, and oleic acid is added at a liquid-solid ratio of 1.4-1.6 mL / kg. Anhydrous ethanol is added as the ball milling medium at a liquid-solid ratio of 0.26-0.28 L / kg. The ball-to-material ratio is (1.5-3):1, the ball milling time is 5-6 h, and the ball mill speed is 36-38 r / min.

[0046] Preferably, in step S3, anhydrous ethanol is added at a liquid-solid ratio of 0.6-0.8 L / kg, and the ultrasonic power is 3.0-5.0 kW.

[0047] Preferably, in step S3, the ultra-coarse tungsten carbide powder and the slurry obtained in step S2 are simultaneously added to the ultrasonic mixer, wherein the ultra-coarse tungsten carbide powder is fed at a rate of 1.8 to 2.2 kg / min, and the slurry is fed at a rate of 0.18 to 0.22 kg / min. After the feeding is completed, mixing is continued for 1 to 1.5 hours.

[0048] Preferably, in step S4, during the secondary ball milling process, the liquid-solid ratio is adjusted (for example, by extracting excess anhydrous ethanol to achieve liquid-solid ratio adjustment) to 0.25-0.30 L / kg, the ball-to-material ratio is (1.0-2.0):1, the ball milling time is 2-6 h, and the ball mill speed is 36-38 r / min.

[0049] The technical solution of the present invention is further described below with reference to specific embodiments.

[0050] Example 1

[0051] A ball milling process for ultra-coarse cemented carbide comprises the following steps:

[0052] S1. Ingredients: According to the composition of cemented carbide, weigh ultra-coarse tungsten carbide powder, binder, and additives as raw materials for batching, and take a molding agent for standby; in terms of weight percentage, the raw materials are: ultra-coarse tungsten carbide powder 93.7wt%, binder 6.0wt%, additive 0.3wt%; the molding agent is added separately at 2wt% of the total weight of the raw materials. The average Fsss particle size of the ultra-coarse tungsten carbide powder is 20μm, the average Fsss particle size of the binder is 100nm, and the average Fsss particle size of the additive is 1.0μm. The additive is tantalum carbide, the binder is cobalt powder, and the molding agent is paraffin wax;

[0053] S2. Primary ball milling: Add the binder, additives, and forming agent to a ball mill, then add oleic acid and anhydrous ethanol for primary ball milling. After the ball milling is completed, the slurry is removed for later use; oleic acid is added at a liquid-to-solid ratio of 1.5 mL / kg, and anhydrous ethanol is added at a liquid-to-solid ratio of 0.26 L / kg. The ball-to-material ratio is 2:1, the ball milling time is 5 h, and the ball mill speed is 38 rpm;

[0054] S3. Ultrasonic mixing: Anhydrous ethanol, the slurry obtained in step S2, and ultra-coarse tungsten carbide powder are added to an ultrasonic mixer for ultrasonic mixing to obtain a mixed slurry. Anhydrous ethanol is added at a liquid-to-solid ratio of 0.8 L / kg and an ultrasonic power of 4.5 kW. The ultra-coarse tungsten carbide powder and the slurry obtained in step S2 are simultaneously added to the ultrasonic mixer. The ultra-coarse tungsten carbide powder is fed at a rate of 2.0 kg / min, and the slurry is fed at a rate of 0.2 kg / min. Mixing is continued for 1 hour after the feeding is completed.

[0055] S4. Secondary ball milling: Add the mixed slurry into a ball mill, adjust the liquid-solid ratio to 0.28 L / kg, and perform secondary ball milling with a ball-to-material ratio of 1:1, a ball milling time of 3 h, and a ball mill speed of 36 r / min; after the ball milling is completed, the final slurry product is obtained.

[0056] The final slurry product is spray-dried and then pressed and sintered to obtain cemented carbide, such as Figure 1 shown.

