CN110396631A - A kind of continuous method and device for preparing WC-10Ni-ZrO2 hard alloy - Google Patents

A kind of continuous method and device for preparing WC-10Ni-ZrO2 hard alloy Download PDF

Info

Publication number
CN110396631A
CN110396631A CN201910711968.8A CN201910711968A CN110396631A CN 110396631 A CN110396631 A CN 110396631A CN 201910711968 A CN201910711968 A CN 201910711968A CN 110396631 A CN110396631 A CN 110396631A
Authority
CN
China
Prior art keywords
powder
zro
storehouse
mixing bunker
heating cabinet
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
CN201910711968.8A
Other languages
Chinese (zh)
Other versions
CN110396631B (en
Inventor
崔凯辉
陈华
周俊文
彭金辉
邱晨
廖天棋
万文军
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.)
Kunming University of Science and Technology
Original Assignee
Kunming University of Science and Technology
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 Kunming University of Science and Technology filed Critical Kunming University of Science and Technology
Priority to CN201910711968.8A priority Critical patent/CN110396631B/en
Publication of CN110396631A publication Critical patent/CN110396631A/en
Application granted granted Critical
Publication of CN110396631B publication Critical patent/CN110396631B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/003Apparatus, e.g. furnaces
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1054Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Powder Metallurgy (AREA)
  • Furnace Details (AREA)

Abstract

The present invention discloses a kind of continuous preparation WC-10Ni-ZrO2The method and device of hard alloy, by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, the mass percentage content of WC powder is 89.00 ~ 89.75% in mixed-powder;The mass percentage content of Ni powder is 10%, ZrO2The mass percentage content of particle is 0.25 ~ 1.00%;By mixed-powder under protective atmosphere, contiguous segmentation microwave heating is carried out, obtains WC-10Ni-ZrO after cooling2Hard alloy;Present invention process is reasonable, easy to operate, sintering period shortening, energy conservation and environmental protection, gained sample consistency are high, and crystal grain is tiny, even tissue, is suitble to industrialized production.

