CN113681010B - Wear-resistant and corrosion-resistant hard alloy milling cutter and preparation method thereof - Google Patents

Wear-resistant and corrosion-resistant hard alloy milling cutter and preparation method thereof Download PDF

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CN113681010B
CN113681010B CN202110984900.4A CN202110984900A CN113681010B CN 113681010 B CN113681010 B CN 113681010B CN 202110984900 A CN202110984900 A CN 202110984900A CN 113681010 B CN113681010 B CN 113681010B
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milling cutter
heating
speed
reactor
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CN113681010A (en
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刘天桂
黎明林
肖孝超
高建华
刘阳
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Ji'an Fuqi Precision Manufacturing Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1021—Removal of binder or filler
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F3/26—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23C—MILLING
    • B23C5/00—Milling-cutters
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/06—Surface hardening
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/60—Aqueous agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23C—MILLING
    • B23C2222/00—Materials of tools or workpieces composed of metals, alloys or metal matrices
    • B23C2222/28—Details of hard metal, i.e. cemented carbide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23C—MILLING
    • B23C2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
    • B23C2228/49—Sintered

Abstract

The invention provides a wear-resistant and corrosion-resistant hard alloy milling cutter and a preparation method thereof. The invention selects the powder metallurgy method to prepare the milling cutter, can effectively reduce segregation in cast ingot, can lead the structure uniformity in alloy to be more wear-resistant, and the milling cutter alloy selects tungsten carbide and titanium carbide as reinforcing materials of the milling cutter, thereby enhancing the strength and wear resistance of the milling cutter, and effectively improving the dispersity of various atoms in the milling cutter by modifying alloy powder. And the plasticizer is added, so that the metal powder can be effectively connected, the alloy is made into a whole, and cracks on the surface of a metal piece are prevented after the metal piece is pressed. The quenching medium can be used for rapidly cooling the surface of the milling cutter, but still keeps the toughness of the alloy inside, and can improve the corrosion resistance of the milling cutter. The quenching medium also contains a cleaning agent and a brightening agent, so that the quenched alloy surface is bright and clean.

Description

Wear-resistant and corrosion-resistant hard alloy milling cutter and preparation method thereof
Technical field:
the invention relates to the technical field related to machining, in particular to an anti-corrosion and wear-resistant hard alloy milling cutter and a preparation method thereof.
Technical Field
Milling tools are rotary tools for milling machining having one or more cutter teeth. When in operation, each cutter tooth cuts off the allowance of the workpiece intermittently in sequence. Milling cutters are mainly used for machining planes, steps, grooves, forming surfaces, cutting workpieces, etc. on milling machines. Milling cutters are broadly divided into two categories: the sharp-tooth milling cutter has the advantages that a narrow cutting edge is ground on the rear cutter surface to form a rear angle, and the service life is longer due to reasonable cutting angle. The back of the tooth of the sharp-tooth milling cutter has 3 forms of straight line, curve and fold line. Linear tooth backs are commonly used in fine tooth finishing mills. The cutter teeth with curve and broken line tooth backs have better strength, can bear heavier cutting load, and are commonly used for coarse tooth milling cutters. The back of the relieved tooth milling cutter is processed into the tooth back of the Archimedes spiral line by a relieving method, and the front of the milling cutter only needs to be regrinded after the milling cutter is dulled, so that the original tooth shape can be kept unchanged, and the relieved tooth milling cutter can be used for manufacturing various formed milling cutters such as gear milling cutters.
With the further development of the China industry, the cutting technology is gradually advanced towards the high-speed, high-efficiency and dry type. High-speed milling is currently the main process for high-speed cutting applications, and high-speed milling is one of the important technologies for realizing high-speed milling. The high-speed cutting technology integrates high efficiency, high quality and low consumption, has high cutting efficiency, good surface machining quality and small unit cutting force, and has higher requirements on the corrosion resistance and wear resistance of the cutter material. In the working process of the milling cutter, the cutting edge of the milling cutter is severely worn due to frequent cutting of hard alloy such as steel, the milling cutter prepared by the ingot casting process at present can generate serious waste of metal materials in the preparation process, 80% of metal is generally consumed in the processing process, and the ingot casting process has extremely high energy requirement. Aiming at the problems, the invention selects powder metallurgy to prepare the milling cutter, provides a process for quenching the surface of the milling cutter, enhances the strength of the milling cutter, and effectively solves the problems of abrasion and corrosion of the milling cutter, in order to solve the problems of lower surface hardness and extremely easy abrasion and corrosion of the milling cutter prepared by powder metallurgy.
Disclosure of Invention
The invention mainly aims to provide a wear-resistant and corrosion-resistant hard alloy milling cutter and a preparation method thereof.
The second object of the invention is to provide a preparation process of modified alloy powder in the wear-resistant and corrosion-resistant hard alloy milling cutter.
The third object of the invention is to provide a method for preparing the plasticizer of the wear-resistant and corrosion-resistant hard alloy milling cutter.
The fourth object of the invention is to provide a surface quenching method of a wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method comprises the following steps:
a wear-resistant and corrosion-resistant cemented carbide milling cutter, wherein the milling cutter comprises the following raw materials: 25-35 parts of modified alloy powder, 0.5-1 part of tungsten carbide powder, 0.5-1 part of titanium carbide powder, 0.1-0.2 part of cobalt powder and 0.1-0.2 part of plasticizer.
The preparation method of the milling cutter comprises the following steps:
1) Putting 25-35 parts of prepared modified alloy powder, 0.5-1 part of tungsten carbide powder, 0.5-1 part of titanium carbide powder and 0.1-0.2 part of cobalt powder into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 10-12 ℃/min, keeping the temperature for sintering for 25-30min, heating to 1450 ℃ at the speed of 5-8 ℃/min, keeping the temperature for sintering for 15-20min, cooling to 1000 ℃ at the cooling speed of 2-4 ℃/min, keeping the temperature for sintering for 2h, and cooling to room temperature at the speed of 1-1.5 ℃/min;
4) And (3) carrying out surface quenching treatment on the sintered milling cutter, heating the surface of the milling cutter to 1350 ℃, immediately placing the milling cutter into a quenching medium for quenching, carrying out polishing treatment on the quenched milling cutter, and placing the polished milling cutter into organic soaking oil for oil immersion for 5 hours to obtain the finished product.
The preparation method of the modified alloy powder comprises the following steps:
1) Adding 3-4 parts of iron into 12-15 parts of No. 45 steel, putting the steel into a high-temperature furnace, heating to 1800 ℃, adding 0.05-0.1 part of nickel and 0.2-0.4 part of silicon carbide into the steel, heating to 1950 ℃ until uniform alloy liquid is formed, and preserving heat to obtain alloy liquid a for later use;
2) Placing 0.4-0.5 part of beryllium oxide and 0.2-0.3 part of titanium oxide into a high-temperature furnace, heating to 2390 ℃, preserving heat for 3-4 hours, adding 0.5-0.8 part of chromium and 0.2-0.4 part of copper again, heating to 2500 ℃ together, preserving heat for 15-30 minutes, and cooling to 1700 ℃ at a speed of 2-3 ℃/min to obtain alloy liquid b;
3) Mixing the alloy liquid a and the alloy liquid b, heating the alloy liquid a and the alloy liquid b to 2100 ℃, preserving heat for 30-50min, cooling the alloy liquid a to 1200 ℃ at the speed of 1-3 ℃/min, preserving heat for 40-60min, heating the alloy liquid a to 1500 ℃ at the speed of 1-3 ℃/min, and standing and preserving heat for 20-30min to obtain a metal liquid c;
4) And (3) preparing the prepared metal liquid c into alloy powder by an atomization method, wherein the prepared alloy powder can pass through a 800-mesh sieve to obtain the alloy powder.
