CN109554628A - The preparation method of graphene composite high speed tool steel - Google Patents

The preparation method of graphene composite high speed tool steel Download PDF

Info

Publication number
CN109554628A
CN109554628A CN201811407391.3A CN201811407391A CN109554628A CN 109554628 A CN109554628 A CN 109554628A CN 201811407391 A CN201811407391 A CN 201811407391A CN 109554628 A CN109554628 A CN 109554628A
Authority
CN
China
Prior art keywords
speed tool
tool steel
high speed
graphene
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811407391.3A
Other languages
Chinese (zh)
Other versions
CN109554628B (en
Inventor
张海平
曹振
***
李炯利
郭建强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AECC Beijing Institute of Aeronautical Materials
Beijing Graphene Technology Research Institute Co Ltd
Original Assignee
AECC Beijing Institute of Aeronautical Materials
Beijing Graphene Technology Research Institute Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by AECC Beijing Institute of Aeronautical Materials, Beijing Graphene Technology Research Institute Co Ltd filed Critical AECC Beijing Institute of Aeronautical Materials
Priority to CN201811407391.3A priority Critical patent/CN109554628B/en
Publication of CN109554628A publication Critical patent/CN109554628A/en
Application granted granted Critical
Publication of CN109554628B publication Critical patent/CN109554628B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/24Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18Hardening; Quenching with or without subsequent tempering
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/005Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy
    • C22C33/0257Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0285Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/30Ferrous alloys, e.g. steel alloys containing chromium with cobalt

Abstract

The present invention relates to a kind of preparation methods of graphene composite high speed tool steel, comprising the following steps: provides mixed liquor, the mixed liquor includes volatile organic solvent, graphene powder and high-speed tool steel powder;It is dried the mixed liquor to obtain mixed powder;The mixed powder after the drying process is loaded into jacket and vacuumize degassing processing and seals the jacket;The sealing jacket for being mounted with the mixed powder is subjected to hip treatment, the temperature of the hot isostatic pressing is 950 DEG C~1300 DEG C, so that the mixed powder forms graphene composite high speed tool steel;And the graphene steel composite high speed tool steel is separated with the jacket.

