CN111970778A - Method and device for microwave high-flux sintering of powder block - Google Patents
Method and device for microwave high-flux sintering of powder block Download PDFInfo
- Publication number
- CN111970778A CN111970778A CN202010862162.1A CN202010862162A CN111970778A CN 111970778 A CN111970778 A CN 111970778A CN 202010862162 A CN202010862162 A CN 202010862162A CN 111970778 A CN111970778 A CN 111970778A
- Authority
- CN
- China
- Prior art keywords
- microwave
- flux
- powder
- cavity
- sintering
- 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
Links
- 239000000843 powder Substances 0.000 title claims abstract description 56
- 238000005245 sintering Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 47
- 239000000945 filler Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 238000012856 packing Methods 0.000 claims description 16
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 239000003575 carbonaceous material Substances 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 9
- 230000004907 flux Effects 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000004044 response Effects 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 239000006249 magnetic particle Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002070 nanowire Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 12
- 238000004663 powder metallurgy Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 2
- 238000010353 genetic engineering Methods 0.000 abstract description 2
- 238000013537 high throughput screening Methods 0.000 abstract 1
- 239000012761 high-performance material Substances 0.000 abstract 1
- 238000004886 process control Methods 0.000 abstract 1
- 238000012937 correction Methods 0.000 description 16
- 238000011049 filling Methods 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 238000009529 body temperature measurement Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 238000012216 screening Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000012925 reference material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000011088 calibration curve 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
- 238000000748 compression moulding Methods 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/64—Heating using microwaves
- H05B6/6408—Supports or covers specially adapted for use in microwave heating apparatus
- H05B6/6411—Supports or covers specially adapted for use in microwave heating apparatus the supports being rotated
-
- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/64—Heating using microwaves
- H05B6/6426—Aspects relating to the exterior of the microwave heating apparatus, e.g. metal casing, power cord
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/64—Heating using microwaves
- H05B6/6432—Aspects relating to testing or detecting leakage in a microwave heating apparatus
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/64—Heating using microwaves
- H05B6/6447—Method of operation or details of the microwave heating apparatus related to the use of detectors or sensors
- H05B6/645—Method of operation or details of the microwave heating apparatus related to the use of detectors or sensors using temperature sensors
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/64—Heating using microwaves
- H05B6/6447—Method of operation or details of the microwave heating apparatus related to the use of detectors or sensors
- H05B6/645—Method of operation or details of the microwave heating apparatus related to the use of detectors or sensors using temperature sensors
- H05B6/6455—Method of operation or details of the microwave heating apparatus related to the use of detectors or sensors using temperature sensors the sensors being infrared detectors
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/64—Heating using microwaves
- H05B6/80—Apparatus for specific applications
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Optics & Photonics (AREA)
- Powder Metallurgy (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a method and a device for sintering a powder block in a microwave high-flux manner, belonging to the field of powder metallurgy material preparation and high-flux material genetic engineering.A pre-pressed powder material block is added into a device cavity filled with a filler, and then the device cavity is vacuumized or filled with protective gas or reducing gas for microwave heating to obtain a high-flux block material; the invention can realize instantaneous high temperature of the material, has high temperature rise process control precision, is safe and environment-friendly, can realize high-throughput preparation and performance improvement of the material, is beneficial to design and development or high-throughput screening of the material, and simultaneously provides a new way for preparation of high-performance materials.
Description
Technical Field
The invention relates to a method and a device for sintering a powder block by microwave high flux, belonging to the field of high flux material preparation.
Background
If the powder metallurgy material can realize the rapid powder sintering and simultaneously ensure the sufficient densification, the powder metallurgy material can refine grains particularly aiming at ceramic powder, and improve the mechanical properties of the material, such as hardness, strength, toughness and the like. Therefore, the sintering process of the powder compact is accurately controlled, and the powder metallurgy product with excellent comprehensive performance can be obtained by realizing the rapid high-temperature sintering of the powder. In addition, the preparation method of the high-flux material has obvious advantages in developing new materials and optimizing new processes, can effectively accelerate the research and development-application process of the material, and is the most important research means of material genetic engineering. The invention combines the characteristics of high-flux preparation, microwave heating and the carbon nano material, realizes the high-flux preparation of the powder metallurgy material under the advantages of rapid and efficient wave absorption and rapid response of the carbon nano material under a microwave heating field, and provides an important research means and development tool for material research and development.