The preparation method of the plasticizer comprises the following steps:
1) Placing 8-12 parts of vinyl alcohol into a reactor, adding 4-6 parts of 1, 3-butadiene into the reactor, adding concentrated sulfuric acid into the reactor, heating to 90-95 ℃ at the speed of 2-4 ℃/min, and carrying out heat preservation reaction for 4-6 hours to obtain a product i;
2) Adding 5-7 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 1-3 ℃/min, and carrying out heat preservation reaction for 3-4 hours to obtain a product ii;
3) Adding 3-4 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 6-9 ℃/min, and carrying out heat preservation reaction for 3-4 hours to obtain a product iii;
4) Taking 5-8 parts of a product iii), adding 8-10 parts of decaglycerol decastearate, and adding ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 8-10 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 5-7h to obtain a product iv;
5) 15-20 parts of liquid paraffin, adding 1-2 parts of product iv, heating to 60 ℃ at the speed of 3-5 ℃/min, stirring while heating, and reacting for 3-4 hours after uniformly stirring.
The preparation method of the quenching medium comprises the following steps:
a. 10-13 parts of ethylene propylene diene monomer is put into a reactor, 5-7 parts of 4, 4-dimethoxy-2-butanone is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 130 ℃, and the reaction is carried out for 3-4 hours under the condition of heat preservation, thus obtaining a reactant a;
b. adding 3-5 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 1-3 ℃/min, and carrying out heat preservation reaction for 3-4 hours to obtain a reactant b;
c. 5-8 parts of thiazolidinethione is put into a reactor, 6-10 parts of alkylphenol ethoxylates are added into the reactor, methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 3-5 ℃/min, and the reaction is carried out for 3-4 hours under heat preservation, thus obtaining a reactant c;
d. putting 6-9 parts of reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 1-3 ℃/min, dripping 5-8 parts of reactant c into the reactor at a speed of 15-20 drops/min, heating to 90-95 ℃, and reacting for 3-4 hours at a temperature maintaining to obtain a reactant d;
e. adding 5-8 parts of sodium thiodipropyl sulfonate into the reactant d, adding an ethyl acetate solution, heating to 95-100 ℃ at the speed of 4-6 ℃/min, and carrying out heat preservation reaction for 5-6h to obtain the catalyst.
The organic soaking oil is as follows: 35-40 parts of mechanical oil, 1-2 parts of tert-butyl hydroquinone, 3-5 parts of triethanolamine sodium hydrochloride and 2-6 parts of 1, 3-dihydroxyurea, and uniformly mixing the components to obtain the finished product.
The invention has the following advantages:
the milling cutter is prepared by adopting a powder metallurgy method, and the powder metallurgy can be pressed into a pressed compact with a final size without using mechanical processing. The loss of metal produced by this method is only 1-5%, while the typical processing consumes 80% of the metal. Meanwhile, the milling cutter is prepared through powder metallurgy, segregation in an ingot can be effectively reduced by adopting a powder metallurgy method, and the structure uniformity in the alloy can be improved, so that the alloy is more wear-resistant, wherein the milling cutter alloy adopts tungsten carbide and titanium carbide as reinforcing materials of the milling cutter. In tungsten carbide, carbon atoms are intercalated into the interstices of the tungsten metal lattice and do not disrupt the original metal lattice to form interstitial solid solutions, and are therefore also known as interstitial compounds. The tungsten carbide is suitable for mechanical processing at high temperature, and can be used for manufacturing cutting tools, structural materials of kilns, jet engines, gas turbines, nozzles and the like; the hard particles TiC with a certain proportion are dispersed in the matrix, so that the hardness is further improved, and the fracture toughness is improved to a certain extent, so that the cutting performance is greatly improved compared with a pure cutter. According to the invention, modified hard alloy powder is used instead of metal powder, and the modified hard alloy powder is simply mixed together, and solid solution atoms can be effectively fused into a matrix through a special heat treatment process in the preparation of modified alloy liquid, so that the hardness of the prepared modified alloy powder is greatly improved, the dispersity of metal in a milling cutter is effectively improved, and the strength of the milling cutter is improved; meanwhile, the wear resistance of the metal is increased by adopting metal carbide, and the impact resistance of the cutter can be increased by distributing the metal carbide on the surrounding steel matrix. When the modified alloy powder is prepared, the alloy liquid is atomized by a nozzle, and the prepared steel particles can effectively improve the condition of uneven particle distribution in the milling cutter. In the sintering process, the temperature is controlled to achieve effective sintering among metal particles, so that the void ratio is reduced to the greatest extent, and the strength of the milling cutter is increased.
The most critical process in powder metallurgy is to reduce the gaps between powders and prevent the performance such as hardness, brittleness and the like of the alloy from being reduced due to overlarge void ratio. The invention provides a plasticizer and a preparation process thereof, wherein the plasticizer can mold metal powder into the shape of a milling cutter, and can be used as a binder at the same time, the metal powder is effectively connected, so that the alloy is made into a whole, and the surface of a metal piece is prevented from cracking after being pressed; meanwhile, the plasticizer can not react with alloy metal powder in a high-temperature environment, can be pyrolyzed in the high-temperature environment, and can not leave carbon in the metal piece, so that the defect in the metal piece is caused, and the service life of the milling cutter is influenced. The components in the plasticizer have larger viscosity, the consumption is less, and the less standing adhesive can lead the mixture to generate better rheological property, so that the metal piece is easy to be molded in the isostatic pressing process.
Because the modified alloy powder and the plasticizer are used in the invention, the powder prepared by high-temperature metallurgy has uniform surface structure components and good toughness, but in the cutting process of the milling cutter, the cutting scraps are extremely easy to damage the surface of the milling cutter under the conditions of high temperature and high speed, and the damaged surface of the milling cutter is extremely easy to corrode, so that the service life of the milling cutter is reduced. Therefore, the inventor tries to carry out surface quenching technology on the prepared alloy surface, increase the surface hardness of the hard alloy cutter and improve the wear resistance of the hard alloy cutter, but the inventor finds that the common quenching medium is selected to improve the hardness of the surface of the hard alloy cutter, but simultaneously increases the brittleness of the milling cutter, so that the milling cutter is extremely easy to generate brittle fracture. Therefore, the surface quenching medium matched with the milling cutter can be used for rapidly cooling the surface of the milling cutter, the toughness of the alloy in the milling cutter is still reserved, meanwhile, the effective components in the quenching medium can form a layer of film on the surface during the quenching of the milling cutter, and the corrosion resistance of the milling cutter is improved. Wherein, the quenching medium contains cleaning agent and brightening agent at the same time, which can make the quenched alloy surface smooth and bright. The anti-corrosion capability of the milling cutter is further enhanced by matching with organic soaking oil for oil immersion, wherein the organic soaking oil contains an anti-corrosion component, so that the rust condition of the milling cutter is effectively reduced, and the service life of the milling cutter is prolonged.
Detailed description of the preferred embodiments
Example 1
A wear-resistant and corrosion-resistant cemented carbide milling cutter, wherein the milling cutter comprises the following raw materials: 30 parts of modified alloy powder, 0.8 part of tungsten carbide powder, 0.8 part of titanium carbide powder, 0.15 part of cobalt powder and 0.15 part of plasticizer.
The preparation method of the milling cutter comprises the following steps:
1) 30 parts of prepared modified alloy powder, 0.8 part of tungsten carbide powder, 0.8 part of titanium carbide powder and 0.15 part of cobalt powder are put into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.3 ℃/min;
4) And (3) carrying out surface quenching treatment on the sintered milling cutter, heating the surface of the milling cutter to 1350 ℃, immediately placing the milling cutter into a quenching medium for quenching, carrying out polishing treatment on the quenched milling cutter, and placing the polished milling cutter into organic soaking oil for oil immersion for 5 hours to obtain the finished product.