Description

The preparation method of graphene composite high speed tool steel
Technical field
The present invention relates to high-speed tool steel field of material technology, more particularly to a kind of graphene composite high speed tool steel Preparation method.
Background technique
High-speed tool steel is mainly used to prepare high speed cutting tool, such as the cutting of drill bit, milling cutter and band saw, has red hard Property the high, characteristics such as wearability is good, intensity is high.The fast development of modern manufacturing industry require high-speed tool steel have better performance and Stability, to improve its processing efficiency and machining accuracy.In recent years, the quality and production technology of domestic and international high-speed tool steel Etc. all achieve very fast development, the development of high-speed tool steel has also pushed industrial products to advanced, individuation, high additional The direction of value is developed.But the performance of existing high-speed tool steel only can satisfy the cutting of general material, and for high property For energy part, existing high-speed tool hardness of steel and hardness are still not high enough, while toughness is lower, is unable to satisfy severe service components Process requirements.
Summary of the invention
Based on this, it is necessary to aiming at the problem that how to improve high-speed tool steel mechanical performance, it is compound to provide a kind of graphene The preparation method of high-speed tool steel.
The present invention provides a kind of preparation method of graphene composite high speed tool steel, comprising the following steps:
Mixed liquor is provided, the mixed liquor includes volatile organic solvent, graphene powder and high-speed tool steel powder;
It is dried the mixed liquor to obtain mixed powder;
The mixed powder after the drying process is loaded into jacket and vacuumize degassing processing and will be described Jacket sealing;
The sealing jacket for being mounted with the mixed powder is subjected to hip treatment, the temperature of the hot isostatic pressing is 950 DEG C~1300 DEG C, so that the mixed powder forms composite body;And
The composite body is separated with the jacket.
The temperature of the hot isostatic pressing is 1050 DEG C~1200 DEG C in one of the embodiments,.
Quality of the graphene powder in the graphene composite high speed tool steel point in one of the embodiments, Number 0.01%~2%.
The piece diameter of the graphene powder is 3 μm~40 μm in one of the embodiments,.
The partial size of the high-speed tool steel powder is 10 μm~70 μm in one of the embodiments,.
The step of drying process in one of the embodiments, includes:
The mixed liquor is stirred at 40 DEG C~50 DEG C, until removing the part volatile organic solvent and being formed Slurry;And
The slurry is dried in vacuo, the volatile organic solvent in the slurry is all removed.
Described the step of vacuumizing degassing processing, includes: in one of the embodiments,
By the jacket for being mounted with the mixed powder be evacuated to the vacuum degree in the jacket be less than or equal to 1.0×10-2Pa;And
It is heated to being mounted with described in the mixed powder to be wrapped under the vacuum degree, the heating temperature is 400 DEG C~600 DEG C.
The heating time is 2 hours~10 hours in one of the embodiments,.
The preparation method of the graphene composite high speed tool steel in one of the embodiments, further include: described dry Dry processing step and it is described vacuumize between degassing processing step, to after the drying process mixed powder carry out low temperature ball milling The step of, the temperature of the low temperature ball milling is -80 DEG C~-160 DEG C.
The preparation method of the graphene composite high speed tool steel further includes to described compound in one of the embodiments, The step of body of material is machined.
The organic solvent is dehydrated alcohol in one of the embodiments,.
In one of the embodiments, the high-speed tool steel powder include ferro element, non-graphite carbon and other Element, mass fraction of the non-graphite carbon in the graphene composite high speed tool steel are 1.4%~1.8%.
In one of the embodiments, the other elements be included in the graphene composite high speed tool steel account for it is following The element of mass fraction:
Cr:4.0%~5.0%;
V:4.0%~5.5%;
Mo:1.5%~2.5%;
Co:7.5%~8.2%;
W:10.2%~12%;
Mn :≤0.3%;
Si :≤0.6%.
In one of the embodiments, the high-speed tool steel powder be by steel it is broken after obtain, or be the height The mixing of the simple substance powder of the component of fast tool steel.
The preparation method of graphene composite high speed tool steel provided by the invention, by by graphene and high-speed tool comminuted steel shot Body carries out mechanical mixture, vacuum suction and hip treatment and graphene composite high speed tool steel is prepared.It is quiet by heat etc. The method of pressure makes graphene and high-speed tool comminuted steel shot be consolidated into type, to realize graphene in the case where high temperature and high pressure acts on simultaneously With the combination of high-speed tool comminuted steel shot matrix, solves graphene and be easy to reunite, it can not evenly dispersed and high temperature circle in the base The problem of face is reacted, while processing step is simplified, avoid the degree of oxidation of graphene during multi-step process.Pass through control The temperature of hot isostatic pressing processed realizes the firm connection of graphene and high-speed tool Steel material, so that stone at 950 DEG C~1300 DEG C There is good combination interface between black alkene and steel element, form the graphene composite high speed tool with high-mechanical property Steel.