Description

A kind of continuous method and device for preparing WC-10Ni-ZrO2 hard alloy
Technical field
The invention belongs to hard alloy technical fields, more particularly to a kind of continuous preparation WC-10Ni-ZrO2Hard alloy Method.
Background technique
WC base cemented carbide is due to steady with high intensity, high rigidity, high abrasion, high temperature resistant, corrosion-resistant and excellent chemistry It is qualitative, it has been widely used in the fields such as cutting tool, mine tool, mechanical seal and wear part.All the time, WC- Co series hard alloy is the first choice in WC base cemented carbide market.However, in recent years, due to the shortage of global cobalt resource, price is high It is expensive, in addition WC-Co series hard alloy is anti-oxidant, corrosion resistance is not good enough, thus WC-Co series hard alloy further apply by Limitation.Therefore, people begin one's study the substitute of binder Co.Result of study shows the function due to Ni with excellent wetting WC Can, and Ni has good anti-oxidant, corrosion resistance, and Ni resource relative abundance, cheap in addition, thus WC-Ni class Hard alloy is increasingly valued by people.But since bonding reinforcing degree of the Ni and Co to hard phase WC is different, so phase Comprehensive mechanical property with the WC-Ni hard alloy of content binder is lower than WC-Co hard alloy.For this purpose, scientific research personnel is to WC- The improvement of Ni hard alloy mechanical property has conducted extensive research.
Currently, the research that WC-Ni hard alloy mechanical property improves is concentrated mainly on two aspects: first is that passing through Fast Sintering Method come achieve the purpose that improve WC-Ni hard alloy mechanical property, such as using high-frequency induction heating be sintered, discharge plasma burn Knot etc..Result of study shows that the mechanical property of the WC-Ni hard alloy of Fast Sintering method preparation is better than traditional sintering side really The WC-Ni hard alloy of method preparation, but fracture toughness has certain decline;Second is that adding one in WC-Ni hard alloy powder Quantitative inhibitor (mainly has VC, TaC, Cr3C2With TiC etc.), inhibit WC-Ni sintering cemented carbide mistake by these carbide WC grain is grown up in journey, to improve the mechanical property of hard alloy.
Microwave be it is a kind of can quickly, the electromagnetic wave of transmitting energy in situ, be a kind of green, quickly, efficiently, be easy to automatic control New energy.Microwave heating is different from conventional heating, it is not required to heat transfer from outward appearance to inner essence, but through microwave in material The energy dissipation in portion directly heats material, has that selective heated material, heating rate is fast, heating efficiency is high, reduces reaction Temperature shortens the advantageous characteristics such as reaction time.ZrO2With high-intensitive, excellent wave absorbtion and thermal stability, but made in addition There are complex procedures during standby, the defects such as long preparation period, forming temperature are high, toughness is low.
Summary of the invention
In view of the problems of the existing technology and it is insufficient, on the basis of the present invention designs a kind of microwave multimode cavity reactor, It is simple that design provides a kind of process, short preparation period, efficiently, the method for sintered products purity is high and good toughness.
The present invention provides a kind of continuous preparation WC-10Ni-ZrO2The method of hard alloy, comprising the following steps:
(1) by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, WC in mixed-powder The mass percentage content of powder is 89.00 ~ 89.75%;The mass percentage content of Ni powder is 10%, ZrO2The quality of particle Degree is 0.25 ~ 1.00%, and the sum of three is 100%;
(2) by the mixed-powder of step (1) under protective atmosphere, cooling obtains WC-10Ni- after carrying out contiguous segmentation microwave heating ZrO2Hard alloy.
Step (1) WC powder granularity is 6 μm ~ 9 μm, and Ni powder size is 10 μm ~ 13 μm, ZrO2Grain graininess be 20nm ~ 25nm。
Step (1) WC powder purity is greater than 99.6%, Ni powder size purity and is greater than 99.91%, ZrO2Particle purity is greater than 99.02%。
Step (2) protective atmosphere is N2And H2It is N according to volume ratio2: H2The mixed gas of=85:15 mixing.
Step (2) contiguous segmentation microwave heating comprises the concrete steps that: 300 DEG C stirring 10 ~ 20 minutes first in mixing bunker, so 1200 ~ 1500 DEG C heat preservation 10 ~ 20 minutes in heating cabinet afterwards, finally 400 ~ 800 DEG C of coolings in cooling storehouse, make the alloy of melting Stablize cooling, avoids rapid cooling;After material enters heating cabinet from mixing bunker, new material enters mixing bunker, and material is from heating After storehouse enters cooling storehouse, the material of mixing bunker enters heating cabinet again, realizes continuous preparation.
The present invention also provides continuous preparation WC-10Ni-ZrO2The device of hard alloy, including feed intake storehouse 1, spiral agitator 2, mixing bunker 3, microwave generator 4, heating cabinet 5, cooling storehouse 6, discharge nozzle 7, cooling bath 8, outlet valve 9, venthole 10, insulating layer 11, venthole 13, thermocouple temperature sensor I 14, air gauge 15, motor 16, electromagnetic door I 17, microwave waveguide I 18, microwave wave Lead II 19, microwave waveguide III 20, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22, electromagnetic door II 23;
It feeds intake and connects at the top of storehouse 1 and mixing bunker 3, spiral agitator 2 is equipped in mixing bunker 3, spiral agitator 2 and motor 16 connect It connecing, venthole 13, thermocouple temperature sensor I 14, air gauge 15 is additionally provided on mixing bunker 3, mixing bunker 3 is connect with heating cabinet 5, Electromagnetic door I 17 is equipped between mixing bunker 3 and heating cabinet 5,3 side of mixing bunker is equipped with thermocouple temperature sensor II 21, mixing bunker 3 It is connect with cooling storehouse 6, electromagnetic door II 23 is equipped between mixing bunker 3 and cooling storehouse 6, cooling 6 side of storehouse is equipped with venthole 10, thermoelectricity Even temperature sensor III 22, cooling storehouse 6 are connect by discharge nozzle 7 with cooling bath 8, and discharge nozzle 7 is equipped with outlet valve 9;