The preparation method of the modified alloy powder comprises the following steps:
1) Adding 3.5 parts of iron into 14 parts of No. 45 steel, putting the steel into a high-temperature furnace, heating to 1800 ℃, adding 0.08 part of nickel and 0.3 part of silicon carbide into the steel, heating to 1950 ℃ until uniform alloy liquid is formed, and preserving heat to obtain alloy liquid a for later use;
2) Placing 0.45 part of beryllium oxide and 0.25 part of titanium oxide into a high-temperature furnace, heating to 2390 ℃, preserving heat for 3.5 hours, adding 0.6 part of chromium and 0.3 part of copper again, heating to 2500 ℃ together, preserving heat for 22 minutes, and cooling to 1700 ℃ at a speed of 2.5 ℃/min to obtain alloy liquid b;
3) Mixing the alloy liquid a and the alloy liquid b, heating the alloy liquid a and the alloy liquid b to 2100 ℃, preserving heat for 40min, cooling the alloy liquid a and the alloy liquid b to 1200 ℃ at the speed of 2 ℃/min, preserving heat for 50min, heating the alloy liquid a and the alloy liquid b to 1500 ℃ at the speed of 2 ℃/min, and preserving heat for 25min to obtain a metal liquid c;
4) And (3) preparing the prepared metal liquid c into alloy powder by an atomization method, wherein the prepared alloy powder can pass through a 800-mesh sieve to obtain the alloy powder.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 93 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 6 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking out the product iii 7 parts, adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The preparation method of the quenching medium comprises the following steps:
a. placing 12 parts of ethylene propylene diene monomer into a reactor, adding 6 parts of 4, 4-dimethoxy-2-butanone into the reactor, adding concentrated sulfuric acid into the reactor, heating the mixture to 130 ℃, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant a;
b. adding 4 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant b;
c. 7 parts of thiazolidinethione is put into a reactor, 8 parts of alkylphenol ethoxylates are added into the reactor, a methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 4 ℃/min, and the reaction is carried out for 3.5 hours under the condition of heat preservation, thus obtaining a reactant c;
d. putting 8 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 2 ℃/min, dropwise adding 7 parts of a reactant c into the reactor at a speed of 18 drops/min, heating to 93 ℃, and reacting for 3.5 hours at a temperature of 3.5 hours to obtain a reactant d;
e. and 7 parts of sodium thiosulfopropane sulfonate is added into the reactant d, an ethyl acetate solution is added, the temperature is raised to 98 ℃ at the speed of 5 ℃/min, and the reaction is carried out for 5.5 hours.
The organic soaking oil is as follows: 38 parts of mechanical oil, 1.5 parts of tert-butyl hydroquinone, 4 parts of triethanolamine sodium hydrochloride and 4 parts of 1, 3-dihydroxyurea, and uniformly mixing the components to obtain the finished product.
Example 2
A wear-resistant and corrosion-resistant cemented carbide milling cutter, wherein the milling cutter comprises the following raw materials: 25 parts of modified alloy powder, 1 part of tungsten carbide powder, 0.5 part of titanium carbide powder, 0.2 part of cobalt powder and 0.1 part of plasticizer.
The preparation method of the milling cutter comprises the following steps:
1) Putting 25 parts of prepared modified alloy powder, 1 part of tungsten carbide powder, 0.5 part of titanium carbide powder and 0.2 part of cobalt powder into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 12 ℃/min, preserving heat and sintering for 30min, heating to 1450 ℃ at the speed of 5 ℃/min, preserving heat and sintering for 20min, cooling to 1000 ℃ at the cooling speed of 2 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.5 ℃/min;
4) And (3) carrying out surface quenching treatment on the sintered milling cutter, heating the surface of the milling cutter to 1350 ℃, immediately placing the milling cutter into a quenching medium for quenching, carrying out polishing treatment on the quenched milling cutter, and placing the polished milling cutter into organic soaking oil for oil immersion for 5 hours to obtain the finished product.
The preparation method of the modified alloy powder comprises the following steps:
1) Adding 4 parts of iron into 12 parts of No. 45 steel, putting the steel into a high-temperature furnace, heating to 1800 ℃, adding 0.05 part of nickel and 0.4 part of silicon carbide into the steel, heating to 1950 ℃ until uniform alloy liquid is formed, and preserving heat to obtain alloy liquid a for later use;
2) Placing 0.4 part of beryllium oxide and 0.3 part of titanium oxide into a high-temperature furnace, heating to 2390 ℃, preserving heat for 3 hours, adding 0.8 part of chromium and 0.2 part of copper again, heating to 2500 ℃ together, preserving heat for 30 minutes, and cooling to 1700 ℃ at a speed of 2 ℃/min to obtain alloy liquid b;
3) Mixing the alloy liquid a and the alloy liquid b, heating the alloy liquid a and the alloy liquid b to 2100 ℃, preserving heat for 50min, cooling the alloy liquid a and the alloy liquid b to 1200 ℃ at the speed of 1 ℃/min, preserving heat for 60min, heating the alloy liquid a to 1500 ℃ at the speed of 1 ℃/min, and preserving heat for 30min to obtain a metal liquid c;
4) And (3) preparing the prepared metal liquid c into alloy powder by an atomization method, wherein the prepared alloy powder can pass through a 800-mesh sieve to obtain the alloy powder.
The preparation method of the plasticizer comprises the following steps:
1) Placing 12 parts of vinyl alcohol into a reactor, adding 4 parts of 1, 3-butadiene into the reactor, adding concentrated sulfuric acid into the reactor, heating to 90 ℃ at the speed of 4 ℃/min, and carrying out heat preservation reaction for 6 hours to obtain a product i;
2) Adding 5 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 3 ℃/min, and carrying out heat preservation reaction for 3 hours to obtain a product ii;
3) Adding 4 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 6 ℃/min, and carrying out heat preservation reaction for 4 hours to obtain a product iii;
4) Taking 5 parts of a product iii), adding 10 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 8 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 7h to obtain a product iv;
5) 15 parts of liquid paraffin, adding iv 2 parts of a product, heating to 60 ℃ at a speed of 3 ℃/min, stirring while heating, and reacting for 4 hours after uniformly stirring.
The preparation method of the quenching medium comprises the following steps:
a. 10 parts of ethylene propylene diene monomer is put into a reactor, 7 parts of 4, 4-dimethoxy-2-butanone is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 130 ℃, and the reaction is carried out for 3 hours under the heat preservation, thus obtaining a reactant a;
b. adding 5 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 1 ℃/min, and carrying out heat preservation reaction for 4 hours to obtain a reactant b;
c. Putting 5 parts of thiazolidinethione into a reactor, adding 10 parts of alkylphenol ethoxylates into the reactor, adding a dichloromethane solution into the reactor, heating to 100 ℃ at a speed of 3 ℃/min, and carrying out heat preservation reaction for 4 hours to obtain a reactant c;
d. putting 6 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 3 ℃/min, dropwise adding 8 parts of a reactant c into the reactor at a speed of 15 drops/min, heating to 90 ℃, and reacting for 4 hours at a temperature of keeping the temperature to obtain a reactant d;
e. and adding 5 parts of sodium thiosulfopropane sulfonate into the reactant d, adding an ethyl acetate solution, heating to 95 ℃ at a speed of 6 ℃/min, and carrying out heat preservation reaction for 6 hours to obtain the catalyst.
The organic soaking oil is as follows: 35 parts of mechanical oil, 2 parts of tert-butyl hydroquinone, 3 parts of triethanolamine sodium hydrochloride and 6 parts of 1, 3-dihydroxyurea, and uniformly mixing the components to obtain the finished product.