Disclosure of Invention
The invention adopts a heating mode of microwave radiation, utilizes the characteristic that the nano-carbon substrate efficiently absorbs microwaves, places the powder pressed compact to be sintered in the nano-carbon substrate filler under a microwave field, fully utilizes the characteristics of instantaneous response and rapid heat dissipation of the nano-carbon substrate, accurately controls the sintering process of the powder pressed compact, provides a method and a research approach for high-flux preparation of powder metallurgy materials, and simultaneously, the prepared material has good mechanical and functional characteristics because the densification of the powder pressed compact is rapidly and accurately realized.
The invention provides a method for sintering a powder block by microwave high flux, which comprises the following specific steps:
adding the pre-pressed powder material block into a device cavity filled with the filler, vacuumizing or introducing protective gas or reducing gas, and performing microwave heating to obtain the high-flux block material.
The powder material block is a ceramic powder block and/or a metal powder block.
The filler is a nano carbon-based material with extremely strong wave absorption or a composite powder taking the nano carbon-based material as a carrier and loading nano magnetic particles and wave-absorbing ceramic particles, and the nano carbon-based material comprises an industrial grade or high-purity carbon nano tube, graphene, a carbon nano wire, a carbon quantum dot, C60 and the like; the nano magnetic particles are Fe, Co, Ni, Fe3O4The wave-absorbing ceramic particles are SiC, AlN and the like; the wave absorbing capacity of the filler is 1-2 orders of magnitude higher than that of the traditional filler, and the sintering temperature rise speed, the sintering temperature and the heat preservation time can be accurately controlled by utilizing the instantaneous response characteristic of the filler to a microwave source, and meanwhile, the heat preservation time is prolongedThe characteristics of no thermal inertia and cold and heat sources of microwave heating are utilized, so that the rapid cooling of the sample can be realized, and the rapid preparation of the material and the high-flux screening of the material are facilitated.
The mass ratio of the powder material blocks to the filler is not more than 1: 1.
The vacuum degree of the vacuumizing is less than or equal to 1 Pa; the protective gas is inert atmosphere such as nitrogen, argon, helium, neon and the like; the reducing gas is hydrogen, carbon monoxide or other reducing gas, or a mixed gas of hydrogen, carbon monoxide and inert gas in any proportion.
The frequency of the microwave heating is 300MHz-300GHz, and the power density of the microwave is 0.1mw/cm2-100w/cm2The microwave power can be accurately regulated and controlled, the regulation and control precision is 0.01mw, and the microwave heating time is more than 10 s.
The invention also provides a device for sintering the powder block in a microwave high-flux manner, which comprises a microwave generator 1, a filler cavity 2, a microwave cavity 3, a high-flux channel 6, a heat insulation layer 7, a sample support table 8, an infrared thermometer 11 and a central channel 12; a plurality of microwave generators 1 are arranged outside a microwave cavity 3, a packing cavity 2 is arranged in the microwave cavity 3, the inside of the packing cavity 2 is divided into a central channel 12 and a plurality of high-flux channels 6 which are arranged at the center by a heat insulation layer 7, a plurality of holes are arranged at the top of the microwave cavity 3, the induction end of an infrared thermometer 11 passes through the holes and just faces the inside of the central channel 12 and the high-flux channels 6, and a sample support stand 8 is arranged in the high-flux channels 6 and the central channel 12.
The device still includes rotation axis 4, revolving stage 13, motor 14, and 2 bottoms in packing chamber set up revolving stage 13, set up rotation axis 4 below revolving stage 13, and the output that is connected with motor 14 after the 3 bottoms of microwave cavity are passed to the 4 other ends of rotation axis, and motor 14 rotates and drives rotation axis 4 and rotate, and rotation axis 4 drives revolving stage 13 and rotates, and revolving stage 13 drives packing chamber 2 and rotates, and infrared thermometer 11 carries out intermittent type formula temperature measurement according to the rotational speed in packing chamber 2 this moment.
The device still includes rotation axis 4, revolving stage 13, motor 14, and 3 bottoms in microwave cavity set up revolving stage 13, set up rotation axis 4 below revolving stage 13, and rotation axis 4 is connected with motor 14's output, and motor 14 rotates the back and drives rotation axis 4 and rotate, and rotation axis 4 drives revolving stage 13 and rotates, and revolving stage 13 drives microwave cavity 3 and rotates, and infrared thermometer 11 also follows microwave cavity 3 to rotate, and infrared thermometer 11 measures the temperature in real time.