[0057] Example 2

[0058] A ball milling process for ultra-coarse cemented carbide comprises the following steps:

[0059] S1. Ingredients: According to the composition of cemented carbide, ultra-coarse tungsten carbide powder, binder, and additives are weighed as raw materials for batching, and a molding agent is taken for standby use; in terms of weight percentage, the raw materials are: ultra-coarse tungsten carbide powder 93.5wt%, binder 6wt%, additive (0.5wt%; the molding agent is added separately at 2wt% of the total weight of the raw materials. The average Fsss particle size of the ultra-coarse tungsten carbide powder is 20μm, the average Fsss particle size of the binder is 100nm, and the average Fsss particle size of the additive is 1.0μm. The additive (is chromium carbide and tantalum carbide in a mass ratio of 3:2, the binder is cobalt powder, and the molding agent is paraffin;

[0060] S2. Primary ball milling: Add the binder, additives, and forming agent to a ball mill, then add oleic acid and anhydrous ethanol for primary ball milling. After the ball milling is completed, the slurry is removed for later use; oleic acid is added at a liquid-to-solid ratio of 1.5 mL / kg, and anhydrous ethanol is added at a liquid-to-solid ratio of 0.26 L / kg. The ball-to-material ratio is 2:1, the ball milling time is 5 h, and the ball mill speed is 38 rpm;

[0061] S3. Ultrasonic mixing: Anhydrous ethanol, the slurry obtained in step S2, and ultra-coarse tungsten carbide powder are added to an ultrasonic mixer for ultrasonic mixing to obtain a mixed slurry. Anhydrous ethanol is added at a liquid-to-solid ratio of 0.8 L / kg and an ultrasonic power of 4.0 kW. The ultra-coarse tungsten carbide powder and the slurry obtained in step S2 are simultaneously added to the ultrasonic mixer. The ultra-coarse tungsten carbide powder is fed at a rate of 2.0 kg / min, and the slurry is fed at a rate of 0.2 kg / min. Mixing is continued for 1 hour after the feeding is completed.

[0062] S4. Secondary ball milling: Add the mixed slurry into a ball mill, adjust the liquid-solid ratio to 0.28 L / kg, and perform secondary ball milling with a ball-to-material ratio of 1:1, a ball milling time of 3 h, and a ball mill speed of 36 r / min; after the ball milling is completed, the final slurry product is obtained.

[0063] The final slurry product is spray-dried and then pressed and sintered to obtain cemented carbide, such as Figure 2 shown.

[0064] Example 3

[0065] A ball milling process for ultra-coarse cemented carbide comprises the following steps:

[0066] S1. Ingredients: According to the composition of cemented carbide, weigh ultra-coarse tungsten carbide powder and binder as raw materials for batching, and take a molding agent for standby; by weight percentage, the raw materials are: ultra-coarse tungsten carbide powder 94wt%, binder 6wt%; the molding agent is added separately at 2wt% of the total weight of the raw materials. The average Fsss particle size of the ultra-coarse tungsten carbide powder is 20μm, the average Fsss particle size of the binder is 100nm, the binder is cobalt powder, and the molding agent is paraffin wax;

[0067] S2, primary ball milling: Add the binder and forming agent to the ball mill, then add oleic acid and anhydrous ethanol for primary ball milling. After the ball milling is completed, the slurry is taken out for use; oleic acid is added at a liquid-to-solid ratio of 1.5 mL / kg, and anhydrous ethanol is added at a liquid-to-solid ratio of 0.26 L / kg. The ball-to-material ratio is 2:1, the ball milling time is 6 h, and the ball mill speed is 38 rpm;

[0068] S3. Ultrasonic mixing: Anhydrous ethanol, the slurry obtained in step S2, and ultra-coarse tungsten carbide powder are added to an ultrasonic mixer for ultrasonic mixing to obtain a mixed slurry. Anhydrous ethanol is added at a liquid-to-solid ratio of 0.8 L / kg and an ultrasonic power of 4.0 kW. The ultra-coarse tungsten carbide powder and the slurry obtained in step S2 are simultaneously added to the ultrasonic mixer. The ultra-coarse tungsten carbide powder is fed at a rate of 2.0 kg / min, and the slurry is fed at a rate of 0.2 kg / min. Mixing is continued for 1 hour after the feeding is completed.

[0069] S4. Secondary ball milling: Add the mixed slurry into a ball mill, adjust the liquid-solid ratio to 0.28 L / kg, and perform secondary ball milling with a ball-to-material ratio of 1:1, a ball milling time of 3 h, and a ball mill speed of 36 r / min; after the ball milling is completed, the final slurry product is obtained.

[0070] The final slurry product is spray-dried and then pressed and sintered to obtain cemented carbide, such as Figure 3 shown.