Insulating layer 11 is equipped with outside mixing bunker 3, heating cabinet 5, the storehouse 6 that cools down, microwave waveguide I 18 passes through the setting of insulating layer 11 and feeding intake Outside storehouse 1, microwave waveguide II 19 passes through insulating layer 11 and is arranged outside heating cabinet 5, and microwave waveguide III 20 passes through insulating layer 11 and sets It sets outside cooling storehouse 6;Microwave waveguide I 18, microwave waveguide II 19, microwave waveguide III 20 are connect with microwave generator 4 respectively.
Described device further includes PLC controller 12, microwave generator 4, outlet valve 9, thermocouple temperature sensor I 14, electricity Machine 16, electromagnetic door I 17, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22, electromagnetic door II 23 respectively with PLC Controller 12 connects.
The storehouse 1 that feeds intake, heating cabinet 5, cool down storehouse 6 cross section be regular pentagon.
1 entrance of storehouse that feeds intake is located in 2 blade outer radii of spiral agitator.
Continuous preparation WC-10Ni-ZrO is carried out using above-mentioned apparatus2Hard alloy, the specific steps are as follows:
(1) by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, WC in mixed-powder The mass percentage content of powder is 89.00 ~ 89.75%;The mass percentage content of Ni powder is 10%, ZrO2The quality of particle Degree is 0.25 ~ 1.00%, and the sum of three is 100%;
(2) electromagnetic door I 17, electromagnetic door II 23 are opened, venthole 10 is closed, in venthole 13 to mixing bunker 3, heating cabinet 5, cooling It is vacuumized in storehouse 6, when air gauge 15 shows that vacuum degree is lower than 100Pa, stops vacuumizing, venthole 10 is opened, to mixing bunker 3, heating cabinet 5, cooling are passed through protective gas in storehouse 6, ventilate ten minutes later, vacuumize again, after so recycling three times, mixing bunker 3, heating cabinet 5, cooling are full of protective gas in storehouse 6, close venthole 10 and venthole 13, by adjusting microwave generator 4, make Microwave waveguide I 18, microwave waveguide II 19, microwave waveguide III 20 are heated to setting to mixing bunker 3, heating cabinet 5, cooling storehouse 6 respectively It is kept the temperature after temperature, may be otherwise each microwave waveguide and connect different microwave generators and heated;
(3) mixed-powder of step (1) is poured into the storehouse 1 that feeds intake, mixed-powder is from blade of the storehouse 1 along spiral agitator 2 that feed intake Into mixing bunker 3, after mixed-powder is sufficiently agitated mixing preheating in mixing bunker 3, electromagnetic door I 17 is opened, material, which enters, to be added In hot storehouse 5, after heating cabinet 5 keeps the temperature a period of time, electromagnetic door II 23 is opened, material enters cooling storehouse 6, and material is in cooling storehouse 6 After interior temperature is down to set temperature, outlet valve 9 is opened, WC-10Ni- is made after entering the cooling of cooling bath 8 along discharge nozzle 7 in material ZrO2Hard alloy;
After the material in mixing bunker 3 enters in heating cabinet 5, new mixed-powder is entered in mixing bunker 3, the object in heating cabinet 5 Material heats after terminating to enter to cool down in storehouse 6, after the material in mixing bunker 3 enters in heating cabinet 5, realizes continuous preparation.
The present invention using microwave heating by electromagnetic energy material internal be converted into thermal energy volume heating behavior to Cause powder consolidation and alloying, has the advantages that the period is short, energy consumption is low and environmental-friendly.The material of acquisition is shown It is fast densified, the advantageous features such as even tissue.Compared with prior art, the invention has the following advantages that
1, process flow is simplified.During the sintering process, addition powder raw material is not necessarily to be pressed into base in advance the method for the present invention, Mix the storehouse that feeds intake.
2, manufacturing cycle is shortened, preparation efficiency is improved.When being prepared using the method for the present invention, powder systems are in electricity Fast Sintering under the coupling of field, magnetic field and temperature field, is added to ZrO2Particle, ZrO2Particle has excellent microwave absorbing property, Heating rate is much higher than traditional heating rate.
3, the mechanical property of WC-10Ni base cemented carbide composite material is improved, consistency is high, and crystal grain is tiny, and tissue is equal Even, properties improve a lot compared to the alloy being sintered in conventional resistive furnace.
4, the present invention is by entire technique serialization, can not parking realization serialization, can be completed within 20 ~ 30 minutes entire Sintering process, and alloy is directly discharged by discharge nozzle and is collected.
5, preparation process is easily controllable.Microwave feed-in power is adjusted using PLC controller to control heating rate, burn The technological parameters such as junction temperature, soaking time efficiently solve and are difficult to carry out in fact multiple technological parameters in preparing alloy process When the problem of controlling.
6, process is pollution-free.The present invention uses TE10Modes microwave feed-in multimode cavity quickly add to metal powder Heat not only realizes Fast Sintering in the short time, realizes high efficiency low energy consumption;And heating cycle is substantially reduced, to inhibit Growing up for crystal grain, has requested the dependence to additive, meets the requirement of " green production ".