The graphene composite high speed tool steel can be applied not only to general cutting material, such as cutter, drill bit and band Saw etc., applies also for the accurate punching tool of heavy-duty machinery tool, high-strength material, and the service life is longer.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, by the following examples, to the present invention It is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit The fixed present invention.
The present invention provides a kind of preparation method of graphene composite high speed tool steel, comprising the following steps:
S10, provides mixed liquor, and the mixed liquor includes volatile organic solvent, graphene powder and high-speed tool steel Powder;
S20 is dried the mixed liquor to obtain mixed powder;
The mixed powder after the drying process is loaded into jacket and vacuumize degassing processing and incite somebody to action by S30 The jacket sealing;
The sealing jacket for being mounted with the mixed powder is carried out hip treatment, the temperature of the hot isostatic pressing by S40 It is 950 DEG C~1300 DEG C, so that the mixed powder forms composite body;
S50 separates the composite body with the jacket.
The embodiment of the present invention is quiet by the way that graphene and high-speed tool steel powder are carried out mechanical mixture, vacuum suction and heat etc. Pressure processing, is prepared graphene composite high speed tool steel.By the method for hot isostatic pressing, acted on simultaneously in high temperature and high pressure Under, so that graphene and high-speed tool comminuted steel shot is consolidated into type, to realize the combination of graphene and high-speed tool comminuted steel shot matrix, solves Graphene is easy to reunite, can not evenly dispersed in the base and high-temperature interface the problem of reacting, while simplifying technique step Suddenly, the problem of oxidation of graphene during multi-step process is avoided.By controlling the temperature of hot isostatic pressing 950 DEG C~1300 DEG C, the firm connection of graphene and high-speed tool Steel material is realized, so that having good knot between graphene and steel element Interface is closed, the graphene composite high speed tool steel with high-mechanical property is formed.
The high-speed tool steel powder obtains after being crushed for each group at the powder of element simple substance or by corresponding steel The powder arrived.The high-speed tool steel powder is to account for the iron of 70% or more graphene composite high speed tool steel gross mass as substantially Element, the high-carbon using tungsten, molybdenum, chromium, vanadium, cobalt as main alloy element, and including non-graphite carbon and other doped chemicals High-alloy steel.Composition high-speed tool is calculated according to mass fraction of each component in the graphene composite high speed tool steel The dosage of each component of comminuted steel shot body.In the graphene composite high speed tool steel, the matter of the non-graphite carbon Measuring score can be 1.4%~1.8%, preferably 1.6%~1.7%;The mass fraction of the main alloy element can be with are as follows: W 10.2%~12%, Mo 1.5%~2.5%, Cr 4%~5%, V 4%~5.5%, Co 7.5%~8.2%;It is described Graphene composite high speed tool steel can also include or not include content lower Mn, Si or other alloying elements, it is preferred that Mn ≤ 0.3%, Si≤0.6%.
The mass ratio of the graphene powder and the high-speed tool steel powder is 0.01:99.9~1:49, i.e., described In graphene composite high speed tool steel, the mass fraction of the graphene powder is 0.01%~2%.The graphene is original Graphene, i.e., not oxidized or linkage function group graphene, the number of plies of the graphene can be 1~8 layer, it is preferred that The number of plies of the graphene is 1~3 layer, and the number of plies of the graphene is fewer, the machine of the graphene composite high speed tool steel of formation Tool performance is better.Preferably, in the graphene composite high speed tool steel, the mass fraction of the graphene is 0.05~ 0.5%.
The partial size of the high-speed tool steel powder can be 10 μm~70 μm, the piece diameter of the graphene powder is 3 μm~ 40 μm, which is more advantageous to uniformly mixing between steel powder and graphene powder and mutually matched raising stone The mechanical performance of black alkene composite high speed tool steel.
In step slo, the graphene powder and the high-speed tool steel powder are in the volatile organic solvent It is mixed by evenly dispersed mode, graphene powder uniformly mixes in the mixed powder after volatile organic solvent volatilization In the high-speed tool steel powder.
In one embodiment, the step of offer mixed liquor may include:
The graphene powder and the high-speed tool steel powder are carried out being mixed to form first and be mixed by S12 in drying regime Close powder;
S14 mixes first mixed powder with the volatile organic solvent.
The volatile organic solvent may be selected to be will not be to the graphene powder and the high-speed tool steel powder At least one of easy volatile solvent that property has an impact, including ethyl alcohol, ether, acetone and other organic solvent, it is preferred that described The component of mixed liquor is not aqueous, and the volatile organic solvent is dehydrated alcohol.