A thermocouple 5 is arranged in the central channel 12; temperature correcting devices 10 are arranged in the high-flux channel 6 and the central channel 12, and the temperature correcting devices 10 are temperature measuring rings, temperature measuring cones, temperature measuring hammers and the like and are used for correcting temperature.
The invention has the beneficial effects that:
according to the invention, the nano carbon-based material with extremely strong wave absorption is used as a filler, and is mixed with the ceramic powder block and/or the metal powder block with extremely weak wave absorption, and the sintering temperature of the sample is controlled through the strength of the wave absorption, so that the sample is distributed according to a certain gradient.
The invention fully utilizes the strong wave absorption of the nano carbon-based material, which is 1-2 orders of magnitude higher than the traditional graphite, is commonly used as a wave-absorbing invisible material, also utilizes the transient response characteristic to a microwave source, can accurately control the sintering temperature rise speed, the sintering temperature and the heat preservation time, simultaneously utilizes the characteristics of no thermal inertia and zero heat source of microwave heating, can realize the rapid temperature reduction of a sample, and is beneficial to the rapid preparation of the material and the high-flux screening of the material.
Each sample channel is provided with an independent heating and heat-insulating cavity, the heating and heat-insulating cavities are not interfered with each other, the middle of the sample channel is provided with a space design and a heat-insulating layer to reduce or avoid the mutual interference, and the sample channel is provided with an independent temperature measuring system which is tested by a thermocouple, an infrared thermometer and a temperature correcting device of a traditional heat conduction temperature sensor and respectively represents the surface temperature and the internal temperature of the filler of the sample.
The invention adopts a heating mode of microwave radiation, utilizes the characteristic that the nano carbon-based material efficiently absorbs microwaves, places the powder pressed compact to be sintered in the nano carbon-based material filler under a microwave field, fully utilizes the characteristics of instantaneous response and rapid heat dissipation of the nano carbon-based material, accurately controls the sintering process of the powder pressed compact, and provides a method and a research way for high-flux preparation of powder metallurgy materials. Meanwhile, the densification of the powder compact is rapidly and accurately realized, so that the prepared material has good mechanical and functional characteristics.
Drawings
FIG. 1 is a schematic structural view of an apparatus according to example 1 of the present invention;
FIG. 2 is a side view of a packing chamber of example 1 of the present invention;
FIG. 3 is a top view of a packing chamber of example 1 of the present invention;
FIG. 4 is a side view of a high-throughput channel of example 1 of the present invention;
FIG. 5 is a graph of the hardness of the sintered material of example 5 of the present invention;
in the figure, 1-a microwave generator; 2-a packing chamber; 3-microwave cavity; 4-a rotating shaft; 5-a thermocouple; 6-high-throughput channel; 7-a heat insulation layer; 8-sample holder stage; 9-sintering the sample; 10-a temperature correcting device; 11-an infrared thermometer; 12-a central channel; 13-rotating table; 14-motor.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
A device for sintering powder blocks in a microwave high-flux mode is shown in figures 1, 2, 3 and 4 and comprises a microwave generator 1, a filling cavity 2, a microwave cavity 3, a rotating shaft 4, a thermocouple 5, a high-flux channel 6, a heat insulation layer 7, a sample support table 8, a temperature correction device 10, an infrared thermometer 11, a central channel 12, a rotating table 13 and a motor 14; a plurality of microwave generators 1 are arranged outside a microwave cavity 3, an infrared thermometer 11 is arranged at the top of the microwave cavity 3, a packing cavity 2 is arranged in the microwave cavity 3, the inside of the packing cavity 2 is divided into a central channel 12 at the central position and 8 high-flux channels 6 by a heat-insulating layer 7, the central channel 12 is the high-flux channel at the central position, materials which are the same as the high-flux channels 6 can be placed in the central channel 12 or only reference materials can be placed in the central channel, a plurality of holes are arranged at the top of the microwave cavity 3, the induction end of the infrared thermometer 11 passes through the holes and just faces the inside of the central channel 12 and the high-flux channels 6, a rotating platform 13 is arranged at the bottom of the packing cavity 2, a rotating shaft 4 is arranged below the rotating platform 13, the rotating shaft 4 is connected with the output end of a motor 14, the motor 14 drives the rotating shaft 4 to rotate, the rotating platform 4 drives the rotating, a thermocouple 5, a sample support platform 8 and a temperature correcting device 10 are arranged in the central channel 12, the sample support platform 8 is arranged in the high-flux channel 6, and a sintered sample 9 is placed on the sample support platform 8; the temperature correcting device 10 is a temperature measuring ring, a temperature measuring cone, a temperature measuring hammer and the like and is used for correcting temperature.