Example 3
A wear-resistant and corrosion-resistant cemented carbide milling cutter, wherein the milling cutter comprises the following raw materials: 35 parts of modified alloy powder, 0.5 part of tungsten carbide powder, 1 part of titanium carbide powder, 0.1 part of cobalt powder and 0.2 part of plasticizer.
The preparation method of the milling cutter comprises the following steps:
1) Putting 35 parts of prepared modified alloy powder, 0.5 part of tungsten carbide powder, 1 part of titanium carbide powder and 0.1 part of cobalt powder into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 10 ℃/min, preserving heat and sintering for 25min, heating to 1450 ℃ at the speed of 8 ℃/min, preserving heat and sintering for 15min, cooling to 1000 ℃ at the cooling speed of 4 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1 ℃/min;
4) And (3) carrying out surface quenching treatment on the sintered milling cutter, heating the surface of the milling cutter to 1350 ℃, immediately placing the milling cutter into a quenching medium for quenching, carrying out polishing treatment on the quenched milling cutter, and placing the polished milling cutter into organic soaking oil for oil immersion for 5 hours to obtain the finished product.
The preparation method of the modified alloy powder comprises the following steps:
1) Adding 3 parts of iron into 15 parts of No. 45 steel, putting the steel into a high-temperature furnace, heating to 1800 ℃, adding 0.1 part of nickel and 0.2 part of silicon carbide into the steel, heating to 1950 ℃ until uniform alloy liquid is formed, and preserving heat to obtain alloy liquid a for later use;
2) Placing 0.5 part of beryllium oxide and 0.2 part of titanium oxide into a high-temperature furnace, heating to 2390 ℃, preserving heat for 4 hours, adding 0.5 part of chromium and 0.4 part of copper again, heating to 2500 ℃ together, preserving heat for 15-30 minutes, and cooling to 1700 ℃ at a speed of 3 ℃/min to obtain alloy liquid b;
3) Mixing the alloy liquid a and the alloy liquid b, heating the alloy liquid a and the alloy liquid b to 2100 ℃, preserving heat for 30min, cooling the alloy liquid a and the alloy liquid b to 1200 ℃ at the speed of 3 ℃/min, preserving heat for 40min, heating the alloy liquid a to 1500 ℃ at the speed of 3 ℃/min, and preserving heat for 20-30min to obtain a metal liquid c;
4) And (3) preparing the prepared metal liquid c into alloy powder by an atomization method, wherein the prepared alloy powder can pass through a 800-mesh sieve to obtain the alloy powder.
The preparation method of the plasticizer comprises the following steps:
1) 8 parts of vinyl alcohol is put into a reactor, 6 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 95 ℃ at the speed of 2 ℃/min, and the reaction is carried out for 4 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 7 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 1 ℃/min, and carrying out heat preservation reaction for 4 hours to obtain a product ii;
3) Adding 3 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 9 ℃/min, and carrying out heat preservation reaction for 3 hours to obtain a product iii;
4) Taking 8 parts of a product iii), adding 8 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 10 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 5 hours to obtain a product iv;
5) Taking 20 parts of liquid paraffin, adding 1 part of product iv, heating to 60 ℃ at a speed of 5 ℃/min, stirring while heating, and reacting for 3 hours after uniformly stirring.
The preparation method of the quenching medium comprises the following steps:
a. 13 parts of ethylene propylene diene monomer is put into a reactor, 5 parts of 4, 4-dimethoxy-2-butanone is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 130 ℃, and the reaction is carried out for 4 hours under the condition of heat preservation, thus obtaining a reactant a;
b. adding 3 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 3 ℃/min, and carrying out heat preservation reaction for 3 hours to obtain a reactant b;
c. putting 8 parts of thiazolidinethione into a reactor, adding 6 parts of alkylphenol ethoxylates into the reactor, adding a dichloromethane solution into the reactor, heating to 100 ℃ at a speed of 5 ℃/min, and carrying out heat preservation reaction for 3 hours to obtain a reactant c;
d. putting 9 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 1 ℃/min, dropwise adding 5 parts of a reactant c into the reactor at a speed of 20 drops/min, heating to 95 ℃, and reacting for 3 hours at a temperature of 3 hours to obtain a reactant d;
e. And adding 8 parts of sodium thiosulfopropane sulfonate into the reactant d, adding an ethyl acetate solution, heating to 100 ℃ at a speed of 4 ℃/min, and carrying out heat preservation reaction for 5 hours to obtain the catalyst.
The organic soaking oil is as follows: 40 parts of mechanical oil, 1 part of tert-butyl hydroquinone, 5 parts of triethanolamine sodium hydrochloride and 2 parts of 1, 3-dihydroxyurea, and uniformly mixing the components to obtain the finished product.
Comparative example 1
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the milling cutter comprises the following raw materials: 20 parts of modified alloy powder, 0.5 part of tungsten carbide powder, 1 part of titanium carbide powder, 0.1 part of cobalt powder and 0.2 part of plasticizer.
The procedure is as in example 1.
Comparative example 2
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the milling cutter comprises the following raw materials: 35 parts of modified alloy powder, 1.2 parts of tungsten carbide powder, 1 part of titanium carbide powder, 0.1 part of cobalt powder and 0.2 part of plasticizer.
The procedure is as in example 1.
Comparative example 3
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the milling cutter comprises the following raw materials: 35 parts of modified alloy powder, 0.5 part of tungsten carbide powder, 0.3 part of titanium carbide powder, 0.1 part of cobalt powder and 0.2 part of plasticizer.
The procedure is as in example 1.
Comparative example 4
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the milling cutter comprises the following raw materials: 35 parts of modified alloy powder, 0.5 part of tungsten carbide powder, 1 part of titanium carbide powder, 0.08 part of cobalt powder and 0.2 part of plasticizer.
The procedure is as in example 1.
Comparative example 5
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the milling cutter comprises the following raw materials: 35 parts of modified alloy powder, 0.5 part of tungsten carbide powder, 1 part of titanium carbide powder, 0.1 part of cobalt powder and 0.22 part of plasticizer.
The procedure is as in example 1.
Comparative example 6
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The step 3) in the preparation method of the milling cutter is as follows:
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 15 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.3 ℃/min;
the procedure is as in example 1.
Comparative example 7
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The step 3) in the preparation method of the milling cutter is as follows:
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 650 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.3 ℃/min;
The procedure is as in example 1.
Comparative example 8
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The step 3) in the preparation method of the milling cutter is as follows:
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 10 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.3 ℃/min;
the procedure is as in example 1.
Comparative example 9
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The step 3) in the preparation method of the milling cutter is as follows:
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 2.5h, and cooling to room temperature at the speed of 1.3 ℃/min;
The procedure is as in example 1.
Comparative example 10
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The step 3) in the preparation method of the milling cutter is as follows:
3) Placing the particles prepared in the steps into isostatic pressing equipment for molding, placing a molded rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, heating to 700 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, stopping heating the high-temperature furnace, and cooling the milling cutter to room temperature along with the furnace;
the procedure is as in example 1.
Comparative example 11
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The step 3) in the preparation method of the milling cutter is as follows:
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, heating to 1450 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 3 hours, and cooling to room temperature at the speed of 1.3 ℃/min;
The procedure is as in example 1.
Comparative example 12
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the milling cutter comprises the following steps:
1) The preparation method comprises the following steps: 30 parts of modified alloy powder, 0.8 part of tungsten carbide powder, 0.8 part of titanium carbide powder and 0.15 part of cobalt powder are put into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.3 ℃/min;
4) Polishing the sintered milling cutter, and putting the polished milling cutter into organic immersion oil for immersion for 5 hours to obtain the oil-immersed milling cutter.
The procedure is as in example 1.