It in step s 12, can be by the method for mechanical mixture by the graphene powder and the high-speed tool comminuted steel shot Body uniformly mixes.Preferably, powder machine is mixed by V-type uniformly to mix the graphene powder and the high-speed tool steel powder. The mixing time can be determined according to the partial size and type of the graphene powder and the high-speed tool steel powder.? In one embodiment, the mixing time can be 4 hours~10 hours.
In step S14, first mixed powder and the volatile organic solvent can be by described in stirring formation Mixed liquor.
, can be to heat to the mixed liquor the step of drying process in step S20, the heating Temperature can be 25 DEG C~50 DEG C.In one embodiment, the step S20 and the step S14 can be carried out simultaneously, be passed through The mixed liquor is heated in whipping process so that volatile organic solvent volatilization, can simplify technique step Suddenly.
Preferably, the step of drying process may include: to be stirred the mixed liquor at 40 DEG C~50 DEG C, directly Slurry is formed to the removal part volatile organic solvent, the content of the volatile organic solvent in the slurry is excellent It is selected as the 5%~20% of slurry total weight;And be dried in vacuo the slurry, it all removes described in the slurry Volatile organic solvent.By the drying process, the high-speed tool steel powder can be avoided in prolonged aerobic environment Surface is oxidized in heat drying process.In one embodiment, the vacuum drying temperature can be 80 DEG C~100 DEG C.
In step s 30, described the step of vacuumizing degassing processing, may include:
S32, by vacuum degree that the jacket for being mounted with the mixed powder is evacuated in the jacket be less than or Equal to 1.0 × 10-2Pa;And
S34 is heated, the heating temperature to being mounted with described in the mixed powder to be wrapped under the vacuum degree It is 400 DEG C~600 DEG C.
The completeness and herein of degassing processing is vacuumized using first vacuumizing the step of reheating processing and advantageously ensuring that The property of the mixed powder is unaffected in the process, and heat treatment step is avoided to aoxidize graphene.
In one embodiment, the heating time of the step S34 is 2 hours~10 hours.
In one embodiment, can also include: the drying process step and it is described vacuumize degassing processing step it Between, to after the drying process mixed powder carry out ball milling the step of.Ball milling is carried out before the vacuumize process step, So that the particle size of the mixed powder is smaller, it is more advantageous to thorough degasification.Meanwhile reducing the particle ruler of the mixed powder It is very little, be conducive to reduce the interface distance between graphene and steel element in further hot isostatic pressing, it is multiple to improve the graphene Close the mechanical performance of high-speed tool steel.The ball-milling technology is preferably low temperature ball milling, and low temperature ball milling can not only make the graphite Alkene powder and the high-speed tool steel powder uniformly mix, and can also make the graphene powder and the high-speed tool steel powder Interface cohesion is formed, the mechanical performance of the graphene composite high speed tool steel is further increased.Preferably, the low temperature ball milling Temperature can be -80 DEG C~-160 DEG C.
In step s 40, by the way that the mixed powder to be loaded into the closed jacket, to being mounted with the mixing The jacket of powder applies each to same pressure, while high temperature is imposed, under the influence of high pressure and temperature, so that the mixing Powder is able to be sintered and densification forms graphene composite high speed tool steel.The material of the jacket can be selected from metal or glass Glass.The pressure medium can be using inert gases such as nitrogen, argon gas.
Preferably, the temperature of the hot isostatic pressing can be 1050 DEG C~1200 DEG C.The pressure of the hot isostatic pressing can be with For 120MPa~200MPa.The hip treatment time can be 2 hours~5 hours.The temperature, pressure and time phase Mutually cooperation, so that the global density for the graphene steel composite material that hot isostatic pressing is formed is more evenly, material is finer and close, mechanical Performance is more preferable.
Preferably, the preparation method of the graphene composite high speed tool steel may further include: S60, will be described multiple After condensation material green body is separated with the jacket, the step of the composite body is machined and is heat-treated.Institute It states machining and heat treatment includes isothermal forging, rolling and one of quenching and tempering heat treatment or a variety of.
In one embodiment, the machining includes carrying out isothermal forging, the isothermal forging to composite body Temperature can be 900 DEG C~1200 DEG C, and forging rate can be 0.005mm/min to 0.02mm/min.It can by isothermal forging To be conducive to the precision and matter that improve the graphene composite high speed tool steel for the graphene composite high speed tool steel moulding Amount.
In one embodiment, the machining can also include the steps that rolling the composite body, The rolling temperature can be 1000 DEG C~1200 DEG C.In one embodiment, the thickness of the green body after rolling can be 1.5mm~30mm.The rolling thickness can be determined according to the concrete application of the graphene composite high speed tool steel.