Detailed description of the invention
Fig. 1 is the structural schematic diagram of 1 device of the embodiment of the present invention;
In figure: 1- feeds intake storehouse;2- spiral agitator;3- mixing bunker;4- microwave generator;5- heating cabinet;6- cooling storehouse;7- discharging Pipe;8- cooling bath;9- outlet valve;10- venthole;11- insulating layer;12-PLC controller;13- venthole;14- electric thermo-couple temperature Sensor I;15- air gauge;16- motor;17- electromagnetic door I;18- microwave waveguide I;19- microwave waveguide II;20- microwave waveguide Ⅲ;21- thermocouple temperature sensor II;22- thermocouple temperature sensor III;23- electromagnetic door II.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples, but the present invention is not by the limit of following embodiments System.
Embodiment 1
A kind of continuous preparation WC-10Ni-ZrO2The device of hard alloy, as shown in Figure 1, include feed intake storehouse 1, spiral agitator 2, Mixing bunker 3, microwave generator 4, heating cabinet 5, cooling storehouse 6, discharge nozzle 7, cooling bath 8, outlet valve 9, venthole 10, insulating layer 11, PLC controller 12, venthole 13, thermocouple temperature sensor I 14, air gauge 15, motor 16, electromagnetic door I 17, microwave wave Lead I 18, microwave waveguide II 19, microwave waveguide III 20, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22, electricity Magnetic gate II 23;It feeds intake and connects at the top of storehouse 1 and mixing bunker 3, spiral agitator 2, spiral agitator 2 and motor are equipped in mixing bunker 3 16 connect, and venthole 13, thermocouple temperature sensor I 14, air gauge 15, mixing bunker 3 and heating cabinet 5 are additionally provided on mixing bunker 3 Connection is equipped with electromagnetic door I 17 between mixing bunker 3 and heating cabinet 5,3 side of mixing bunker is equipped with thermocouple temperature sensor II 21, mixes It closes storehouse 3 to connect with cooling storehouse 6, electromagnetic door II 23 is equipped between mixing bunker 3 and cooling storehouse 6, cooling 6 side of storehouse is equipped with venthole 10, thermocouple temperature sensor III 22, cooling storehouse 6 are connect by discharge nozzle 7 with cooling bath 8, and cooling storehouse 6 is connect with cooling bath 8 Discharge nozzle 7 be equipped with outlet valve 9;
Insulating layer 11 is equipped with outside mixing bunker 3, heating cabinet 5, the storehouse 6 that cools down, microwave waveguide I 18 passes through the setting of insulating layer 11 and feeding intake Outside storehouse 1, microwave waveguide II 19 passes through insulating layer 11 and is arranged outside heating cabinet 5, and microwave waveguide III 20 passes through insulating layer 11 and sets It sets outside cooling storehouse 6, microwave waveguide I 18, microwave waveguide II 19, microwave waveguide III 20 are connect with microwave generator 4 respectively, Can each microwave waveguide connect different microwave generators, microwave generator 4, outlet valve 9, thermocouple temperature sensor I 14, Motor 16, electromagnetic door I 17, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22, electromagnetic door II 23 respectively with PLC controller 12 connects, and the storehouse 1 that feeds intake, heating cabinet 5, cooling storehouse 6 are that cross section is positive pentagonal hollow cylinder;It throws 1 entrance of feed bin is located in 2 blade outer radii of spiral agitator.
Embodiment 2
A kind of continuous preparation WC-10Ni-ZrO of progress2The method of hard alloy, using the device of embodiment 1, specific steps are such as Under:
(1) by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, WC in mixed-powder The mass percentage content of powder is 89.75%;The mass percentage content of Ni powder is 10%, ZrO2The mass percent of particle Content is 0.25%, and the sum of three is 100%;WC powder granularity is 6 μm ~ 9 μm, and Ni powder size is 10 μm ~ 13 μm, ZrO2 Grain granularity is 20nm ~ 25nm;WC powder purity is greater than 99.6%, Ni powder size purity and is greater than 99.91%, ZrO2Particle purity is big In 99.02%;Ball milling is wet-milling, and medium is water, ball milling one hour;
(2) electromagnetic door I 17, electromagnetic door II 23 are opened, venthole 10 is closed, in venthole 13 to mixing bunker 3, heating cabinet 5, cooling It is vacuumized in storehouse 6, when air gauge 15 shows that vacuum degree is lower than 100Pa, stops vacuumizing, venthole 10 is opened, to mixing bunker 3, heating cabinet 5, cooling are passed through protective gas, protective atmosphere N in storehouse 62And H2It is N according to volume ratio2: H2=85:15 mixing Mixed gas, ventilation ten minutes later, vacuumize again, and after so recycling three times, mixing bunker 3, heating cabinet 5, cooling are full of in storehouse 6 Protective gas closes venthole 10 and venthole 13, by adjusting microwave generator 4, makes microwave waveguide I 18, microwave waveguide II 19, microwave waveguide III 20 is heated to 300 DEG C, 1200 DEG C, 400 DEG C to mixing bunker 3, heating cabinet 5, cooling storehouse 6 respectively, reaches target After temperature, thermocouple temperature sensor I 14, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22 are anti-by temperature PLC controller of feeding 12, after PLC controller 12 receives temperature information, adjust microwave generator 4, to mixing bunker 3, heating cabinet 5, Cooling storehouse 6 is kept the temperature;
(3) mixed-powder of step (1) is poured into the storehouse 1 that feeds intake, enters mixing along the blade of spiral agitator 2 from storehouse 1 is fed intake Storehouse 3, mixed-powder is sufficiently agitated mixing preheating after twenty minutes in mixing bunker 3, and PLC controller 12 closes spiral agitator 2 Motor 16, stop stirring, open electromagnetic door I 17, after material enters in heating cabinet 5, turn off electromagnetic door I 17, material is adding After twenty minutes, PLC controller 12 opens electromagnetic door II 23 for 1200 DEG C of heat preservations in hot storehouse 5, and material enters cooling storehouse 6, PLC controller 12 close electromagnetic doors II 23, and for material after temperature is down to 400 DEG C in cooling storehouse 6, PLC controller 12 opens outlet valve 9, material edge Discharge nozzle 7 be included in into cooling bath 8 it is cooling after obtain WC-10Ni-ZrO2Hard alloy;