Comparative example 13
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the milling cutter comprises the following steps:
1) The preparation method comprises the following steps: 30 parts of modified alloy powder, 0.8 part of tungsten carbide powder, 0.8 part of titanium carbide powder and 0.15 part of cobalt powder are put into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.3 ℃/min;
4) Quenching the sintered milling cutter, heating the whole milling cutter to 1350 ℃, immediately placing the milling cutter into a quenching medium for quenching, polishing the quenched milling cutter, and placing the polished milling cutter into organic immersion oil for immersion for 5 hours to obtain the finished product.
The procedure is as in example 1.
Comparative example 14
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The step 4) in the preparation method of the milling cutter is as follows:
4) And (3) carrying out surface quenching treatment on the sintered milling cutter, heating the surface of the milling cutter to 1350 ℃, immediately placing the milling cutter into a quenching medium for quenching, and polishing the quenched milling cutter.
The procedure is as in example 1.
Comparative example 15
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the modified alloy powder comprises the following steps of:
1) Adding 3.5 parts of iron into 14 parts of No. 45 steel, putting the steel into a high-temperature furnace, adding 0.08 part of nickel and 0.3 part of silicon carbide into the steel, heating to 1950 ℃ until uniform alloy liquid is formed, and preserving heat to obtain alloy liquid a for later use;
the procedure is as in example 1.
Comparative example 16
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the modified alloy powder comprises the following step 1):
1) Adding 3.5 parts of iron into 14 parts of No. 45 steel, putting the steel into a high-temperature furnace, heating to 1800 ℃, adding 0.12 part of nickel and 0.3 part of silicon carbide into the steel, heating to 1950 ℃ until uniform alloy liquid is formed, and preserving heat to obtain alloy liquid a for later use;
The procedure is as in example 1.
Comparative example 17
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the modified alloy powder comprises the following step 2):
2) Placing 0.53 part of beryllium oxide and 0.25 part of titanium oxide into a high-temperature furnace, heating to 2390 ℃, preserving heat for 3.5 hours, adding 0.6 part of chromium and 0.3 part of copper again, heating to 2500 ℃ together, preserving heat for 22 minutes, and cooling to 1700 ℃ at a speed of 2.5 ℃/min to obtain alloy liquid b;
the procedure is as in example 1.
Comparative example 18
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the modified alloy powder comprises the following step 2):
2) Placing 0.45 part of beryllium oxide and 0.25 part of titanium oxide into a high-temperature furnace, heating to 2390 ℃, preserving heat for 3.5 hours, adding 0.6 part of chromium and 0.3 part of copper again, heating to 2500 ℃ together, preserving heat for 22 minutes, and cooling to 1700 ℃ at a speed of 5 ℃/min to obtain alloy liquid b;
the procedure is as in example 1.
Comparative example 19
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the modified alloy powder comprises the following step 3):
3) Mixing the alloy liquid a and the alloy liquid b, heating the alloy liquid a and the alloy liquid b to 2100 ℃, preserving heat for 40min, cooling the alloy liquid a and the alloy liquid b to 1200 ℃ at a speed of 5 ℃/min, preserving heat for 50min, heating the alloy liquid a and the alloy liquid b to 1500 ℃ at a speed of 2 ℃/min, and preserving heat for 25min to obtain a metal liquid c;
The procedure is as in example 1.
Comparative example 20
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the modified alloy powder comprises the following step 3):
3) Mixing the alloy liquid a and the alloy liquid b, heating the mixture to 2100 ℃, preserving heat for 40min, cooling the mixture to 1500 ℃ at a speed of 2 ℃/min, and preserving heat for 1.5h to obtain a metal liquid c;
the procedure is as in example 1.
Comparative example 21
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The alloy powder is prepared by uniformly mixing 14 parts of common No. 45 steel powder, 3.5 parts of iron powder, 0.05-0.1 part of nickel powder, 0.2-0.4 part of silicon carbide powder, 0.4-0.5 part of beryllium oxide powder, 0.2-0.3 part of titanium oxide powder, 0.5-0.8 part of chromium powder and 0.2-0.4 part of copper powder.
The preparation method of the milling cutter comprises the following steps:
1) 30 parts of prepared alloy powder, 0.8 part of tungsten carbide powder, 0.8 part of titanium carbide powder and 0.15 part of cobalt powder are put into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 11 ℃/min, preserving heat and sintering for 28min, heating to 1450 ℃ at the speed of 7 ℃/min, preserving heat and sintering for 18min, cooling to 1000 ℃ at the cooling speed of 3 ℃/min, preserving heat and sintering for 2h, and cooling to room temperature at the speed of 1.3 ℃/min;
4) And (3) carrying out surface quenching treatment on the sintered milling cutter, heating the surface of the milling cutter to 1350 ℃, immediately placing the milling cutter into a quenching medium for quenching, carrying out polishing treatment on the quenched milling cutter, and placing the polished milling cutter into organic soaking oil for oil immersion for 5 hours to obtain the finished product.
The procedure is as in example 1.
Comparative example 22
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) Placing 14 parts of vinyl alcohol into a reactor, adding 5 parts of 1, 3-butadiene into the reactor, adding concentrated sulfuric acid into the reactor, heating to 93 ℃ at the speed of 3 ℃/min, and carrying out heat preservation reaction for 5 hours to obtain a product i;
2) Adding 6 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking out the product iii 7 parts, adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The procedure is as in example 1.
Comparative example 23
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 93 ℃ at the speed of 6 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 6 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking out the product iii 7 parts, adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The procedure is as in example 1.
Comparative example 24
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 93 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 9 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking out the product iii 7 parts, adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The procedure is as in example 1.
Comparative example 25
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 93 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 6 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 90 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking out the product iii 7 parts, adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The procedure is as in example 1.
Comparative example 26
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene and 6 parts of butynedioic acid are added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 100 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining the product;
2) Adding 3.5 parts of 4-isopropylbenzoic acid into the product i, adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain the product ii;
3) Taking 7 parts of a product ii), adding 9 parts of decaglycerol decastearate, and adding ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iii;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of a product iii, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, uniformly stirring, and then carrying out heat preservation reaction for 3.5 hours to obtain the product iii.
The procedure is as in example 1.
Comparative example 27
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 93 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 6 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 120 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking out the product iii 7 parts, adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The procedure is as in example 1.
Comparative example 28
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 93 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 6 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking 10 parts of a product iii), adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 18 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at a speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The procedure is as in example 1.
Comparative example 29
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the plasticizer comprises the following steps:
1) 10 parts of vinyl alcohol is put into a reactor, 5 parts of 1, 3-butadiene is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 93 ℃ at the speed of 3 ℃/min, and the reaction is carried out for 5 hours under the condition of heat preservation, thus obtaining a product i;
2) Adding 6 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a product ii;
3) Adding 3.5 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 8 ℃/min, and carrying out heat preservation reaction for 3.4 hours to obtain a product iii;
4) Taking out the product iii 7 parts, adding 9 parts of decaglycerol decastearate, and putting into ethanol: heating the mixed solution with the volume ratio of 1, 2-dichloroethane to be 4:3 to 120 ℃ at the speed of 9 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 6 hours to obtain a product iv;
5) Taking 13 parts of liquid paraffin, adding 1.5 parts of product iv, heating to 60 ℃ at the speed of 4 ℃/min, stirring while heating, and reacting for 3.5 hours after uniformly stirring.
The procedure is as in example 1.
Comparative example 30
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the plasticizer is paraffin wax.
The procedure is as in example 1.