In one embodiment, the machining further comprises being quenched and being tempered heat for the composite body Processing, the hardening heat are 1150~1200 DEG C, and the tempering temperature can be 500 DEG C~600 DEG C, and times of tempering can be 2 to 3 times.The quenching and tempering heat treatment can be further improved the hardness and wearability of workpiece, keep the graphene compound High-speed tool steel obtains better comprehensive mechanical performance.
The embodiment of the present invention also provides a kind of graphene high-speed tool steel, can be prepared by above-mentioned preparation method, the stone Black alkene high-speed tool steel includes high-speed tool steel matrix and the graphene compound with the high-speed tool steel matrix, the high speed work Having steel matrix includes ferro element, non-graphite carbon and other elements, and the other elements include Cr, V, Mo, Co and W;? The mass fraction of each component in the graphene composite high speed tool steel are as follows:
Graphene 0.01%~2%;
Non-graphite carbon 1.4%~1.8%;
Cr 4%~5%;
V 4%~5.5%;
Mo 1.5%~2.5%;
Co 7.5%~8.2%;
W 10.2%~12%.
The graphene composite high speed tool steel of the embodiment of the present invention, the two-dimensional nano for being 0.01%~2% by mass fraction Material graphene and high-speed tool steel matrix containing element-specific are uniformly compound, the unique bi-dimensional cellular crystal structure of graphene With high bond strength, make graphene composite high speed tool steel mechanical performance with higher, bending resistance especially with higher is strong Degree, hardness and impact flexibility.
Further, not only the mass fraction of graphene has an impact to the mechanical performance of bimetal, high-speed tool base steel The mass fraction of each element also will affect the mechanical performance of bimetal in body, such as Cr can promote crystal grain to grow up, and lead to steel Brittleness increase, and W can inhibit crystal grain to grow up and play the role of crystal grain refinement, thus avoid the embrittlement of steel.The present invention is real Example is applied by the proportion of various elements in the control graphene and the high-speed tool steel matrix, makes the compound height of the graphene Fast tool steel comprehensive mechanical performance is more excellent.
In one embodiment, in the graphene composite high speed tool steel, the other elements further include Mn and Si, Mass fraction≤0.3% of the Mn, mass fraction≤0.6% of the Si.
The bending strength of the graphene composite high speed tool steel can reach 3800Mpa~4500Mpa, and the graphene is multiple The hardness for closing high-speed tool steel can reach 70HRC~80HRC, and the impact flexibility of the graphene composite high speed tool steel can reach 70J/cm2~90J/cm2
Embodiment 1
The raw material of following quality is provided, the powder including graphene powder He each element simple substance that can make up high-speed tool steel Totally 1000 grams of body, wherein 2 grams of graphene, 16 grams of agraphitic carbon, 47 grams of Cr, 18 grams of Mo, 49 grams of V, 110 grams of W, Co 80 Gram, 6 grams of Si, 3 grams of Mn, surplus Fe.The average diameter for forming the powder of each element simple substance of high-speed tool steel is 50 μm.
Graphene powder and each element simple substance powder are put into the mixed powder machine of V-type and carry out mixed powder 8h;
It disperses mixed powder in dehydrated alcohol, it is in slurry that mixture is dried under 40 DEG C of mechanical stirrings Shape is transferred in vacuum drying box and is thoroughly dried, and drying temperature is 100 DEG C, obtains mixed powder;
Mixed powder after drying is fitted into cylindrical steel jacket, and being evacuated to vacuum pressure is 1 × 10-2After Pa, heating To 600 DEG C, 2h is kept the temperature, is cooled to welding steel capsule sealing sealing after room temperature;
By the steel capsule sealed temperature be 1200 DEG C, pressure be 160MPa under conditions of carry out hip treatment 2 it is small When, mixed powder consolidation is bimetal;
By the steel capsule removal outside the bimetal after hot isostatic pressing, then in 1180 DEG C of progress isothermal forgings, forging speed Rate is 0.01mm/min;
Bimetal after isothermal forging is rolled at 1150 DEG C;
The bimetal rolled is subjected to 1180 DEG C of quenchings, carries out the tempering of 550 DEG C × 1h × 3 time later.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, the results are shown in Table 1.
Embodiment 2
It is essentially identical with the preparation method of embodiment 1, the difference is that, in raw material, form each member of high-speed tool steel The average diameter of the powder of plain simple substance is less than 10 μm.
Measuring Mechanical Properties are carried out to the graphene composite high speed tool steel of preparation, the results are shown in Table 1.It can be with from table 1 Find out, embodiment 1 prepare Steel material bending strength, hardness and in terms of performance all be better than embodiment 2, Illustrate that size controlling is conducive to enhance in the appropriate range the mechanical performance of graphene composite high speed tool steel.
Embodiment 3
It is essentially identical with the raw material and preparation method of embodiment 1, it the difference is that only, disperse mixed powder in After dehydrated alcohol, mixed powder is thoroughly dried to obtain under 100 DEG C of mechanical stirrings directly in open environment.
