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 PDFInfo
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- 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
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000000956 alloy Substances 0.000 title claims abstract description 51
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 51
- 238000011437 continuous method Methods 0.000 title description 2
- 238000010438 heat treatment Methods 0.000 claims abstract description 87
- 238000001816 cooling Methods 0.000 claims abstract description 86
- 239000000843 powder Substances 0.000 claims abstract description 59
- 239000011812 mixed powder Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 230000001681 protective effect Effects 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 230000011218 segmentation Effects 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 98
- 239000000463 material Substances 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 6
- 235000021050 feed intake Nutrition 0.000 claims description 5
- 235000019628 coolness Nutrition 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- 238000005452 bending Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 238000005242 forging Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000001238 wet grinding Methods 0.000 description 4
- 229910009043 WC-Co Inorganic materials 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- -1 corrosion resistance Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/003—Apparatus, e.g. furnaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- 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)
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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
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.
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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 |
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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 |
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