Comparative example 31
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the quenching medium comprises the following steps:
a. 15 parts of ethylene propylene diene monomer is put into a reactor, 6 parts of 4, 4-dimethoxy-2-butanone is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 130 ℃, and the reaction is carried out for 3.5 hours under the heat preservation, thus obtaining a reactant a;
b. adding 4 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant b;
c. 7 parts of thiazolidinethione is put into a reactor, 8 parts of alkylphenol ethoxylates are added into the reactor, a methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 4 ℃/min, and the reaction is carried out for 3.5 hours under the condition of heat preservation, thus obtaining a reactant c;
d. Putting 8 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 2 ℃/min, dropwise adding 7 parts of a reactant c into the reactor at a speed of 18 drops/min, heating to 93 ℃, and reacting for 3.5 hours at a temperature of 3.5 hours to obtain a reactant d;
e. and 7 parts of sodium thiosulfopropane sulfonate is added into the reactant d, an ethyl acetate solution is added, the temperature is raised to 98 ℃ at the speed of 5 ℃/min, and the reaction is carried out for 5.5 hours.
The procedure is as in example 1.
Comparative example 32
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the quenching medium comprises the following steps:
a. placing 12 parts of ethylene propylene diene monomer into a reactor, adding 6 parts of 4, 4-dimethoxy-2-butanone into the reactor, adding concentrated sulfuric acid into the reactor, heating the mixture to 100 ℃, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant a;
b. adding 4 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant b;
c. 7 parts of thiazolidinethione is put into a reactor, 8 parts of alkylphenol ethoxylates are added into the reactor, a methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 4 ℃/min, and the reaction is carried out for 3.5 hours under the condition of heat preservation, thus obtaining a reactant c;
d. Putting 8 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 2 ℃/min, dropwise adding 7 parts of a reactant c into the reactor at a speed of 18 drops/min, heating to 93 ℃, and reacting for 3.5 hours at a temperature of 3.5 hours to obtain a reactant d;
e. and 7 parts of sodium thiosulfopropane sulfonate is added into the reactant d, an ethyl acetate solution is added, the temperature is raised to 98 ℃ at the speed of 5 ℃/min, and the reaction is carried out for 5.5 hours.
The procedure is as in example 1.
Comparative example 33
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the quenching medium comprises the following steps:
a. placing 12 parts of ethylene propylene diene monomer into a reactor, adding 6 parts of 4, 4-dimethoxy-2-butanone, 4 parts of butyl hydroxy anisole and concentrated sulfuric acid into the reactor, heating to 130 ℃, and reacting for 3.5 hours at a constant temperature to obtain a reactant a;
b. 7 parts of thiazolidinethione is put into a reactor, 8 parts of alkylphenol ethoxylates are added into the reactor, a methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 4 ℃/min, and the reaction is carried out for 3.5 hours under the condition of heat preservation, thus obtaining a reactant b;
c. putting 8 parts of a reactant a into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 2 ℃/min, dropwise adding 7 parts of a reactant b into the reactor at a speed of 18 drops/min, heating to 93 ℃, and reacting for 3.5h at a temperature of 3.5h to obtain a reactant c;
d. And 7 parts of sodium thiosulfopropane sulfonate is added into the reactant c, an ethyl acetate solution is added, the temperature is raised to 98 ℃ at the speed of 5 ℃/min, and the reaction is carried out for 5.5 hours.
The procedure is as in example 1.
Comparative example 34
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the quenching medium comprises the following steps:
a. placing 12 parts of ethylene propylene diene monomer into a reactor, adding 6 parts of 4, 4-dimethoxy-2-butanone into the reactor, adding concentrated sulfuric acid into the reactor, heating the mixture to 130 ℃, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant a;
b. adding 4 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant b;
c. 10 parts of thiazolidinethione is put into a reactor, 8 parts of alkylphenol ethoxylates are added into the reactor, a methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 4 ℃/min, and the reaction is carried out for 3.5 hours under the condition of heat preservation, thus obtaining a reactant c;
d. putting 8 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 2 ℃/min, dropwise adding 7 parts of a reactant c into the reactor at a speed of 18 drops/min, heating to 93 ℃, and reacting for 3.5 hours at a temperature of 3.5 hours to obtain a reactant d;
e. And 7 parts of sodium thiosulfopropane sulfonate is added into the reactant d, an ethyl acetate solution is added, the temperature is raised to 98 ℃ at the speed of 5 ℃/min, and the reaction is carried out for 5.5 hours.
The procedure is as in example 1.
Comparative example 35
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the quenching medium comprises the following steps:
a. placing 12 parts of ethylene propylene diene monomer into a reactor, adding 6 parts of 4, 4-dimethoxy-2-butanone into the reactor, adding concentrated sulfuric acid into the reactor, heating the mixture to 130 ℃, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant a;
b. adding 4 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant b;
c. 7 parts of thiazolidinethione is put into a reactor, 8 parts of alkylphenol ethoxylates are added into the reactor, a methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 6 ℃/min, and the reaction is carried out for 3.5 hours under the condition of heat preservation, thus obtaining a reactant c;
d. putting 8 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 2 ℃/min, dropwise adding 7 parts of a reactant c into the reactor at a speed of 18 drops/min, heating to 93 ℃, and reacting for 3.5 hours at a temperature of 3.5 hours to obtain a reactant d;
e. And 7 parts of sodium thiosulfopropane sulfonate is added into the reactant d, an ethyl acetate solution is added, the temperature is raised to 98 ℃ at the speed of 5 ℃/min, and the reaction is carried out for 5.5 hours.
The procedure is as in example 1.
Comparative example 36
A wear-resistant and corrosion-resistant hard alloy milling cutter.
The preparation method of the quenching medium comprises the following steps:
a. placing 12 parts of ethylene propylene diene monomer into a reactor, adding 6 parts of 4, 4-dimethoxy-2-butanone into the reactor, adding concentrated sulfuric acid into the reactor, heating the mixture to 130 ℃, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant a;
b. adding 4 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 2 ℃/min, and carrying out heat preservation reaction for 3.5 hours to obtain a reactant b;
c. 7 parts of thiazolidinethione is put into a reactor, 8 parts of alkylphenol ethoxylates are added into the reactor, a methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 4 ℃/min, and the reaction is carried out for 3.5 hours under the condition of heat preservation, thus obtaining a reactant c;
d. putting 8 parts of a reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 2 ℃/min, dropwise adding 7 parts of a reactant c into the reactor at a speed of 18 drops/min, heating to 93 ℃, and reacting for 3.5 hours at a temperature of 3.5 hours to obtain a reactant d;
e. 10 parts of sodium thiosulfopropane sulfonate is added into the reactant d, an ethyl acetate solution is added, the temperature is raised to 98 ℃ at the speed of 5 ℃/min, and the reaction is carried out for 5.5 hours.
The procedure is as in example 1.
Comparative example 37
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the quenching medium is Hengxin THIF-511 quick bright quenching oil.
The procedure is as in example 1.
Comparative example 38
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the organic immersion oil is: 38 parts of mechanical oil, 1.5 parts of tert-butyl hydroquinone, 7 parts of triethanolamine sodium hydrochloride and 4 parts of 1, 3-dihydroxyurea, and uniformly mixing the components to obtain the finished product.
The procedure is as in example 1.
Comparative example 39
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein the organic immersion oil is: 38 parts of mechanical oil, 2.2 parts of tert-butyl hydroquinone, 4 parts of triethanolamine sodium hydrochloride and 4 parts of 1, 3-dihydroxyurea, and uniformly mixing the components to obtain the finished product.
The procedure is as in example 1.
Comparative example 40
A wear-resistant and corrosion-resistant hard alloy milling cutter.
Wherein, the mechanical soaking oil is common rust-proof oil, and the model is R5001.
The procedure is as in example 1.
Comparative example 41
A common hard alloy face milling cutter.
Experimental example 1 wear resistance of cemented carbide milling cutter
The milling cutters prepared in the examples and the comparative examples are subjected to wear resistance test, the original weight of the milling cutter is firstly tested and recorded, and after the record is made, the milling cutter is used according to the test method specified in the national standard GB/T16459-2016 face milling cutter life test.
Wherein the working cutting conditions of the face milling cutter were tested according to the cutting conditions iii specified in the standard, wherein the back draft was 2.5mm, the feed per tooth was 0.315/(mm/tooth), the cutting speed was 180m/min, and after the milling cutter continuously cut for 28 days (same work load), the wear condition of the milling cutter was observed, and the evaluation results were recorded in table 2 in comparison with the cutting wear standards of the milling cutter of table 1.
Table 1 wear evaluation criteria for milling cutter
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Table 2 wear resistance test of milling cutter
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As can be seen from Table 1, examples 1-3 all had wear resistance evaluations of I, which were much higher than comparative example 41; comparative examples 1 to 5 change the ratio of raw materials for preparing a milling cutter, resulting in that elements in the milling cutter cannot be effectively dissolved and dispersed, so that the abrasion resistance of the milling cutter is reduced; comparative examples 6 to 14 are examples in which the manufacturing process of the milling cutter is changed, and the heat treatment process in the manufacturing process of the milling cutter is changed, so that pores still exist in the milling cutter in the sintering process, and the wear resistance of the milling cutter is reduced; comparative examples 15 to 20 were modified with respect to the preparation process of the modified alloy powder, resulting in a decrease in hardness of the modified alloy powder and dispersion of atoms therein, so that the prepared milling cutter was evaluated as ii or iii in wear resistance; comparative examples 22 to 29 were modified in terms of the preparation process of the plasticizer, resulting in a change in the composition or post-conditioning of the plasticizer, and the plasticizing binding ability was weakened, so that the alloy powder binding ability of the milling cutter was deteriorated, and the wear resistance of the prepared milling cutter was lowered; the low ratio 31-39 changes with respect to the surface quenching medium and rust preventive oil of the milling cutter, resulting in a lower surface quenching effect of the milling cutter, and a lower surface hardening effect of the milling cutter, so that the wear resistance of the milling cutter becomes lower. The common hard alloy powder is adopted for mixing in the comparative example 21, the common plasticizer is adopted in the comparative example 30, the common quenching oil is adopted as the quenching medium in the comparative example 37, the common rust-preventive oil is adopted in the comparative example 40 to soak the metal parts for rust prevention, but the unmodified reagents cannot be effectively matched in the invention, even the cohesiveness among the metal parts is reduced, the effective sintering time cannot be achieved, even the hardness of the milling cutter cannot be enhanced by surface quenching, even the brittleness of the milling cutter is enhanced, so the evaluation effect of the abrasion resistance experiment is only V.
Experimental example 2 hardness of milling cutter
The milling cutters prepared in the examples and the comparative examples are used in accordance with the national standard GB/T5342.3-2016 indexable face milling cutter part 3: technical conditions, hardness test, specific test results are recorded in table 3;
table 3 hardness of milling cutter
Figure 467325DEST_PATH_IMAGE003
As can be seen from Table 3, the hardness of the milling cutters prepared in examples 1-3 far exceeded that of the conventional milling cutter of comparative example 41. Comparative examples 1 to 5 change the ratio of alloy powder for preparing a milling cutter, resulting in excessive or insufficient solid solution atoms of the milling cutter, and thus reduced hardness of the milling cutter; comparative examples 6, 8 and 10 change the temperature rising speed or the temperature reducing speed of the milling cutter in the sintering process, so that the metal powder in the milling cutter cannot be effectively bonded in the flowing and melting process, and the highest hardness HRC of the milling cutter is only 51; comparative examples 7 and 9, in which the sintering heat preservation temperature was changed during the preparation of the milling cutter, resulted in hardness HRC of only 49 and 50 for the prepared milling cutter; comparative example 11, comparative examples 12-14 the sintering preparation process and the quenching process of the milling cutter were changed, resulting in lower hardness of the milling cutter than examples 1-3. Comparative example 15, comparative examples 18 to 20, the preparation process of the modified cemented carbide powder resulted in uneven distribution of elements in the alloy powder, so that the hardness of the prepared milling cutter was lowered; comparative examples 16 to 17 the hardness HRC of the milling cutter was only 46, 48, since the proportions of the raw materials of the modified alloy powder were changed. Comparative example 21 only mechanically mixes the cemented carbide powder, resulting in a segregation phenomenon of the milling cutter during the powder metallurgy sintering, so the hardness of the milling cutter is even lower than that of comparative example 41; in the comparative example 30, paraffin wax is selected as a plasticizer, and only alloy powder is subjected to simple bonding plasticization, but the hardness of the milling cutter cannot be effectively ensured in the sintering process due to the existence of modified alloy powder and a quenching medium, so that the hardness HRC of the milling cutter is only 34; comparative example 37 used a conventional quench medium and comparative example 40 used a conventional rust preventive oil, which resulted in a reduction in hardness of the milling cutter, which was lower than examples 1-3.
Experimental example 3 Corrosion resistance of cemented carbide milling cutter
Placing the milling cutters prepared in the examples and the comparative examples into a high-temperature environment at 450 ℃ to work, externally simulating the chip spraying condition, spraying the surface of the milling cutter for 14 days, placing the milling cutter into the environment with the humidity of 60% and the temperature of 65 ℃ to stand for 10 days after the test is finished, and observing whether the surface of the milling cutter rusts or not after 10 days; if the rust condition exists, the corrosion percentage is measured and calculated, and the specific calculation method is as follows:
corrosion = corrosion area x 100%/surface area of milling cutter
Record specific data in table 4;
table 4 test of milling cutter at 350 c
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The milling cutter is sprayed at high temperature and placed in a high-humidity and high-temperature environment in the test, so that conditions are created for corrosion of the alloy. As can be seen from Table 4, the milling cutters prepared in examples 1 to 3 all showed corrosion, whereas comparative example 41 showed a corrosion area of 4.88%, and it was found that the milling cutters prepared in accordance with the present invention had excellent corrosion resistance. The milling cutter of comparative example 12 was not subjected to surface quenching, the milling cutter of comparative example 14 was not subjected to an organic oil soaking process, and the milling cutter of comparative example 21 was prepared using a common alloy powder, and these changes all resulted in a decrease in the corrosion resistance of the milling cutter. Comparative examples 22 to 29 were modified with respect to the preparation process of the plasticizer, wherein the formulation ratio of the plasticizer was modified in comparative example 22, comparative example 24, and comparative examples 28 to 29, resulting in a change in the composition of the plasticizer and a decrease in the corrosion resistance of the milling cutter, so that the corrosion area of the milling cutter was between 3.22% and 3.64%; comparative example 23 and comparative examples 25 to 27 change the process in the preparation process of the plasticizer, resulting in a change in the molecular structure of the plasticizer, the cohesive plasticizing effect of the plasticizer is greatly dying, and the corrosion resistance of the prepared milling cutter is reduced. In comparative example 30, paraffin wax was used as a plasticizer, and although the molding effect of paraffin wax was good, the adhesion property was lowered in the presence of the modified alloy powder, so that the corrosion percentage of the prepared milling cutter was as high as 5.04%. Comparative examples 31 to 39 were modified for the preparation process of the surface quenching medium and the organic immersion oil of the milling cutter, wherein the comparative examples 31, 34 and 36 changed the raw materials of the surface quenching medium, resulting in the change of the effective components of the surface quenching medium, so that the surface quenching effect of the milling cutter was deteriorated, and the corrosion resistance of the milling cutter was lowered; comparative examples 32 to 33, comparative example 35 changed the preparation process of the surface quenching medium, resulting in a change in the structure of groups in the active ingredients of the surface quenching medium, so that the corrosion resistance of the quenched milling cutter was lowered; comparative examples 38 to 39 change the proportion of the organic immersion oil, resulting in a reduction in the rust preventive effect of the organic immersion oil and a reduction in the corrosion resistance of the metal, so that corrosion occurs on the surface of the milling cutter. The comparative examples 37 and 40 were each prepared by using a common quenching medium and rust preventive oil, but were not suitable for the milling cutter prepared in the present invention, and the effective components therein even accelerated the corrosion of the milling cutter, even the corrosion area was larger than that of the common milling cutter of comparative example 41.

Claims (3)

1. A wear-resistant and corrosion-resistant hard alloy milling cutter comprises the following raw materials: 25-35 parts of modified alloy powder, 0.5-1 part of tungsten carbide powder, 0.5-1 part of titanium carbide powder, 0.1-0.2 part of cobalt powder and 0.1-0.2 part of plasticizer, and is characterized in that: the preparation method of the modified alloy powder comprises the following steps:
1) Adding 3-4 parts of iron into 12-15 parts of No. 45 steel, putting the steel into a high-temperature furnace, heating to 1800 ℃, adding 0.05-0.1 part of nickel and 0.2-0.4 part of silicon carbide into the steel, heating to 1950 ℃ until uniform alloy liquid is formed, and preserving heat to obtain alloy liquid a for later use;
2) Placing 0.4-0.5 part of beryllium oxide and 0.2-0.3 part of titanium oxide into a high-temperature furnace, heating to 2390 ℃, preserving heat for 3-4 hours, adding 0.5-0.8 part of chromium and 0.2-0.4 part of copper again, heating to 2500 ℃ together, preserving heat for 15-30 minutes, and cooling to 1700 ℃ at a speed of 2-3 ℃/min to obtain alloy liquid b;
3) Mixing the alloy liquid a and the alloy liquid b, heating the alloy liquid a and the alloy liquid b to 2100 ℃, preserving heat for 30-50min, cooling the alloy liquid a to 1200 ℃ at the speed of 1-3 ℃/min, preserving heat for 40-60min, heating the alloy liquid a to 1500 ℃ at the speed of 1-3 ℃/min, and standing and preserving heat for 20-30min to obtain a metal liquid c;
4) Preparing the prepared metal liquid c into alloy powder by an atomization method, wherein the prepared alloy powder can pass through a 800-mesh sieve to obtain the alloy powder;
The preparation method of the plasticizer comprises the following steps:
1) Placing 8-12 parts of vinyl alcohol into a reactor, adding 4-6 parts of 1, 3-butadiene into the reactor, adding concentrated sulfuric acid into the reactor, heating to 90-95 ℃ at the speed of 2-4 ℃/min, and carrying out heat preservation reaction for 4-6 hours to obtain a product i;
2) Adding 5-7 parts of butynedioic acid into the product i, adding an diethyl ether solution, placing the mixture into a reactor, heating to 100 ℃ at a speed of 1-3 ℃/min, and carrying out heat preservation reaction for 3-4 hours to obtain a product ii;
3) Adding 3-4 parts of 4-isopropylbenzoic acid into the product ii), adding an ethyl acetate solution, heating to 130 ℃ at the speed of 6-9 ℃/min, and carrying out heat preservation reaction for 3-4 hours to obtain a product iii;
4) Taking 5-8 parts of a product iii), adding 8-10 parts of decaglycerol decastearate, and adding ethanol: 1, heating the mixed solution with the volume ratio of 2-dichloroethane of 4:3 to 120 ℃ at the speed of 8-10 ℃/min, introducing nitrogen in the heating process, and carrying out heat preservation reaction for 5-7h to obtain a product iv;
5) 15-20 parts of liquid paraffin, adding 1-2 parts of product iv, heating to 60 ℃ at the speed of 3-5 ℃/min, stirring while heating, and reacting for 3-4 hours after uniformly stirring.
2. The method for preparing the wear-resistant and corrosion-resistant hard alloy milling cutter as claimed in claim 1, wherein the method comprises the following steps: the preparation method of the milling cutter comprises the following steps:
1) Putting 25-35 parts of prepared modified alloy powder, 0.5-1 part of tungsten carbide powder, 0.5-1 part of titanium carbide powder and 0.1-0.2 part of cobalt powder into a ball milling tank for ball milling until the mixture is uniform;
2) Putting the ball-milled mixed powder into granulation, adding a plasticizer for granulation, and repeatedly sieving the granules through a 600-mesh screen for 3 times;
3) Placing the particles prepared in the steps into a cold isostatic press for molding, wherein the molding temperature is 30 ℃ and the molding pressure is 450MPa; placing the formed rough milling cutter into a high-temperature furnace for sintering, introducing nitrogen into the high-temperature furnace for protection in the sintering process, firstly heating to 700 ℃ at the speed of 10-12 ℃/min, keeping the temperature for sintering for 25-30min, heating to 1450 ℃ at the speed of 5-8 ℃/min, keeping the temperature for sintering for 15-20min, cooling to 1000 ℃ at the cooling speed of 2-4 ℃/min, keeping the temperature for sintering for 2h, and cooling to room temperature at the speed of 1-1.5 ℃/min;
4) Carrying out surface quenching treatment on the sintered milling cutter, immediately placing the surface of the milling cutter into a quenching medium for quenching after the surface of the milling cutter is heated to 1350 ℃, carrying out polishing treatment on the quenched milling cutter, and placing the polished milling cutter into organic soaking oil for oil immersion for 5 hours to obtain the ceramic cutting tool;
The preparation method of the quenching medium comprises the following steps:
1) 10-13 parts of ethylene propylene diene monomer is put into a reactor, 5-7 parts of 4, 4-dimethoxy-2-butanone is added into the reactor, concentrated sulfuric acid is added into the reactor, the temperature is raised to 130 ℃, and the reaction is carried out for 3-4 hours under the condition of heat preservation, thus obtaining a reactant a;
2) Adding 3-5 parts of butyl hydroxy anisole into the reactant a, adding a propanol solution, heating to 110 ℃ at a speed of 1-3 ℃/min, and carrying out heat preservation reaction for 3-4 hours to obtain a reactant b;
3) 5-8 parts of thiazolidinethione is put into a reactor, 6-10 parts of alkylphenol ethoxylates are added into the reactor, methylene dichloride solution is added into the reactor, the temperature is raised to 100 ℃ at the speed of 3-5 ℃/min, and the reaction is carried out for 3-4 hours under heat preservation, thus obtaining a reactant c;
4) Putting 6-9 parts of reactant b into a reactor, adding a dichlorotoluene solution into the reactor, heating to 40 ℃ at a speed of 1-3 ℃/min, dripping 5-8 parts of reactant c into the reactor at a speed of 15-20 drops/min, heating to 90-95 ℃, and reacting for 3-4 hours at a temperature maintaining to obtain a reactant d;
5) Adding 5-8 parts of sodium thiodipropyl sulfonate into the reactant d, adding an ethyl acetate solution, heating to 95-100 ℃ at the speed of 4-6 ℃/min, and carrying out heat preservation reaction for 5-6h to obtain the catalyst.
3. The method for preparing the wear-resistant and corrosion-resistant hard alloy milling cutter as claimed in claim 2, wherein the method comprises the following steps: the organic soaking oil is as follows: 35-40 parts of mechanical oil, 1-2 parts of tert-butyl hydroquinone, 3-5 parts of triethanolamine hydrochloride and 2-6 parts of 1, 3-dihydroxyurea, and uniformly mixing the components to obtain the finished product.
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JP2792027B2 (en) * 1988-02-05 1998-08-27 日産自動車株式会社 Heat- and wear-resistant iron-based sintered alloy
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