Measuring Mechanical Properties are carried out to the graphene composite high speed tool steel of preparation, the results are shown in Table 1.It can be with from table 1 Find out, since graphene is there are a degree of oxidation in the drying process of embodiment 3, the Steel material for preparing embodiment 3 Embodiment 1 can be lower than.
Embodiment 4
It is essentially identical with the raw material and preparation method of embodiment 1, it the difference is that only, to mixed after the drying process It closes powder and carries out low temperature ball milling before jacket, the temperature of the low temperature ball milling is -120 DEG C, and Ball-milling Time is 6 hours.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, as a result as shown in table 1 below.From table 1 As can be seen that low temperature ball milling is conducive to improve the mechanical performance of high-speed tool steel.
Embodiment 5
It is essentially identical with the raw material and preparation method of embodiment 1, it the difference is that only, to mixed after the drying process It closes powder and carries out room temperature ball milling before jacket, the temperature of the room temperature ball milling is 25 DEG C, and Ball-milling Time is 6 hours.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, as a result as shown in table 1 below.
As it can be seen from table 1 graphene is unfavorable for improving high speed work there are a degree of oxidation in room temperature mechanical milling process Has the mechanical performance of steel.
Comparative example 1
It is essentially identical with the preparation method of embodiment 1, it the difference is that only, graphene is not added in raw material.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, as a result as shown in table 1 below.
Comparative example 2
It is identical as the raw material of embodiment 1, the difference is that, using cold isostatic compaction technique, the preparation method comprises the following steps:
Specifically, the steel for being sealed with mixed powder is prepared under the same conditions by step same as Example 1 Jacket, by steel capsule in 25 DEG C of progress isostatic cool pressing processing, pressure 300MPa, time 10min;Obtained bimetal is existed It is sintered 2h at 1150 DEG C, then carries out isothermal forging same as Example 1, rolling, quenching and tempering step.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, as a result as shown in table 1 below.
Comparative example 3
It is identical as the raw material of embodiment 1, the difference is that, using pressure forming and high-sintering process.
Specifically, preparing mixed powder under the same conditions using step same as Example 1.
Mixed powder is fitted into cylindrical die, compaction treatment, pressure maintaining are carried out to mixed powder using 2000T press machine 10min.1150 DEG C of sintering are warming up to green body after extrusion forming, heat preservation 2h obtains bimetal, then carries out and 1 phase of embodiment Same isothermal forging, rolling, quenching and tempering step.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, as a result as shown in table 1 below.
Comparative example 4
It is essentially identical with the preparation method of embodiment 1, the difference is that, the temperature of hot isostatic pressing is 850 DEG C.
Measuring Mechanical Properties are carried out to the graphene composite high speed tool steel of preparation, the results are shown in Table 1.
Comparative example 5
It is identical as the preparation method of embodiment 1, it the difference is that only, the quality of Cr is increased to 100 grams in raw material, The Fe for reducing corresponding amount, makes the mass fraction 10% of Cr.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, as a result as shown in table 1 below.
Comparative example 6
It is identical as the preparation method of embodiment 1, it the difference is that only, by the Mass lost of W to 50 grams in raw material, increase The Fe for adding corresponding amount makes the mass fraction 5% of W.
Measuring Mechanical Properties are carried out to the graphene steel composite high speed tool steel of preparation, as a result as shown in table 1 below.
Table 1
Graphene composite high speed tool steel Bending strength Hardness Impact toughness α k
Embodiment 1 4000MPa 72HRC 88J/cm2
Embodiment 2 3450MPa 67HRC 48J/cm2
Embodiment 3 3560MPa 68HRC 50J/cm2
Embodiment 4 4050MPa 73HRC 90J/cm2
Embodiment 5 3550MPa 68HRC 50J/cm2
Comparative example 1 2900MPa 60HRC 39J/cm2
Comparative example 2 3100MPa 65HRC 42J/cm2
Comparative example 3 3230MPa 64HRC 41J/cm2
Comparative example 4 3010MPa 64HRC 40J/cm2
Comparative example 5 2800MPa 59HRC 38J/cm2
Comparative example 6 3055MPa 61HRC 44J/cm2
As it can be seen from table 1 the steel of embodiment preparation are in the mechanical performances such as bending strength, hardness and impact toughness It is better than the steel of comparative example preparation, illustrates addition, the molding technique of consolidation, the temperature of hot isostatic pressing and the element of graphene The proportion of mass fraction is to influence the mechanical key factor of steel to be conducive to make institute by these key factors of comprehensively control Graphene composite high speed tool steel is stated with excellent mechanical performance, bending strength especially with higher, hardness and impact are tough Property.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (14)