After the material in mixing bunker 3 enters in heating cabinet 5, new mixed-powder is entered in mixing bunker 3, the object in heating cabinet 5 Material heats after terminating to enter to cool down in storehouse 6, after the material in mixing bunker 3 enters in heating cabinet 5, realizes continuous preparation.
The present embodiment discharge nozzle 7 can also connect forging press etc. according to actual needs, forge into the shape knot of needs while hot Structure.
It is relatively close using Archimedes (Archimedes) drainage test sample by polishing, polishing after sintered body is cooling Degree;Using the fracture toughness (points is taken to be all larger than 5 points) of indentation method test sample;Using HVS-50 microhardness testers, apply 196N load, 10 s of pressure maintaining, the Vickers hardness of test sample;Using the bending strength of three-point bending method test sample, span 30mm.The relative density for measuring alloy sample is 98.50%, fracture toughness 11.52MPam1/2, vickers hardness hv reaches 1498MPa, bending strength reach 702.25MPa.
Embodiment 3
A kind of continuous preparation WC-10Ni-ZrO of progress2The method of hard alloy, using the device of embodiment 1, specific steps are such as Under:
(1) by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, WC in mixed-powder The mass percentage content of powder is 89%;The mass percentage content of Ni powder is 10%, ZrO2The mass percent of particle contains Amount is 1%, and the sum of three is 100%;WC powder granularity is 6 μm ~ 9 μm, and Ni powder size is 10 μm ~ 13 μm, ZrO2Particle Degree is 20nm ~ 25nm;WC powder purity is greater than 99.6%, Ni powder size purity and is greater than 99.91%, ZrO2Particle purity is greater than 99.02%;Ball milling is wet-milling, and medium is water, ball milling one hour;
(2) electromagnetic door I 17, electromagnetic door II 23 are opened, venthole 10 is closed, in venthole 13 to mixing bunker 3, heating cabinet 5, cooling It is vacuumized in storehouse 6, when air gauge 15 shows that vacuum degree is lower than 100Pa, stops vacuumizing, venthole 10 is opened, to mixing bunker 3, heating cabinet 5, cooling are passed through protective gas, protective atmosphere N in storehouse 62And H2It is N according to volume ratio2: H2=85:15 mixing Mixed gas, ventilation ten minutes later, vacuumize again, and after so recycling three times, mixing bunker 3, heating cabinet 5, cooling are full of in storehouse 6 Protective gas closes venthole 10 and venthole 13, by adjusting microwave generator 4, makes microwave waveguide I 18, microwave waveguide II 19, microwave waveguide III 20 is heated to 300 DEG C, 1300 DEG C, 500 DEG C to mixing bunker 3, heating cabinet 5, cooling storehouse 6 respectively, reaches target After temperature, thermocouple temperature sensor I 14, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22 are anti-by temperature PLC controller of feeding 12, after PLC controller 12 receives temperature information, adjust microwave generator 4, to mixing bunker 3, heating cabinet 5, Cooling storehouse 6 is kept the temperature;
(3) mixed-powder of step (1) is poured into the storehouse 1 that feeds intake, enters mixing along the blade of spiral agitator 2 from storehouse 1 is fed intake Storehouse 3, after mixed-powder is sufficiently agitated mixing preheating 18 minutes in mixing bunker 3, PLC controller 12 closes spiral agitator 2 Motor 16, stop stirring, open electromagnetic door I 17, after material enters in heating cabinet 5, turn off electromagnetic door I 17, material is adding In hot storehouse 5 1300 DEG C heat preservation 18 minutes after, PLC controller 12 open electromagnetic door II 23, material enter cooling storehouse 6, PLC controller 12 close electromagnetic doors II 23, and for material after temperature is down to 500 DEG C in cooling storehouse 6, PLC controller 12 opens outlet valve 9, material edge Discharge nozzle 7 be included in into cooling bath 8 it is cooling after obtain WC-10Ni-ZrO2Hard alloy;
After the material in mixing bunker 3 enters in heating cabinet 5, new mixed-powder is entered in mixing bunker 3, the object in heating cabinet 5 Material heats after terminating to enter to cool down in storehouse 6, after the material in mixing bunker 3 enters in heating cabinet 5, realizes continuous preparation.
The present embodiment discharge nozzle 7 can also connect forging press etc. according to actual needs, forge into the shape knot of needs while hot Structure.
It is 98.2% according to the relative density that the method for embodiment 2 measures alloy sample, fracture toughness 9.87MPam1 /2, vickers hardness hv reaches 1601MPa, bending strength reaches 497.3MPa.
Embodiment 4
A kind of continuous preparation WC-10Ni-ZrO of progress2The method of hard alloy, using the device of embodiment 1, specific steps are such as Under:
(1) by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, WC in mixed-powder The mass percentage content of powder is 89.5%;The mass percentage content of Ni powder is 10%, ZrO2The mass percent of particle Content is 0.5%, and the sum of three is 100%;WC powder granularity is 6 μm ~ 9 μm, and Ni powder size is 10 μm ~ 13 μm, ZrO2 Grain granularity is 20nm ~ 25nm;WC powder purity is greater than 99.6%, Ni powder size purity and is greater than 99.91%, ZrO2Particle purity is big In 99.02%;Ball milling is wet-milling, and medium is water, ball milling one hour;
(2) electromagnetic door I 17, electromagnetic door II 23 are opened, venthole 10 is closed, in venthole 13 to mixing bunker 3, heating cabinet 5, cooling It is vacuumized in storehouse 6, when air gauge 15 shows that vacuum degree is lower than 100Pa, stops vacuumizing, venthole 10 is opened, to mixing bunker 3, heating cabinet 5, cooling are passed through protective gas, protective atmosphere N in storehouse 62And H2It is N according to volume ratio2: H2=85:15 mixing Mixed gas, ventilation ten minutes later, vacuumize again, and after so recycling three times, mixing bunker 3, heating cabinet 5, cooling are full of in storehouse 6 Protective gas closes venthole 10 and venthole 13, by adjusting microwave generator 4, makes microwave waveguide I 18, microwave waveguide II 19, microwave waveguide III 20 is heated to 300 DEG C, 1400 DEG C, 600 DEG C to mixing bunker 3, heating cabinet 5, cooling storehouse 6 respectively, reaches target After temperature, thermocouple temperature sensor I 14, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22 are anti-by temperature PLC controller of feeding 12, after PLC controller 12 receives temperature information, adjust microwave generator 4, to mixing bunker 3, heating cabinet 5, Cooling storehouse 6 is kept the temperature;
(3) mixed-powder of step (1) is poured into the storehouse 1 that feeds intake, enters mixing along the blade of spiral agitator 2 from storehouse 1 is fed intake Storehouse 3, after mixed-powder is sufficiently agitated mixing preheating 16 minutes in mixing bunker 3, PLC controller 12 closes spiral agitator 2 Motor 16, stop stirring, open electromagnetic door I 17, after material enters in heating cabinet 5, turn off electromagnetic door I 17, material is adding In hot storehouse 5 1400 DEG C heat preservation 16 minutes after, PLC controller 12 open electromagnetic door II 23, material enter cooling storehouse 6, PLC controller 12 close electromagnetic doors II 23, and for material after temperature is down to 600 DEG C in cooling storehouse 6, PLC controller 12 opens outlet valve 9, material edge Discharge nozzle 7 be included in into cooling bath 8 it is cooling after obtain WC-10Ni-ZrO2Hard alloy;
After the material in mixing bunker 3 enters in heating cabinet 5, new mixed-powder is entered in mixing bunker 3, the object in heating cabinet 5 Material heats after terminating to enter to cool down in storehouse 6, after the material in mixing bunker 3 enters in heating cabinet 5, realizes continuous preparation.
The present embodiment discharge nozzle 7 can also connect forging press etc. according to actual needs, forge into the shape knot of needs while hot Structure.
It is 98.8% according to the relative density that the method for embodiment 2 measures alloy sample, fracture toughness 12.75MPa m1/2, vickers hardness hv reaches 1825MPa, bending strength reaches 899.5MPa.
Embodiment 5
A kind of continuous preparation WC-10Ni-ZrO of progress2The method of hard alloy, using the device of embodiment 1, specific steps are such as Under:
(1) by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, WC in mixed-powder The mass percentage content of powder is 89.25%;The mass percentage content of Ni powder is 10%, ZrO2The mass percent of particle Content is 0.75%, and the sum of three is 100%;WC powder granularity is 6 μm ~ 9 μm, and Ni powder size is 10 μm ~ 13 μm, ZrO2 Grain granularity is 20nm ~ 25nm;WC powder purity is greater than 99.6%, Ni powder size purity and is greater than 99.91%, ZrO2Particle purity is big In 99.02%;Ball milling is wet-milling, and medium is water, ball milling one hour;
(2) electromagnetic door I 17, electromagnetic door II 23 are opened, venthole 10 is closed, in venthole 13 to mixing bunker 3, heating cabinet 5, cooling It is vacuumized in storehouse 6, when air gauge 15 shows that vacuum degree is lower than 100Pa, stops vacuumizing, venthole 10 is opened, to mixing bunker 3, heating cabinet 5, cooling are passed through protective gas, protective atmosphere N in storehouse 62And H2It is N according to volume ratio2: H2=85:15 mixing Mixed gas, ventilation ten minutes later, vacuumize again, and after so recycling three times, mixing bunker 3, heating cabinet 5, cooling are full of in storehouse 6 Protective gas closes venthole 10 and venthole 13, by adjusting microwave generator 4, makes microwave waveguide I 18, microwave waveguide II 19, microwave waveguide III 20 is heated to 300 DEG C, 1500 DEG C, 800 DEG C to mixing bunker 3, heating cabinet 5, cooling storehouse 6 respectively, reaches target After temperature, thermocouple temperature sensor I 14, thermocouple temperature sensor II 21, thermocouple temperature sensor III 22 are anti-by temperature PLC controller of feeding 12, after PLC controller 12 receives temperature information, adjust microwave generator 4, to mixing bunker 3, heating cabinet 5, Cooling storehouse 6 is kept the temperature;
(3) mixed-powder of step (1) is poured into the storehouse 1 that feeds intake, enters mixing along the blade of spiral agitator 2 from storehouse 1 is fed intake Storehouse 3, mixed-powder is sufficiently agitated mixing preheating after ten minutes in mixing bunker 3, and PLC controller 12 closes spiral agitator 2 Motor 16, stop stirring, open electromagnetic door I 17, after material enters in heating cabinet 5, turn off electromagnetic door I 17, material is adding After ten minutes, PLC controller 12 opens electromagnetic door II 23 for 1500 DEG C of heat preservations in hot storehouse 5, and material enters cooling storehouse 6, PLC controller 12 close electromagnetic doors II 23, and for material after temperature is down to 800 DEG C in cooling storehouse 6, PLC controller 12 opens outlet valve 9, material edge Discharge nozzle 7 be included in into cooling bath 8 it is cooling after obtain WC-10Ni-ZrO2Hard alloy;
After the material in mixing bunker 3 enters in heating cabinet 5, new mixed-powder is entered in mixing bunker 3, the object in heating cabinet 5 Material heats after terminating to enter to cool down in storehouse 6, after the material in mixing bunker 3 enters in heating cabinet 5, realizes continuous preparation.
The present embodiment discharge nozzle 7 can also connect forging press etc. according to actual needs, forge into the shape knot of needs while hot Structure.
It is 98.6% according to the relative density that the method for embodiment 2 measures alloy sample, fracture toughness 11.15MPa m1/2, vickers hardness hv reaches 1631MPa, bending strength reaches 897.5MPa.