[0071] Comparative Example 1

[0072] The process steps of this comparative example are as follows:

[0073] S1. Ingredients: According to the composition of cemented carbide, weigh ultra-coarse tungsten carbide powder, binder, and additives as raw materials for batching, and take a molding agent for standby use; in terms of weight percentage, the raw materials are: ultra-coarse tungsten carbide powder 93.7wt%, binder 6wt%, additive 0.3wt%; the molding agent is added separately at 2wt% of the total weight of the raw materials. The average Fsss particle size of the ultra-coarse tungsten carbide powder is 20μm, the average Fsss particle size of the binder is 100nm, and the average Fsss particle size of the additive is 1.0μm. The additive is tantalum carbide powder, the binder is cobalt powder, and the molding agent is paraffin wax;

[0074] S2. Ball milling: Add the ultra-coarse tungsten carbide powder, cobalt powder, tantalum carbide powder, and paraffin wax prepared in step 1 into a ball mill, add oleic acid at a liquid-to-solid ratio of 1.5 mL / kg, and then add anhydrous ethanol at a liquid-to-solid ratio of 0.26 L / kg. Mill the mixture in a ball mill at a ball-to-material ratio of 2:1 for 8 h at a ball mill speed of 36 r / min to obtain a slurry.

[0075] The slurry is spray-dried and then pressed and sintered to obtain cemented carbide, such as Figure 4 shown.

[0076] Comparative Example 2

[0077] The process steps of this comparative example are as follows:

[0078] S1. Ingredients: According to the composition of cemented carbide, ultra-coarse tungsten carbide powder, binder, and additives are weighed as raw materials for batching, and a molding agent is prepared for use; in terms of weight percentage, the raw materials are: 93.5wt% of ultra-coarse tungsten carbide powder, 6wt% of binder, and 0.5wt% of additive; the molding agent is added separately at 2wt% of the total weight of the raw materials. The average Fsss particle size of the ultra-coarse tungsten carbide powder is 20μm, the average Fsss particle size of the binder is 100nm, and the average Fsss particle size of the additive is 1.0μm. The additives are chromium carbide and tantalum carbide in a mass ratio of 3:2, the binder is cobalt powder, and the molding agent is paraffin wax;

[0079] S2. Ball milling: Add the ultra-coarse tungsten carbide powder, cobalt powder, tantalum carbide powder, chromium carbide powder, and paraffin wax prepared in step 1 into a ball mill, add oleic acid at a liquid-to-solid ratio of 1.5 mL / kg, and then add anhydrous ethanol at a liquid-to-solid ratio of 0.26 L / kg. Mill the mixture in a ball mill at a ball-to-material ratio of 2:1 for 8 h at a ball mill speed of 36 r / min to obtain a slurry.

[0080] The slurry is spray-dried and then pressed and sintered to obtain cemented carbide, such as Figure 5 shown.

[0081] Comparative Example 3

[0082] The process steps of this comparative example are as follows:

[0083] S1. Ingredients: According to the composition of cemented carbide, weigh ultra-coarse tungsten carbide powder and binder as raw materials for batching, and take a molding agent for standby; by weight percentage, the raw materials are: ultra-coarse tungsten carbide powder 94wt%, binder 6wt%; the molding agent is added separately at 2wt% of the total weight of the raw materials. The average Fsss particle size of the ultra-coarse tungsten carbide powder is 20μm, the average Fsss particle size of the binder is 100nm, the binder is cobalt powder, and the molding agent is paraffin wax;

[0084] S2. Ball milling: Add the ultra-coarse tungsten carbide powder, cobalt powder, and paraffin wax prepared in step 1 into a ball mill, add oleic acid at a liquid-to-solid ratio of 1.5 mL / kg, and then add anhydrous ethanol at a liquid-to-solid ratio of 0.26 L / kg. Mill the mixture in a ball mill at a ball-to-material ratio of 2:1 for 8 h at a ball mill speed of 36 r / min to obtain a slurry.

[0085] The slurry is spray-dried and then pressed and sintered to obtain cemented carbide, such as Figure 6 shown.

[0086] Comparative Example 4

[0087] The difference from Example 3 is that the average Fsss particle size of the cobalt powder is 0.9 μm.

[0088] The slurry prepared in this comparative example is spray-dried and then pressed and sintered to obtain a cemented carbide. Figure 7 shown.

[0089] Comparative Example 5

[0090] The difference from Example 3 is that the average Fsss particle size of the cobalt powder is 1.1 μm.

[0091] The slurry prepared in this comparative example is spray-dried and then pressed and sintered to obtain a cemented carbide. Figure 8 shown.

[0092] Comparative Example 6

[0093] The difference from Example 3 is that the ultrasonic power is 1.5 kW.

[0094] The slurry prepared in this comparative example is spray-dried and then pressed and sintered to obtain a cemented carbide. Figure 9 shown.

[0095] The above examples and comparative examples were vacuum sintered in the same furnace and in the same area, and metallographic examination was performed after sintering (see Figure 1-9 ), the results are shown in Table 1:

[0096] Table 1 Test results

[0097]

[0098] It can be seen from the above embodiments and comparative examples that the embodiments of the method of the present invention can effectively reduce porosity and the occurrence of cobalt aggregation, additive segregation, coarse crystal aggregation and other component unevenness problems while ensuring the integrity of tungsten carbide.

[0099] The above description is only a preferred embodiment of the present invention and does not limit the patent scope of the present invention. All equivalent structural transformations made by using the contents of the present invention specification under the inventive concept of the present invention, or direct / indirect application in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. A ball milling process for ultra-coarse cemented carbide, characterized in that: The process comprises the following steps: S1. Ingredients: According to the composition of cemented carbide, weigh ultra-coarse tungsten carbide powder, binder, and additives as raw materials for batching, and take a forming agent for standby; the average Fsss particle size of the binder is 80-120nm; the additive is other metal carbide other than tungsten, including at least one of chromium carbide, tantalum carbide, titanium carbide, and niobium carbide; S2, primary ball milling: Add the binder, additives, and forming agent into the ball mill, then add oleic acid and anhydrous ethanol for primary ball milling. After the ball milling is completed, the slurry is taken out for later use; S3, ultrasonic mixing: adding anhydrous ethanol, the slurry obtained in step S2, and the ultra-coarse tungsten carbide powder into an ultrasonic mixer for ultrasonic mixing at an ultrasonic power of 3.0-5.0 kW to obtain a mixed slurry after the mixing is completed; S4. Secondary ball milling: After recovering the anhydrous ethanol in the mixed slurry, the mixed slurry is added to a ball mill for secondary ball milling. After the ball milling is completed, the final slurry product is obtained.

2. The ball milling process of ultra-coarse cemented carbide according to claim 1, characterized in that: In step S1, the raw materials are as follows, calculated by weight percentage: 93.5-94 wt % of ultra-coarse tungsten carbide powder, 5.5-6.5 wt % of binder, and 0-0.5 wt % of additives.

3. The ball milling process of ultra-coarse cemented carbide according to claim 2, characterized in that: In step S1, the forming agent is added separately at 2 wt % of the total weight of the raw materials.

4. The ball milling process of ultra-coarse cemented carbide according to claim 2, characterized in that: In the step S1, the average Fsss particle size of the ultra-coarse tungsten carbide powder is 17-23 μm, and the average Fsss particle size of the additive is 0.8-1.2 μm.

5. The ball milling process of ultra-coarse cemented carbide according to claim 2, characterized in that: In the step S1, the binder is cobalt powder and the molding agent is paraffin.

6. The ball milling process of ultra-coarse cemented carbide according to claim 1, characterized in that: In step S2, during the first ball milling process, oleic acid is added at a liquid-solid ratio of 1.4-1.6 mL / kg, anhydrous ethanol is added at a liquid-solid ratio of 0.26-0.28 L / kg, the ball-to-material ratio is (1.5-3):1, the ball milling time is 5-6 h, and the ball mill speed is 36-38 r / min.

7. The ball milling process of ultra-coarse cemented carbide according to claim 1, characterized in that: In step S3, anhydrous ethanol is added at a liquid-to-solid ratio of 0.6-0.8 L / kg.

8. The ball milling process of ultra-coarse cemented carbide according to claim 1, characterized in that: In step S3, the ultra-coarse tungsten carbide powder and the slurry obtained in step S2 are simultaneously added to the ultrasonic mixer, wherein the feeding rate of the ultra-coarse tungsten carbide powder is 1.8-2.2 kg / min, and the feeding rate of the slurry is 0.18-0.22 kg / min.

9. The ball milling process of ultra-coarse cemented carbide according to claim 1, characterized in that: In the step S4, during the secondary ball milling process, the liquid-solid ratio is 0.25-0.30 L / kg, the ball-to-material ratio is (1.0-2.0):1, the ball milling time is 2-6 h, and the ball mill speed is 36-38 r / min.

Citation Information

Patent Citations

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