1. a kind of preparation method of graphene composite high speed tool steel, which comprises the following steps:
Mixed liquor is provided, the mixed liquor includes volatile organic solvent, graphene powder and high-speed tool steel powder;
It is dried the mixed liquor to obtain mixed powder;
The mixed powder after the drying process is loaded into jacket and vacuumize degassing processing and by the jacket Sealing;
The sealing jacket for being mounted with the mixed powder is subjected to hip treatment, the temperature of the hot isostatic pressing is 950 DEG C ~1300 DEG C, so that the mixed powder forms composite body;And
The composite body is separated with the jacket.
2. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that described heat etc. is quiet The temperature of pressure is 1050 DEG C~1200 DEG C.
3. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that the graphene Mass fraction 0.01%~2% of the powder in the graphene composite high speed tool steel.
4. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that the graphene The piece diameter of powder is 3 μm~40 μm.
5. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that the high speed work The partial size for having comminuted steel shot body is 10 μm~70 μm.
6. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that at the drying The step of reason includes:
The mixed liquor is stirred at 40 DEG C~50 DEG C, until removing the part volatile organic solvent and forming slurry Material;And
The slurry is dried in vacuo, the volatile organic solvent in the slurry is all removed.
7. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that described to vacuumize The step of degassing processing includes:
By the jacket for being mounted with the mixed powder be evacuated to the vacuum degree in the jacket be less than or equal to 1.0 × 10-2Pa;And
It is heated to being mounted with described in the mixed powder to be wrapped under the vacuum degree, the heating temperature is 400 DEG C ~600 DEG C.
8. the preparation method of graphene composite high speed tool steel according to claim 7, which is characterized in that when the heating Between be 2 hours~10 hours.
9. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that further include: The drying process step and it is described vacuumize between degassing processing step, to after the drying process mixed powder carry out it is low The step of warm ball milling, the temperature of the low temperature ball milling are -80 DEG C~-160 DEG C.
10. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that further include pair The step of composite body is machined.
11. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that described organic Solvent is dehydrated alcohol.
12. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that the high speed Tool steel powder includes ferro element, non-graphite carbon and other elements, and the non-graphite carbon is in the graphene Mass fraction in composite high speed tool steel is 1.4%~1.8%.
13. the preparation method of graphene composite high speed tool steel according to claim 12, which is characterized in that it is described other Element includes the element that following mass fraction is accounted in the graphene composite high speed tool steel:
Cr:4.0%~5.0%;
V:4.0%~5.5%;
Mo:1.5%~2.5%;
Co:7.5%~8.2%;
W:10.2%~12%;
Mn :≤0.3%;
Si :≤0.6%.
14. the preparation method of graphene composite high speed tool steel according to claim 1, which is characterized in that the high speed Tool steel powder be by steel it is broken after obtain, or for the high-speed tool steel component simple substance powder mixing.
CN201811407391.3A 2018-11-23 2018-11-23 Preparation method of graphene composite high-speed tool steel Active CN109554628B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811407391.3A CN109554628B (en) 2018-11-23 2018-11-23 Preparation method of graphene composite high-speed tool steel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811407391.3A CN109554628B (en) 2018-11-23 2018-11-23 Preparation method of graphene composite high-speed tool steel