When a sample is placed in the central passage 12, a sample holder stage 8 is placed in the central passage 12.
Example 2
A device for sintering powder blocks in a microwave high-flux mode comprises a microwave generator 1, a filling cavity 2, a microwave cavity 3, a rotating shaft 4, a thermocouple 5, a high-flux channel 6, a heat insulation layer 7, a sample support table 8, a temperature correction device 10, an infrared thermometer 11, a central channel 12, a rotating table 13 and a motor 14; a plurality of microwave generators 1 are arranged outside a microwave cavity 3, an infrared thermometer 11 is arranged at the top of the microwave cavity 3, a packing cavity 2 is arranged in the microwave cavity 3, the inside of the packing cavity 2 is divided into a central channel 12 and 8 high-flux channels 6 at the central position by a heat-insulating layer 7, the central channel 12 is the high-flux channel at the central position, materials which are the same as the high-flux channels 6 can be placed in the central channel 12, only reference materials can be placed in the reference channels, a plurality of holes are arranged at the top of the microwave cavity 3, the induction end of the infrared thermometer 11 passes through the holes and just faces the inside of the central channel 12 and the high-flux channels 6, a rotary table 13 is arranged at the bottom of the microwave cavity 3, a rotary shaft 4 is arranged below the rotary table 13, the rotary shaft 4 is connected with the output end of a motor 14, the motor, the infrared thermometer 11 also rotates along with the microwave cavity 3, the infrared thermometer 11 measures temperature in real time, a thermocouple 5, a sample support stand 8 and a temperature correcting device 10 are arranged in the central channel 12, a sample support stand 8 is arranged in the high-flux channel 6, and a sintered sample 9 is placed on the sample support stand 8; the temperature correcting device 10 is a temperature measuring ring, a temperature measuring cone, a temperature measuring hammer and the like and is used for correcting temperature.
When a sample is placed in the central passage 12, a sample holder stage 8 is placed in the central passage 12.
Example 3
The thermocouple 5, the temperature correcting device 10 and the infrared thermometer 11 in the embodiments 1 and 2 form a temperature measuring system of the device, and the temperature measuring system is corrected by the specific method:
before use, the filling material is put into the central channel 12 and the high-flux channel 6 of the filling cavity 2, the powder material block of the pressed compact sample is not put in the filling material, a thermocouple 5 and a temperature correcting device 10 are placed in the central channel 12, a microwave source is turned on to start recording the temperature rising process of the thermocouple 5 and the infrared thermometer 11, the temperature of the infrared thermometer 11 is taken as a reference, at least 3 times of repeated heating processes are carried out, the heating processes are respectively heated to 3 different temperature points, the temperature of the thermocouple 5 is corrected by taking the temperature of the temperature correcting device 10 at each time as a reference, and simultaneously a relation curve between the thermocouple 5 and the infrared thermometer 11 is established, i.e., the temperature calibration curve, in short, the thermocouple 5 is calibrated by the temperature of the temperature calibration device 10, then, correcting the temperature of the infrared thermometer 11 by taking the temperature of the thermocouple 5 as a reference, and finally taking the temperature measured by the infrared thermometer 11 as a controlled temperature parameter during actual sintering; and (3) recording the temperature of the central thermocouple 5 and the temperature of the infrared thermometer 11 of each channel when sintering or normal production is started, correcting the temperature of the infrared thermometer 11 through a temperature correction curve to obtain the actual sintering temperature, and taking out the temperature correction device 10 after correction.
When the temperature correction device 10 is provided in both the high-flux passage 6 and the center passage 12, the respective passages can be temperature-corrected.
Example 4
The device of example 1 was used to perform microwave high flux sintering of powder blocks, the specific steps were as follows:
(1) weighing 120g of electrolytic copper powder, dividing the electrolytic copper powder into 12 equal parts, 10g of each sample, and then carrying out die forming under the pressure of 80MPa to obtain 12 cylindrical samples with the diameter of 20mm under corresponding pressure conditions;
(2) temperature correction, using carbon nanotube (Fe) loaded with nano ferroferric oxide3O4@CNT，Fe3O415%) and alumina as filler, wherein 1 to 6#Cavity bodyFe of medium filler3O4The @ CNT contents are respectively: 100%, 80%, 60%, 40%, 20% and 0%, the balance being alumina, the central channel 12 being 1#A cavity, and 5 high-flux channels 6 are randomly selected to be 2-6#Filling the filling materials into each cavity in sequence, then opening the microwave generator 1, recording the relationship between the temperature of the infrared thermometer 11, the temperature correcting device 10 and the temperature measured by the thermocouple 5 and the time and the microwave power, and drawing a temperature correcting curve according to the method of the embodiment 3;
(3) putting 12 cylindrical samples in a group of two samples in 1-6#On a sample support table 8 in the cavity, the mass ratio of the powder material block to the filler is 1:5, the filler is placed in the high-flux channel 6 except the sample support table 8, and the filler covers the sample completely;
(4) introducing nitrogen as a protective atmosphere, opening the microwave generator 1, controlling the microwave power, opening the motor 14 to rotate the rotating shaft 4, driving the rotating shaft 4 to rotate the rotating table 13, driving the filling cavity 2 to rotate by the rotating table 13, carrying out intermittent temperature measurement by the infrared thermometer 11 according to the rotating speed of the filling cavity 2 at the moment, taking the temperature in the central channel 12 as a main reference, recording the temperature change of all channels fed back by the infrared thermometer 11 along with the time, and when the microwave input power is 100w/cm2，1-6#The heating rates of the cavities are respectively 112 ℃/s, 94 ℃/s, 71 ℃/s, 42 ℃/s, 23 ℃/s and 5 ℃/s, the microwave heating time is 10s, at the moment, because the heating time is short, the heat conduction is not balanced yet, the reaction of the thermocouple 5 is slow, the temperature measured by the thermocouple 5 is slightly lower than the temperature measured by the infrared thermometer 11, the actual temperature is the temperature measured by the infrared thermometer 11 and is obtained by correcting the temperature through the temperature correction curve of the step (2), and the heating rate is 1 ℃ which is the fastest#When the actual temperature of the cavity reaches 900 ℃, the microwave generator 1 is closed, the cavity is cooled along with the furnace, a sample is taken out after 30min, and density test is carried out, and 1-6#The relative densities of the samples were: 99.2%, 97.1%, 89.5%, 77.7%, 65.9% and 58.6%, which are the corresponding relative densities at different temperatures, respectively, so that the method and the device provided by the invention can provide important reference basis for optimizing and regulating the process of the sample.
Example 5
The high-flux channel 6 of the embodiment 2 is cut into ten cavities including the central channel 12, the rest is the same as the embodiment 1, the device is adopted to carry out microwave high-flux sintering on the powder block, and the specific steps are as follows:
(1) acidizing the pre-purchased CNT, and then performing ball milling on the CNT and copper powder with different mass fractions for 5 hours to obtain CNT/Cu composite powder, wherein the mass fractions of the CNT in the CNT/Cu are respectively as follows: 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 10 groups of samples in total, each sample is 10g, the composite powder is subjected to compression molding under the pressure of 60MPa, and each sample is obtained into two cylindrical samples with the diameter of 20mm under corresponding pressure conditions;
(2) temperature correction, namely adopting mixed powder consisting of graphene (Co @ GR) loaded with nano cobalt particles and silicon dioxide powder as a filler, wherein the content of the Co @ GR in the filler is 80%, and the central channel 12 is 1#The other 9 high-flux channels 6 of the cavity are 2-10#Filling the filling materials into each cavity in sequence, then opening the microwave generator 1, recording the relation between the temperature measurement and correction devices 10 of the infrared thermometer 11 and the temperature measurement of the thermocouple 5 and the time and the microwave power, and drawing a temperature correction curve according to the method of the embodiment 3;
(3) putting two 20 cylindrical samples into a group on a sample support table 8 in ten cavities, wherein the mass ratio of the powder material block to the filler is 1:10, putting the filler in the high-flux channel 6 except the sample support table 8, and completely covering the samples by the filler;
(4) vacuumizing until the vacuum degree is less than 1Pa, opening a microwave generator 1, controlling the microwave power, opening a motor 14 to rotate a rotating shaft 4, driving the rotating shaft 4 to rotate a rotating platform 13, driving a microwave cavity 3 to rotate the rotating platform 13, driving an infrared thermometer 11 to rotate along with the microwave cavity 3, measuring the temperature of the infrared thermometer 11 in real time, taking the temperature in a central channel 12 as a main reference, recording the change of the temperature of all cavities fed back by the infrared thermometer 11 along with the time, and when the microwave input power is 20w/cm2Microwave, microwaveThe heating time is 20s, and the temperature rise is the fastest 1#The temperature rise rate of the cavity is 151 ℃/s, and the temperature rise rates of the other cavities are between 136 ℃ and 152 ℃, when 1#When the actual temperature of the cavity reaches 900 ℃, reducing the microwave power, wherein the actual temperature is the temperature measured by the infrared thermometer 11 and obtained by correcting the temperature through the temperature correction curve in the step (2), keeping the temperature for 2 minutes, then closing the microwave generator 1, cooling along with the furnace, taking out a sample after 50 minutes, testing the mechanical properties, and finding that the temperature is 1-10 DEG C#The hardness of the samples is shown in fig. 5, where the hardness of the 5# and 6# samples is the highest, respectively: 88.3 and 86.9HV, respectively, corresponding to hardness at different temperatures, it can be seen that optimization and design screening of the components of the sample by the method and apparatus of the invention is feasible and the efficiency of material preparation and screening can be improved.
Example 6
The high-flux channel 6 of the embodiment 1 is cut into ten cavities including the central channel 12, the rest is the same as the embodiment 1, the device is adopted to carry out microwave high-flux sintering on the powder block, and the specific steps are as follows:
(1) firstly, preparing alumina powders with different component characteristics (wherein the granularity of the alumina powders of samples No. 1-5 is 80nm, 300nm, 800nm, 5 μm and 12 μm respectively, the granularity of the alumina powders of samples No. 1-5 is added with 1wt% of stearic acid, the granularity of the alumina powders of samples No. 6-10 is 5 microns, the adding amount of the stearic acid is 0.5wt%, 1.5wt%, 2.0wt%, 2.5wt% and 3.0wt%, dividing each of the ceramic powders into two equal parts, and then carrying out die pressing under the pressure of 50MPa to obtain 20 cylindrical samples with the diameter of 15 mm;
(2) temperature correction, using industrial carbon nanotubes as filler, a central channel 12 of 1#The other 9 high-flux channels 6 of the cavity are 2-10#Filling the filling materials into each cavity in sequence, then opening the microwave generator 1, recording the relation between the temperature measurement and correction devices 10 of the infrared thermometer 11 and the temperature measurement of the thermocouple 5 and the time and the microwave power, and drawing a temperature correction curve according to the method of the embodiment 3;
(3) putting two 20 cylindrical samples into a group on a sample support table 8 in ten cavities, wherein the mass ratio of the powder material block to the filler is 1:1, putting the filler in the high-flux channel 6 except the sample support table 8, and completely covering the samples by the filler;
(4) introducing mixed gas of nitrogen and hydrogen (volume ratio is 4: 1) as sintering atmosphere, opening a microwave generator 1, controlling microwave power, opening a motor 14 to rotate a rotating shaft 4, driving the rotating shaft 4 to rotate a rotating table 13, driving a filling cavity 2 to rotate by the rotating table 13, carrying out intermittent temperature measurement by an infrared thermometer 11 according to the rotating speed of the filling cavity 2, taking the temperature in a central channel 12 as a main reference, recording the temperature change of all cavities fed back by the infrared thermometer 11 along with time, and when the microwave input power is 0.1/cm2The microwave heating time is 1000s, and the temperature rise is the fastest 1#The temperature rise rate of the cavity is 280-#When the actual temperature of the cavity reaches 1500 ℃, the actual temperature is the temperature measured by the infrared thermometer 11 and is obtained by correcting the temperature through the temperature correction curve in the step (2), the microwave generator 1 is closed, furnace cooling is carried out, the sample is taken out after 100min, and density testing is carried out, so that the relative density of alumina with the average particle size of 12 microns can reach 97 percent, and the relative densities are corresponding to the relative densities at different temperatures respectively.
Claims (10)
1. A method for sintering powder blocks by microwaves at high flux is characterized by comprising the following specific steps:
adding the pre-pressed powder material block into a device cavity filled with the filler, vacuumizing or introducing protective gas or reducing gas, and performing microwave heating to obtain the high-flux block material.
2. The microwave high-throughput sintering powder block according to claim 1, wherein the powder material block is a ceramic powder block and/or a metal powder block.
3. According to claimThe method for sintering the powder block with the microwave high flux is characterized in that the filler is a nano-carbon-based material or composite powder taking the nano-carbon-based material as a carrier and loading nano-magnetic particles or wave-absorbing ceramic particles, the nano-carbon-based material comprises industrial grade or high-purity carbon nano tubes, graphene, carbon nano wires, carbon quantum dots or C60, and the nano-magnetic particles are Fe, Co, Ni or Fe3O4The wave-absorbing ceramic particles are SiC or AlN.
4. The microwave high-throughput sintering powder block of claim 1, wherein the mass ratio of powder material block to filler is not greater than 1: 1.
5. The method for microwave high-throughput sintering of powder blocks according to claim 1, wherein the degree of vacuum of the vacuum is less than or equal to 1 Pa; the protective gas is nitrogen, argon or helium; the reducing gas is hydrogen and carbon monoxide, or a mixed gas of hydrogen, carbon monoxide and inert gas in any proportion.
6. The method of claim 1, wherein the microwave heating frequency is 300MHz-300GHz and the microwave power density is 0.1mw/cm2-100w/cm2The microwave heating time is more than 10 s.
7. The microwave high-flux sintering powder block device of claim 1, characterized by comprising a microwave generator (1), a filler cavity (2), a microwave cavity body (3), a high-flux channel (6), a heat insulation layer (7), a sample support table (8), an infrared thermometer (11) and a central channel (12); microwave cavity (3) are provided with a plurality of microwave generator (1) outward, set up packing chamber (2) in microwave cavity (3), packing chamber (2) inside central channel (12) and a plurality of high flux passageway (6) that are divided into central point and put by insulating layer (7), microwave cavity (3) top is equipped with a plurality of holes, the response end of infrared thermometer (11) is just passing inside central channel (12) and high flux passageway (6), set up sample support platform (8) in high flux passageway (6) and central channel (12).
8. The microwave high-flux powder block sintering device according to claim 7, further comprising a rotating shaft (4), a rotating table (13), and a motor (14), wherein the rotating table (13) is disposed at the bottom of the packing cavity (2), the rotating shaft (4) is disposed below the rotating table (13), and the other end of the rotating shaft (4) penetrates through the bottom of the microwave cavity (3) and is connected to an output end of the motor (14).
9. The microwave high-flux powder block sintering device according to claim 7, further comprising a rotating shaft (4), a rotating table (13) and a motor (14), wherein the rotating table (13) is arranged at the bottom of the microwave cavity (3), the rotating shaft (4) is arranged below the rotating table (13), and the rotating shaft (4) is connected with an output end of the motor (14).
10. The apparatus for microwave high-throughput sintering of powder agglomerates of claim 7, wherein a thermocouple (5) is arranged in the central channel (12); temperature correcting devices (10) are also arranged in the high-flux channel (6) and the central channel (12); the temperature correcting device (10) is a temperature measuring ring, a temperature measuring cone or a temperature measuring hammer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010862162.1A CN111970778B (en) | 2020-08-25 | 2020-08-25 | Method and device for microwave high-flux sintering of powder block |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010862162.1A CN111970778B (en) | 2020-08-25 | 2020-08-25 | Method and device for microwave high-flux sintering of powder block |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111970778A true CN111970778A (en) | 2020-11-20 |
| CN111970778B CN111970778B (en) | 2023-03-17 |
Family
ID=73390385
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010862162.1A Active CN111970778B (en) | 2020-08-25 | 2020-08-25 | Method and device for microwave high-flux sintering of powder block |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111970778B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114986970A (en) * | 2022-05-07 | 2022-09-02 | 昆明理工大学 | High-flux powder pressing control system and high-flux powder pressing method |
| CN115449343A (en) * | 2022-10-17 | 2022-12-09 | 衡阳凯新特种材料科技有限公司 | Silicon nitride wave-absorbing material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020108949A1 (en) * | 2001-01-17 | 2002-08-15 | Penn State Research Foundation | Microwave processing using highly microwave absorbing powdered material layers |
| CN101786165A (en) * | 2009-12-31 | 2010-07-28 | 华中科技大学 | Method for synthesizing Nb/Nb5Si3 composite materials at high temperature through microwave induced self propagating |
| 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 |
| CN108707731A (en) * | 2018-07-23 | 2018-10-26 | 昆明理工大学 | A kind of microwave high throughput prepares the device and method of alloy |
| CN109922555A (en) * | 2019-04-08 | 2019-06-21 | 昆明理工大学 | A kind of chassis Concentric rotation type micro-wave high throughput material handling device |
-
2020
- 2020-08-25 CN CN202010862162.1A patent/CN111970778B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020108949A1 (en) * | 2001-01-17 | 2002-08-15 | Penn State Research Foundation | Microwave processing using highly microwave absorbing powdered material layers |
| CN101786165A (en) * | 2009-12-31 | 2010-07-28 | 华中科技大学 | Method for synthesizing Nb/Nb5Si3 composite materials at high temperature through microwave induced self propagating |
| 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 |
| CN108707731A (en) * | 2018-07-23 | 2018-10-26 | 昆明理工大学 | A kind of microwave high throughput prepares the device and method of alloy |
| CN109922555A (en) * | 2019-04-08 | 2019-06-21 | 昆明理工大学 | A kind of chassis Concentric rotation type micro-wave high throughput material handling device |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114986970A (en) * | 2022-05-07 | 2022-09-02 | 昆明理工大学 | High-flux powder pressing control system and high-flux powder pressing method |
| CN114986970B (en) * | 2022-05-07 | 2023-08-11 | 昆明理工大学 | High-flux powder pressing control system and high-flux powder pressing method |
| CN115449343A (en) * | 2022-10-17 | 2022-12-09 | 衡阳凯新特种材料科技有限公司 | Silicon nitride wave-absorbing material and preparation method thereof |
| CN115449343B (en) * | 2022-10-17 | 2024-01-12 | 衡阳凯新特种材料科技有限公司 | Silicon nitride wave-absorbing material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111970778B (en) | 2023-03-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111970778B (en) | Method and device for microwave high-flux sintering of powder block | |
| CN107557612A (en) | A kind of graphene enhancing titanium-based nano composite and preparation method | |
| CN101786162B (en) | Preparation method of bismuth telluride based bulk nano crystalline thermoelectric material | |
| CN104313380B (en) | A kind of step sintering prepares the method for high-compactness Nanograin Cemented Carbide | |
| JP2019534376A (en) | Control variation of magnetocaloric material parameters | |
| CN102931335B (en) | A kind of Graphene is combined thermoelectric material of cobalt stibide based skutterudite and preparation method thereof | |
| CN109180187B (en) | Preparation method of highly oriented nanometer MAX phase ceramic and MAX phase in-situ authigenic oxide nanometer complex phase ceramic | |
| CN110629061B (en) | Preparation method of aluminum-based composite material with controllable in-situ nano aluminum oxide content | |
| CN202571280U (en) | Mould for discharge plasma sintering equipment | |
| CN106367683B (en) | A kind of lightweight high heat conductance Fe Al based alloys and preparation method thereof | |
| CN106498313A (en) | High-strength high ductility CNTs SiCp reinforced aluminum matrix composites and preparation method thereof | |
| CN206330417U (en) | A kind of ceramic material densification sintering stove of unidirectional oscillation pressure | |
| CN108374198A (en) | A kind of monocrystalline Bi2Te3The preparation method of thermoelectric material | |
| CN102211783A (en) | Method for reducing content of magnetic substances in electrical engineering grade magnesium oxide | |
| CN106898691A (en) | A kind of preparation method of oxygen doping molybdenum bisuphide thermoelectric material | |
| CN111139453B (en) | Preparation method of high-conductivity copper/graphene composite material | |
| CN102925757B (en) | Method for preparing Al-Fe alloy by virtue of nanometre powder | |
| Yan et al. | Tunable band gap of diamond twin boundaries by strain engineering | |
| CN108198934A (en) | A kind of composite thermoelectric material and preparation method thereof | |
| Guo et al. | Relationship between the MgOp/Cu interfacial bonding state and the arc erosion resistance of MgO/Cu composites | |
| CN111515404A (en) | Preparation method of cBN/Al composite material | |
| CN104766717A (en) | Method for improving magnetic property of sintered neodymium-iron-boron permanent magnet | |
| CN113526959B (en) | Method and device for rapidly sintering tungsten carbide powder without adhesive | |
| CN104711444B (en) | A kind of method of quick preparation high-performance SiGe high temperature thermoelectric alloy materials | |
| CN101486564B (en) | Preparation of boron nitride nano tube enhanced alumina ceramic |
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 |