Claims (9)

1. a kind of continuous preparation WC-10Ni-ZrO2The method of hard alloy, which comprises the following steps:
(1) by WC powder, ZrO2Particle and Ni powder ball milling are uniformly mixed so as to obtain WC-10Ni-ZrO2Mixed-powder, WC in mixed-powder The mass percentage content of powder is 89.00 ~ 89.75%;The mass percentage content of Ni powder is 10%, ZrO2The quality of particle Degree is 0.25 ~ 1.00%;
(2) by the mixed-powder of step (1) under protective atmosphere, cooling obtains WC-10Ni- after carrying out contiguous segmentation microwave heating ZrO2Hard alloy.
2. continuously preparing WC-10Ni-ZrO according to claim 12The method of hard alloy, which is characterized in that step (1) WC Powder size is 6 μm ~ 9 μm, and Ni powder size is 10 μm ~ 13 μm, ZrO2Grain graininess is 20nm ~ 25nm.
3. continuously preparing WC-10Ni-ZrO according to claim 12The method of hard alloy, which is characterized in that step (1) WC Powder purity is greater than 99.6%, Ni powder purity and is greater than 99.91%, ZrO2Particle purity is greater than 99.02%.
4. continuously preparing WC-10Ni-ZrO according to claim 12The method of hard alloy, which is characterized in that step (2) is protected Shield atmosphere is N2And H2It is N according to volume ratio2: H2The mixed gas of=85:15 mixing.
5. continuously preparing WC-10Ni-ZrO according to claim 12The method of hard alloy, which is characterized in that step (2) is even Continuous segmentation microwave heating comprises the concrete steps that: stir 10 ~ 20 minutes for 300 DEG C first in mixing bunker, then 1200 in heating cabinet ~ 1500 DEG C keep the temperature 10 ~ 20 minutes, finally 400 ~ 800 DEG C of coolings in cooling storehouse;After material enters heating cabinet from mixing bunker, new Material puts into mixing bunker, and after material enters cooling storehouse from heating cabinet, the material of mixing bunker enters heating cabinet again, realizes and continuously makes It is standby.
6. claim 1 continuously prepares WC-10Ni-ZrO2The device of hard alloy, which is characterized in that including the storehouse that feeds intake (1), spiral shell Revolve blender (2), mixing bunker (3), microwave generator (4), heating cabinet (5), cooling storehouse (6), discharge nozzle (7), cooling bath (8), Outlet valve (9), venthole (10), insulating layer (11), venthole (13), thermocouple temperature sensor I (14), air gauge (15), Motor (16), electromagnetic door I (17), microwave waveguide I (18), microwave waveguide II (19), microwave waveguide III (20), electric thermo-couple temperature pass Sensor II (21), thermocouple temperature sensor III (22), electromagnetic door II (23);It feeds intake and connect at the top of storehouse (1) and mixing bunker (3), Spiral agitator (2) are equipped in mixing bunker (3), spiral agitator (2) is connect with motor (16), and mixing bunker is additionally provided with out on (3) Stomata (13), thermocouple temperature sensor I (14), air gauge (15), mixing bunker (3) are connect with heating cabinet (5), mixing bunker (3) Electromagnetic door I (17) is equipped between heating cabinet (5), mixing bunker (3) side is equipped with thermocouple temperature sensor II (21), mixing bunker (3) it is connect with cooling storehouse (6), electromagnetic door II (23) is equipped between mixing bunker (3) and cooling storehouse (6), cooling storehouse (6) side is equipped with Venthole (10), thermocouple temperature sensor III (22), cooling storehouse (6) are connect by discharge nozzle (7) with cooling bath (8), are discharged It manages (7) and is equipped with outlet valve (9);
Mixing bunker (3), heating cabinet (5), cooling storehouse (6) are external equipped with insulating layer (11), and microwave waveguide I (18) passes through insulating layer (11) setting is external in the storehouse that feeds intake (1), and microwave waveguide II (19) passes through insulating layer (11) and, microwave external in heating cabinet (5) is arranged Waveguide III (20) passes through insulating layer (11) and is arranged in cooling storehouse (6) outside;Microwave waveguide I (18), microwave waveguide II (19), microwave Waveguide III (20) is connect with microwave generator (4) respectively.
7. continuously preparing WC-10Ni-ZrO according to claim 62The device of hard alloy, which is characterized in that further include PLC Controller (12), microwave generator (4), outlet valve (9), thermocouple temperature sensor I (14), motor (16), electromagnetic door I (17), thermocouple temperature sensor II (21), thermocouple temperature sensor III (22), electromagnetic door II (23) are controlled with PLC respectively Device (12) connection.
8. continuously preparing WC-10Ni-ZrO according to claim 62The device of hard alloy, which is characterized in that described to feed intake Storehouse (1), heating cabinet (5), cool down storehouse (6) cross section be regular pentagon.
9. continuously preparing WC-10Ni-ZrO according to claim 62The device of hard alloy, which is characterized in that described to feed intake Storehouse (1) entrance is located in spiral agitator (2) blade outer radii.
CN201910711968.8A 2019-08-02 2019-08-02 Method and device for continuously preparing WC-10Ni-ZrO2 hard alloy Active CN110396631B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910711968.8A CN110396631B (en) 2019-08-02 2019-08-02 Method and device for continuously preparing WC-10Ni-ZrO2 hard alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910711968.8A CN110396631B (en) 2019-08-02 2019-08-02 Method and device for continuously preparing WC-10Ni-ZrO2 hard alloy

Publications (2)

Publication Number Publication Date
CN110396631A true CN110396631A (en) 2019-11-01
CN110396631B CN110396631B (en) 2021-04-23

Family

ID=68327361

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910711968.8A Active CN110396631B (en) 2019-08-02 2019-08-02 Method and device for continuously preparing WC-10Ni-ZrO2 hard alloy

Country Status (1)

Country Link
CN (1) CN110396631B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114517269A (en) * 2021-12-29 2022-05-20 蓬莱市超硬复合材料有限公司 Tungsten carbide alloy material, preparation method and equipment

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5871303A (en) * 1981-10-21 1983-04-28 Tatsuro Kuratomi Production of tungstem carbide tool material
CN1718790A (en) * 2005-07-22 2006-01-11 株洲硬质合金集团有限公司 Method of preparing cobalt oxide by microwave calcining cobalt salt and it powder material microwave calcining furnace
CN103695685A (en) * 2013-12-26 2014-04-02 昆明理工大学 Method for preparing WC-Co hard alloy in microwave reaction sintering way

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5871303A (en) * 1981-10-21 1983-04-28 Tatsuro Kuratomi Production of tungstem carbide tool material
CN1718790A (en) * 2005-07-22 2006-01-11 株洲硬质合金集团有限公司 Method of preparing cobalt oxide by microwave calcining cobalt salt and it powder material microwave calcining furnace
CN103695685A (en) * 2013-12-26 2014-04-02 昆明理工大学 Method for preparing WC-Co hard alloy in microwave reaction sintering way

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
贾佐诚: "以镍代钴碳化钨基硬质合金的发展", 《粉末冶金工业》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114517269A (en) * 2021-12-29 2022-05-20 蓬莱市超硬复合材料有限公司 Tungsten carbide alloy material, preparation method and equipment
CN114517269B (en) * 2021-12-29 2024-03-19 蓬莱市超硬复合材料有限公司 Tungsten carbide alloy material, preparation method and equipment

Also Published As

Publication number Publication date
CN110396631B (en) 2021-04-23

Similar Documents

Publication Publication Date Title
CN101603132B (en) Method and device for producing vanadium-nitrogen alloy
CN101985717B (en) Method for preparing high-tenacity super-coarse-grained tungsten and cobalt hard alloy
CN104294072B (en) A kind of fast preparation method of gradient hard alloy/cermet
CN105522137B (en) A kind of cermet complex and preparation method thereof
CN107937799B (en) A kind of burr cylinder jacket of centrifugal casting and preparation method thereof
CN105272260B (en) A kind of soap-free emulsion polymeization phase tungsten carbide composite and preparation method thereof
CN102628138A (en) Trace cobalt-containing tungsten carbide without bonding phase and preparation method thereof
CN106498205A (en) A kind of manufacture method of the CuCr alloys of large scale high-compactness high uniformity
CN103045925A (en) Preparation process of sputtered rotary molybdenum-sodium-alloy tubular target
CN105478777A (en) Metal/ceramic gradient material and preparation method thereof
CN102140603A (en) Hard alloy using nickel-aluminum intermetallic compound Ni3Al as bonding phase and preparation method thereof
CN107523710A (en) A kind of whisker modified Ti (C, N) based composite metal ceramic preparation of resistance to high temperature oxidation
CN105950897B (en) A kind of preparation method of copper-based neutron absorber material
CN107142388A (en) A kind of preparation method of Ti 13Nb 13Zr alloys
CN110144481A (en) A kind of high strength at high temperature height leads wear-resistant copper based composites and preparation method thereof
CN104308161A (en) Preparation method of low-cost boron carbide/aluminum composite board
CN107571472A (en) The wear-resisting manufacture of casing of organic-inorganic nano powder graded composite and its application
CN105219992B (en) Method for preparing AlV 55 intermediate alloy
CN110396631A (en) A kind of continuous method and device for preparing WC-10Ni-ZrO2 hard alloy
CN105014062A (en) Powder warm-compaction near-net molded molybdenum-based rare earth alloy top and manufacturing technology thereof
CN114703394A (en) High-temperature material and preparation method and application thereof
CN105986139B (en) A kind of titanium carbide ceramic and preparation method thereof
CN111778436B (en) Method for preparing WC-Y2O3 binderless hard alloy by cold pressing-hot pressing sintering
CN109014220A (en) A kind of the circulation hydrogenation and dehydrogenization Preparation equipment and method of hypoxemia metal powder
CN100357180C (en) Method of microwave synthetizing nano powder of tungsten carbide

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