Publications (2)

Publication Number Publication Date
CN109554628A true CN109554628A (en) 2019-04-02
CN109554628B CN109554628B (en) 2020-04-28

Family

ID=65867203

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811407391.3A Active CN109554628B (en) 2018-11-23 2018-11-23 Preparation method of graphene composite high-speed tool steel

Country Status (1)

Country Link
CN (1) CN109554628B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061813A (en) * 2021-03-22 2021-07-02 吉林省大维科技发展有限公司 Anti-corrosion alloy steel for heating radiator and preparation method thereof
CN114457275A (en) * 2021-09-29 2022-05-10 北京机科国创轻量化科学研究院有限公司 Graphene reinforced alloy steel and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08277403A (en) * 1995-04-06 1996-10-22 Sumitomo Special Metals Co Ltd Production of permanent magnet alloy powder for bond magnet and apparatus therefor
CN103590089A (en) * 2013-11-20 2014-02-19 上海应用技术学院 Preparation method of graphene/silver composite material
CN103614583A (en) * 2013-09-29 2014-03-05 魏玲 Novel high-conductivity and high-strength graphene/copper material and preparation method thereof
CN104466110A (en) * 2014-11-05 2015-03-25 惠州龙为科技有限公司 Preparation method of high-performance lithium ion battery negative electrode material
CN105063401A (en) * 2015-06-25 2015-11-18 中国航空工业集团公司北京航空材料研究院 Preparation method of aluminum base graphene alloy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08277403A (en) * 1995-04-06 1996-10-22 Sumitomo Special Metals Co Ltd Production of permanent magnet alloy powder for bond magnet and apparatus therefor
CN103614583A (en) * 2013-09-29 2014-03-05 魏玲 Novel high-conductivity and high-strength graphene/copper material and preparation method thereof
CN103590089A (en) * 2013-11-20 2014-02-19 上海应用技术学院 Preparation method of graphene/silver composite material
CN104466110A (en) * 2014-11-05 2015-03-25 惠州龙为科技有限公司 Preparation method of high-performance lithium ion battery negative electrode material
CN105063401A (en) * 2015-06-25 2015-11-18 中国航空工业集团公司北京航空材料研究院 Preparation method of aluminum base graphene alloy

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061813A (en) * 2021-03-22 2021-07-02 吉林省大维科技发展有限公司 Anti-corrosion alloy steel for heating radiator and preparation method thereof
CN113061813B (en) * 2021-03-22 2022-02-22 吉林省大维科技发展有限公司 Anti-corrosion alloy steel for heating radiator and preparation method thereof
CN114457275A (en) * 2021-09-29 2022-05-10 北京机科国创轻量化科学研究院有限公司 Graphene reinforced alloy steel and preparation method thereof
CN114457275B (en) * 2021-09-29 2022-08-02 北京机科国创轻量化科学研究院有限公司 Graphene-reinforced 20CrMnTi alloy steel and preparation method thereof

Also Published As

Publication number Publication date
CN109554628B (en) 2020-04-28

Similar Documents

Publication Publication Date Title
CN108823478B (en) Ultra-fine high-entropy alloy binding phase metal ceramic and preparation method thereof
KR100976731B1 (en) Ultra-hard composite material and method for manufacturing the same
EP0600421B1 (en) Low alloy sintered steel and method of preparing the same
CN103667873B (en) P/m high speed steel and preparation method thereof
KR101711496B1 (en) High strength low alloyed sintered steel
CN111793762B (en) Intermetallic compound and carbonitride jointly-strengthened hardening powder metallurgy high-speed steel and preparation method thereof
CN111793773B (en) High-speed steel through Laves phase and mu phase composite strong hardening and preparation method thereof
CN110257688B (en) High-speed steel containing boride powder and preparation method thereof
JP2020501027A (en) Powder metallurgically produced steel material comprising hard material particles, a method for producing parts from such steel material, and parts produced from steel material
CN113265573A (en) High-strength high-toughness high-entropy alloy ceramic and preparation method thereof
CN107557704A (en) A kind of hot forming dies materials and preparation method thereof
CN113512687A (en) Preparation method of composite rare earth reinforced powder metallurgy high-speed steel
CN109554628A (en) The preparation method of graphene composite high speed tool steel
US3809541A (en) Vanadium-containing tool steel article
CN114635069A (en) High-strength-toughness medium-entropy alloy binding phase Ti (C, N) -based metal ceramic and preparation method thereof
JP4703005B2 (en) Steel, use of the steel, product made of the steel and method for producing the steel
CN109554627A (en) Graphene composite high speed tool steel
CN112981265A (en) Carbon-free high-speed steel and preparation method thereof
CN109702206A (en) The preparation method of skates
CN111074166A (en) Molybdenum-containing high-strength powder metallurgy composite material and preparation method thereof
JPH09157805A (en) High strength iron base sintered alloy
JP2001214238A (en) Powder hot tool steel excellent in heat crack resistance and wear resistance and hot die
JPH06212368A (en) Low alloy sintered steel excellent in fatigue strength and its production
CN111101011A (en) Carbide-cobalt nickel iron amorphous-based hard alloy material generated in situ and preparation method thereof
JPH0321621B2 (en)

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant