CN108516843B - Microwave sintering method and multi-gas microwave sintering furnace - Google Patents

Microwave sintering method and multi-gas microwave sintering furnace Download PDF

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Publication number
CN108516843B
CN108516843B CN201810598069.7A CN201810598069A CN108516843B CN 108516843 B CN108516843 B CN 108516843B CN 201810598069 A CN201810598069 A CN 201810598069A CN 108516843 B CN108516843 B CN 108516843B
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furnace
sleeve body
wedge block
locking
locking wedge
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CN108516843A (en
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胡俊旭
刘辉汉
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Zhuzhou Jurunhe Microwave Industrial Furnace Co ltd
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Zhuzhou Jurunhe Microwave Industrial Furnace Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/003Apparatus, e.g. furnaces
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5626Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on tungsten carbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638Removal thereof
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06Details, accessories, or equipment peculiar to furnaces of these types
    • F27B5/14Arrangements of heating devices
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D1/00Casings; Linings; Walls; Roofs
    • F27D1/18Door frames; Doors, lids, removable covers
    • F27D1/1858Doors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1054Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/667Sintering using wave energy, e.g. microwave sintering
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27MINDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
    • F27M2003/00Type of treatment of the charge
    • F27M2003/04Sintering
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention discloses a microwave sintering method and a multi-gas microwave sintering furnace, wherein the microwave sintering method is to directly heat a blank material prepared from a tungsten carbide mixture with an organic binder by microwaves, and improve the dielectric constant of the blank material by utilizing the mutual coordination of the microwaves, the organic binder in the blank material and carbon elements in the blank material, thereby improving the wave absorbing capacity of the blank material and enabling the temperature in the sintering furnace to be quickly increased for sintering. The invention can raise temperature rapidly, does not need to additionally increase a heating body for preheating, shortens the production time, reduces the production cost and improves the production efficiency.

Description

Microwave sintering method and multi-gas microwave sintering furnace
Technical Field
The invention relates to a sintering method and a sintering furnace, in particular to a microwave sintering method and a multi-gas microwave sintering furnace.
Background
Sintering refers to the transformation of a powdery material into a dense body, and is a traditional technological process. This process has long been used to produce ceramics, powder metallurgy (e.g., cemented carbide), refractory materials, ultra-high temperature materials, and the like. In general, after the powder is molded, a compact obtained by sintering is a polycrystalline material whose microstructure is composed of crystals, glass bodies and pores. The sintering process directly affects the grain size, pore size, and grain boundary shape and distribution in the microstructure, thereby affecting the properties of the material.
The microwave sintering is a new method for sintering materials by utilizing microwave heating, and is different from the traditional heating mode, and the microwave sintering has the characteristics of high heating speed, high energy utilization rate, high heating efficiency, safety, sanitation, no pollution and the like, can improve the uniformity and the yield of products, improve the production efficiency, shorten the production time and shorten a plurality of production periods to a certain extent.
The existing microwave sintering process generally comprises the steps of firstly preparing powdery materials, adding an organic adhesive (such as paraffin, alcohol or a mixture of paraffin and alcohol) to obtain a mixture, then pressing the mixture to obtain a blank, drying to separate the organic adhesive, and finally sintering. However, in the sintering, the temperature is often raised slowly, and it is necessary to preheat by a separate heating element, and after the temperature is raised to a certain level, the sintering can be performed by microwaves. Thus, the production time is prolonged, the production efficiency is reduced, and the production cost is increased.
The Chinese invention patent with publication number of CN107774993A and publication date of 2018, 3 month and 9 days discloses a preparation method of a hard alloy furnace end, which comprises the following steps: 1) 6.0-13.2 wt% of cobalt and 86.3-93.5 wt% of tungsten carbide, wherein the average grain size of the hard alloy is 0.6-1.0 mu m, the structure is uniform, the hardness is HRA91.5-93.0, the bending strength is 3000-4500Mpa, the fracture toughness value is 9-15 MPam1/2, and the WC/Co composite powder is used as a raw material for stirring and ball milling for 13-20 hours to obtain a mixture; 2) Pressing; 3) Dewaxing; 4) And (5) sintering at low pressure.
The Chinese invention patent with publication number of CN107287460A and publication date of 2017, 10 month and 24 days discloses a preparation method of hard alloy, which comprises the following steps: 1) Respectively dissolving WC powder, co powder, rare earth and alkaline earth into a liquid-phase dispersion medium, pouring into a mixing barrel, and uniformly mixing to obtain a mixture; 2) Ball milling the mixture in a ball mill for 36-40h, vacuum drying at 100 ℃, adding slurry, stirring, drying, sieving with a sieve, and preparing into granules; 3) And pressing, forming and dewaxing the material particles, and then sintering in vacuum at 1200-1300 ℃ to obtain the hard alloy.
In the above patent documents, dewaxing is performed first and then sintering is performed, so that the problems of long production time, low production efficiency, high production cost and the like are caused.
In summary, how to design a microwave sintering method and a multi-gas microwave sintering furnace, so that the temperature of the microwave sintering method and the multi-gas microwave sintering furnace can be quickly increased, a heating body is not required to be additionally added for preheating, the production time is shortened, the production cost is reduced, and the production efficiency is improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a microwave sintering method and a multi-gas microwave sintering furnace, which can rapidly heat up without additionally adding a heating body for preheating, thereby shortening the production time, reducing the production cost and improving the production efficiency.
In order to solve the technical problems, the invention adopts the following technical scheme: a microwave sintering method is characterized in that a blank material piece prepared from a tungsten carbide mixture with an organic binder is directly heated by microwaves, and the dielectric constant of the blank material piece is improved by utilizing the mutual coordination of the microwaves, the organic binder in the blank material piece and carbon elements in the blank material piece, so that the wave absorbing capacity of the blank material piece is improved, and the temperature in a sintering furnace is rapidly increased to sinter.
Preferably, the microwave source is communicated with the sintering furnace through a waveguide tube, the vacuum source is communicated with the sintering furnace through a vacuum pipeline, and a drainage tube is arranged at the bottom of the sintering furnace;
the microwave sintering method comprises the following specific steps:
1) Placing a blank piece prepared from the tungsten carbide mixture with the organic binder into a sintering furnace;
2) Starting a microwave source, enabling part of the organic adhesive in the blank material to flow out through the drainage tube, and simultaneously enabling the interior of the sintering furnace to be quickly heated by utilizing the mutual coordination of the microwaves, the organic adhesive in the blank material and carbon elements in the blank material;
3) Observing the temperature in the sintering furnace, when the temperature in the sintering furnace rises to a higher temperature, the dielectric constant and the wave absorbing capacity of the blank piece reach a higher value, the organic adhesive in the blank piece is completely vaporized, and the vaporized organic adhesive is sucked out through a vacuum pipeline;
4) And continuously heating by interaction of microwaves and blank materials with higher dielectric constants and higher wave absorption capacities, observing the temperature in the sintering furnace, keeping the constant temperature in the sintering furnace for a period of time when the temperature in the sintering furnace rises to the sintering temperature, and then turning off the microwave source to cool the temperature in the sintering furnace to normal temperature to finish sintering.
Preferably, the sintering furnace is further provided with an air inlet pipe, and air is filled into the sintering furnace through the air inlet pipe so as to ensure the positive pressure state in the sintering furnace.
The invention also discloses a multi-gas microwave sintering furnace for sintering according to the microwave sintering method, which comprises a furnace body, a waveguide tube arranged on the top of the furnace body, and a vacuum pipeline arranged on the side part of the furnace body, wherein one end of the vacuum pipeline is connected with a vacuum source through a valve I, the other end of the vacuum pipeline is communicated with the inside of the furnace body, one end of the waveguide tube is connected with the microwave source, the other end of the waveguide tube is communicated with the inside of the furnace body, and a drainage tube with a valve II is further arranged at the bottom of the furnace body.
Preferably, one end of the waveguide tube is connected with a microwave source, and the other end of the waveguide tube is communicated with the inside of the furnace body through a joint tube; and a glass partition plate is arranged between the waveguide tube and the joint tube, and the inner cavity of the waveguide tube is separated from the inner cavity of the joint tube by the glass partition plate.
Preferably, the joint pipe is in a truncated cone shape, the small end of the truncated cone-shaped joint pipe is close to one side of the waveguide tube, and the large end of the truncated cone-shaped joint pipe is close to one side of the furnace body.
Preferably, the furnace body comprises a round cylinder with one end closed and the other end open and a furnace door arranged on the open end of the round cylinder; the round cylinder body is horizontally arranged, the other end of the vacuum pipeline is connected to the closed end of the round cylinder body, and a locking mechanism for locking the furnace door on the open end of the round cylinder body is further arranged between the furnace door and the open end of the round cylinder body.
Preferably, the locking mechanism comprises a locking wedge block I and a pressing sleeve body; the first locking wedge block is fixedly connected to the periphery of the opening end of the circular cylinder body, and the compressing sleeve body comprises a sleeve body, a second locking wedge block arranged on one end of the sleeve body and a pressing block arranged on the other end of the sleeve body; when in locking, the rotating sleeve body drives the sleeve body to move through the matching of the locking wedge block I and the locking wedge block II, so that the furnace door is pressed on the opening end of the circular cylinder body by utilizing the pressing block on the sleeve body; when the door is unlocked, the sleeve body is reversely rotated through the matching of the first locking wedge block and the second locking wedge block, so that the pressing block on the sleeve body is loosened to press the door.
Preferably, the first locking wedge block and the second locking wedge block each comprise an annular body and a plurality of wedge-shaped blocks which are sequentially arranged on one side part of the annular body along the circumferential direction of the annular body; the inclined surfaces of the plurality of wedge blocks in the locking wedge block I are matched and contacted with the inclined surfaces of the plurality of wedge blocks in the locking wedge block II, and when the locking wedge block I is locked, the rotating sleeve body drives the sleeve body to axially move along the sleeve body through the matching of the inclined surfaces of the plurality of wedge blocks in the locking wedge block I and the inclined surfaces of the plurality of wedge blocks in the locking wedge block II, so that the furnace door is pressed on the opening end of the circular cylinder body by utilizing the pressing block on the sleeve body; when the furnace door is in the unlocking state, the sleeve body is reversely moved along the axial direction of the sleeve body by the combination of the plurality of wedge blocks in the locking wedge block I and the plurality of wedge blocks in the locking wedge block II, so that the pressing block on the sleeve body is loosened to press the furnace door.
Preferably, a plurality of pressing blocks are arranged, and the pressing blocks are sequentially arranged at the other end of the sleeve body along the circumferential direction of the sleeve body; the furnace door is round, and a plurality of protruding blocks are sequentially arranged on the periphery of the round furnace door along the circumferential direction of the round furnace door; when in locking, the pressing blocks on the pressing sleeve body are respectively contacted with the convex blocks on the furnace door, so that the furnace door is pressed on the opening end of the round cylinder body.
The invention has the beneficial effects that: the invention uses the mutual cooperation of the organic adhesive, carbon element and microwave in the blank in the early stage of sintering to rapidly raise the temperature in the early stage of sintering furnace, rapidly raise the dielectric constant and wave absorbing capacity of the blank to a higher value to complete the auxiliary heating function, and then uses the continuous action of the carbon element in the tungsten carbide blank with stronger wave absorbing capacity to reach the sintering temperature to complete sintering. Therefore, the invention can rapidly and uniformly heat from inside to outside without additionally adding a heating body for preheating, shortens the production time, reduces the production cost and improves the production efficiency. The sintering furnace is also provided with an air inlet pipe, and air is filled into the sintering furnace through the air inlet pipe so as to ensure that the positive pressure state in the sintering furnace is ensured, so that the air pressure in the sintering furnace is larger than the external atmospheric pressure, and the external oxygen is ensured not to enter the sintering furnace, so that the mixture in the sintering furnace is ensured not to be oxidized by the oxygen. By arranging the glass partition plate between the waveguide tube and the joint tube, arranging the joint tube in a truncated cone shape and arranging the small end of the truncated cone shape joint tube close to one side of the waveguide tube, arranging the large end of the truncated cone shape joint tube close to one side of the furnace body and arranging the furnace body into a round cylinder body and arranging the furnace body horizontally, the invention can control the constant temperature field of microwaves at a hearth in the furnace body, namely, the mixture in the hearth can be uniformly heated and sintered in the environment of the constant temperature field, thereby further improving the quality of products. Through setting up locking mechanism, can realize locking and unblock fast to the furnace gate, further improve work efficiency.
Drawings
FIG. 1 is a schematic view showing a three-dimensional structure of a microwave sintering furnace according to an embodiment of the present invention;
FIG. 2 is a schematic view of a partially cut-away perspective structure of a microwave sintering furnace according to an embodiment of the present invention;
FIG. 3 is a schematic view of a partial perspective view of the joint tube of FIG. 2;
FIG. 4 is a schematic axial sectional view of a furnace body according to an embodiment of the present invention;
FIG. 5 is an enlarged schematic view of the portion A in FIG. 4;
FIG. 6 is a schematic view of a partial perspective view of the locking mechanism of FIG. 2;
FIG. 7 is a schematic diagram of the principle structure of the first locking wedge and the second locking wedge cooperating with each other in the embodiment of the present invention;
FIG. 8 is a schematic perspective view of a second locking wedge in an embodiment of the present invention;
FIG. 9 is a schematic view of a partial perspective view of the oven door of FIG. 2;
in the figure: 1. furnace body, 111, circular cylinder, 112, furnace door, 113, lug, 2, waveguide tube, 3, vacuum pipeline, 4, drainage tube, 5, support frame, 6, heat insulation layer, 7, furnace chamber, 8, joint pipe, 9, glass partition, 10, top connecting pipe, 11, condensing tower, 12, locking wedge I, 13, sleeve, 14, locking wedge II, 15, briquetting, 16, annular body, 17, wedge block, K1. through hole I, K2. through hole II.
Detailed Description
The technical scheme of the invention is further elaborated below with reference to the drawings and specific embodiments.
Examples: a microwave sintering method is characterized in that a blank material piece prepared from a tungsten carbide mixture with an organic binder is directly heated by microwaves, and the dielectric constant of the blank material piece is improved by utilizing the mutual coordination of the microwaves, the organic binder in the blank material piece and carbon elements in the blank material piece, so that the wave absorbing capacity of the blank material piece is improved, and nonmetallic friction is carried out, so that the temperature in a sintering furnace is quickly increased for sintering.
The applicant has found through long-term experiments and research analysis that in the existing resistance heating and microwave heating technologies, the organic adhesive is separated from the mixture (such as dewaxing) before sintering, when the microwave is started to heat the mixture, the dielectric constant of the mixture is low at normal temperature, and the wave absorbing capacity of the mixture is weak, so that the temperature in the sintering furnace is slow to raise, and more than ten hours are needed to raise the temperature. Therefore, in the prior art, it is necessary to raise the temperature in the furnace by the heating element before the main sintering by microwaves. In the embodiment, the blank material prepared by the tungsten carbide mixture with the organic adhesive is directly subjected to multi-gas integral sintering, and due to the existence of the organic adhesive, hydrocarbon in the organic adhesive can absorb microwaves and simultaneously absorb microwaves by utilizing carbon elements in the blank material, so that the dielectric constant of the blank material can be improved, the wave absorbing capacity of the blank material is improved, the temperature in the furnace in the early stage of the sintering furnace is quickly increased, the organic adhesive is vaporized and separated from the blank material in the heating process, and after the organic adhesive is completely vaporized, the temperature in the furnace reaches a higher value at the moment, and the dielectric constant and the wave absorbing capacity of the blank material also reach a higher value, therefore, the auxiliary heating of the organic adhesive is not needed at the moment, and the temperature in the furnace can reach the sintering temperature directly through the continuous action of the microwaves and the carbon elements in the blank material, so that the sintering process is completed. In the embodiment, the organic adhesive, carbon elements and microwaves in the tungsten carbide blank piece are used for mutual interaction in the early sintering stage, the early temperature in a sintering furnace is rapidly increased, the dielectric constant and the wave absorbing capacity of the blank piece are rapidly increased to a higher value, the auxiliary heating effect is completed, and then the microwaves and the carbon elements in the tungsten carbide blank piece with higher wave absorbing capacity are used for continuing to act so as to reach the sintering temperature to complete sintering. Therefore, the invention can quickly and evenly heat from inside to outside without additionally adding a heating body for preheating, shortens the production time, reduces the production cost and improves the quality and the production efficiency of the product. In this embodiment, the microwave source generally employs a frequency of 245MHz to 915 MHz.
The microwave source is communicated with the sintering furnace through a waveguide tube, the vacuum source is communicated with the sintering furnace through a vacuum pipeline, a drainage tube is arranged at the bottom of the sintering furnace, and the drainage tube is connected with a storage tube to store the flowing liquid;
the microwave sintering method comprises the following specific steps:
1) Placing a blank piece prepared from the tungsten carbide mixture with the organic binder into a sintering furnace;
2) Starting a microwave source, wherein part of the organic adhesive flows out of the blank material in the early temperature rising process, and part of the organic adhesive flows out of the blank material through a drainage tube, and meanwhile, the interior of the sintering furnace is quickly heated by utilizing the mutual coordination of microwaves, the organic adhesive in the blank material and carbon elements in the blank material;
3) Observing the temperature in the sintering furnace, when the temperature in the sintering furnace rises to a higher temperature (700-850 ℃), the dielectric constant and the wave absorbing capacity of the blank material reach higher values, the organic adhesive in the blank material is completely vaporized, and then the vaporized organic adhesive is sucked out through a vacuum pipeline;
4) And continuously heating by interaction of microwaves and nonmetallic carbon in the blank material piece with higher dielectric constant and higher wave absorbing capacity, observing the temperature in the sintering furnace, keeping the constant temperature in the sintering furnace for a period of time (0.5 to 1 hour) when the temperature in the sintering furnace rises to the sintering temperature (1350 to 1400 ℃), and then turning off the microwave source to cool the temperature in the sintering furnace to normal temperature to finish sintering.
The sintering furnace is also provided with an air inlet pipe, and air is filled into the sintering furnace through the air inlet pipe so as to ensure the positive pressure state in the sintering furnace. Therefore, the air pressure in the sintering furnace is larger than the external atmospheric pressure, and the external oxygen is prevented from entering the sintering furnace, so that the mixture in the sintering furnace is prevented from being oxidized by the oxygen.
As shown in fig. 1 and 2, the present embodiment also discloses a multi-gas microwave sintering furnace for sintering according to the microwave sintering method described above, comprising a furnace body 1, the microwave sintering furnace further comprising a waveguide 2 provided on the top of the furnace body 1 and a vacuum pipe 3 provided on the side of the furnace body 1, one end of the vacuum pipe 3 being connected to a vacuum source (not shown in the drawing) through a valve one, the other end of the vacuum pipe 3 being in communication with the inside of the furnace body 1, one end of the waveguide 2 being connected to a microwave source (not shown in the drawing), the other end of the waveguide 2 being in communication with the inside of the furnace body 1, and a drain tube 4 having a valve two (not shown in the drawing) being further provided at the bottom of the furnace body 1.
The microwave sintering method comprises the following specific steps:
1) Placing the mixture with the organic adhesive into the furnace body 1;
2) Starting a microwave source, closing a valve I, and starting a valve II so that part of the organic adhesive flows out through the drainage tube 4;
3) Observing the temperature in the furnace, when the temperature in the furnace rises to 700-850 ℃, closing the valve II, and opening the valve I to suck out the vaporized organic adhesive by the vacuum pipeline 3;
4) And continuously heating by microwaves, observing the temperature in the furnace, keeping the constant temperature in the furnace for 0.5 to 1 hour when the temperature in the furnace rises to 1350 to 1400 ℃, and then turning off the microwave source to cool the furnace to the normal temperature to finish sintering.
The furnace comprises a furnace body 1, a supporting frame 5, a furnace chamber 7 with a heat preservation layer 6 arranged on the supporting frame 5, and a mixture after compression molding is placed in the furnace chamber 7 for sintering. The heat-insulating layer can be made of heat-insulating cotton, and the hearth is made of corundum material. The side parts of the heat preservation layer and the hearth are provided with a first through hole K1, and the bottoms of the heat preservation layer and the hearth are provided with a second through hole K2.
As shown in fig. 3, one end of the waveguide 2 is connected to a microwave source (not shown in the figure), and the other end of the waveguide 2 is communicated with the inside of the furnace body 1 through a joint pipe 8; a glass partition 9 is further provided between the waveguide 2 and the joint pipe 8, and the inner cavity of the waveguide 2 and the inner cavity of the joint pipe 8 are partitioned by the glass partition 9. Thus being beneficial to the diffusion of microwave and ensuring the uniformity of microwave diffusion. In this embodiment, the glass separator is made of quartz glass. The waveguide 2 is a square tube, and the top connection tube 10 connected to the joint tube 8 and provided on the top of the furnace body 1 is a round tube, so that the joint tube 8 is a square-round joint tube, i.e., one end connected to the waveguide 2 is square, and one end connected to the top connection tube 10 is round.
The joint pipe 8 is in a truncated cone shape, the small end of the truncated cone-shaped joint pipe 8 is close to one side of the waveguide pipe 2, and the large end of the truncated cone-shaped joint pipe 8 is close to one side of the furnace body 1.
As shown in fig. 2, the furnace body 1 is also provided as a circular cylinder and the furnace body 1 is horizontally provided, and it should be noted that in this embodiment, by providing the glass partition 9 between the waveguide tube 2 and the joint tube 8, and providing the joint tube 8 with a truncated cone shape and the small end of the truncated cone shape joint tube 8 near the waveguide tube 2, the large end of the truncated cone shape joint tube 8 near the furnace body 1 and providing the furnace body 1 as a circular cylinder and the furnace body 1 is horizontally provided, the constant temperature field of the microwave can be controlled at the furnace chamber 7 in the furnace body, that is, the mixture in the furnace chamber 7 can be sintered under the environment of the constant temperature field, thereby further improving the quality of the product.
An intake pipe (not shown) is also provided on the joint pipe 8. During sintering, gas is filled into the sintering furnace through the gas inlet pipe so as to ensure the positive pressure state in the sintering furnace, so that the gas pressure in the sintering furnace is larger than the external atmospheric pressure, and external oxygen is prevented from entering the sintering furnace, and the mixture in the sintering furnace is prevented from being oxidized by the oxygen. In the embodiment, the gas filled in adopts the mixed gas of hydrogen and argon, so that the positive pressure state in the sintering furnace can be ensured, and the complete reducing atmosphere in the sintering furnace can be ensured, thereby further ensuring that the mixture in the sintering furnace is not oxidized by oxygen.
An air inlet of the air inlet pipe is connected with an air source (not shown in the figure), and an air outlet of the air inlet pipe is arranged towards one side of the glass partition plate. During sintering, the vaporized organic adhesive is adhered to the glass partition board, so that the diffusion of the microwave is adversely affected, and the embodiment blows air towards the glass partition board through the air inlet pipe, so that sundries adhered to the glass partition board can be blown clean, and the diffusion of the microwave is further ensured.
As shown in fig. 2 and 4, the furnace body 1 includes a circular cylinder 111 having one end closed and the other end opened, and a furnace door 112 provided on the opened end of the circular cylinder 111; the circular cylinder 111 is horizontally arranged, the other end of the vacuum pipeline 3 is connected to the closed end of the circular cylinder 111, and a locking mechanism for locking the furnace door 112 on the open end of the circular cylinder 111 is arranged between the furnace door 112 and the open end of the circular cylinder 111. A condensing tower 11 is also arranged on the vacuum pipeline 3, and one end of the vacuum pipeline 3 is communicated with a vacuum source through the condensing tower.
As shown in fig. 4 to 6, the locking mechanism comprises a locking wedge block one 12 and a pressing sleeve body 13; the first locking wedge block 12 is fixedly connected to the outer periphery of the opening end of the circular cylinder 111, the pressing sleeve body comprises a sleeve body 13, a second locking wedge block 14 arranged on one end of the sleeve body 13 and a pressing block 15 arranged on the other end of the sleeve body 13, and the pressing block 15 and the sleeve body 13 are of an integrated structure; during locking, the rotating sleeve body 13 drives the sleeve body 13 to move through the matching of the locking wedge block I12 and the locking wedge block II 14, so that the furnace door 112 is pressed on the opening end of the circular cylinder 111 by the pressing block 15 on the sleeve body 13; when unlocking, the sleeve body 13 is reversely rotated, and the sleeve body 13 is driven to reversely move by matching the locking wedge block I12 with the locking wedge block II 14, so that the pressing block 15 on the sleeve body is released to press the furnace door. Through setting up locking mechanism, can realize locking and unblock fast to the furnace gate, further improve work efficiency.
As shown in fig. 7 and 8, the first locking wedge 12 and the second locking wedge 13 each comprise an annular body 16 and a plurality of wedge blocks 17 sequentially arranged on one side of the annular body 16 along the circumferential direction of the annular body, and the annular body 16 and the wedge blocks 17 are of an integral structure; the inclined surfaces of the plurality of wedge blocks 17 in the first locking wedge block 12 are matched and contacted with the inclined surfaces of the plurality of wedge blocks 17 in the second locking wedge block 14, and when the locking is performed, the rotating sleeve body drives the sleeve body to axially move along the sleeve body through the matching of the inclined surfaces of the plurality of wedge blocks 17 in the first locking wedge block 12 and the inclined surfaces of the plurality of wedge blocks 17 in the second locking wedge block 14, so that the furnace door 112 is pressed on the opening end of the circular cylinder 111 by the pressing block 15 on the sleeve body; when the sleeve body is loosened, the sleeve body is driven to move reversely along the axial direction of the sleeve body by matching the inclined planes of the wedge blocks 17 in the first locking wedge block 12 and the inclined planes of the wedge blocks 17 in the second locking wedge block 14, so that the pressing block 15 on the sleeve body loosens the pressing of the furnace door 112.
As shown in fig. 9, a plurality of pressing blocks 15 are provided, and the plurality of pressing blocks 15 are sequentially provided on the other end of the sleeve 13 along the circumferential direction of the sleeve 13; the furnace door 112 is circular, and a plurality of protruding blocks 113 are sequentially arranged on the periphery of the circular furnace door 112 along the circumferential direction of the circular furnace door 112, so that the furnace door 112 is gear-shaped, and when the furnace door is locked, a plurality of pressing blocks 15 on the pressing sleeve body are respectively contacted with the plurality of protruding blocks 113 on the furnace door, so that the furnace door 112 is pressed on the opening end of the circular cylinder 111. When the furnace door is unlocked, after the pressing blocks are loosened by reversely rotating the sleeve body, the furnace door is rotated, each protruding block 113 on the furnace door 112 is located at a gap B (in a state shown in fig. 9) between two adjacent pressing blocks 15, and then the furnace door is axially taken out along the sleeve body, so that the problem of mutual collision interference between the protruding blocks and the pressing blocks when the furnace door is taken out can be avoided, and the furnace door can be taken out smoothly.
In summary, the invention utilizes the interaction of the organic adhesive, the carbon element and the microwave in the blank piece in the early sintering stage to rapidly raise the temperature in the early sintering furnace, rapidly raise the dielectric constant and the wave absorbing capacity of the blank piece to a higher value to complete the auxiliary heating effect, and then utilizes the continuous action of the carbon element in the tungsten carbide blank piece with stronger wave absorbing capacity to reach the sintering temperature to complete the sintering. Therefore, the invention can rapidly and uniformly heat from inside to outside without additionally adding a heating body for preheating, shortens the production time, reduces the production cost and improves the production efficiency. The sintering furnace is also provided with an air inlet pipe, and air is filled into the sintering furnace through the air inlet pipe so as to ensure that the positive pressure state in the sintering furnace is ensured, so that the air pressure in the sintering furnace is larger than the external atmospheric pressure, and the external oxygen is ensured not to enter the sintering furnace, so that the mixture in the sintering furnace is ensured not to be oxidized by the oxygen. By arranging the glass partition plate between the waveguide tube and the joint tube, arranging the joint tube in a truncated cone shape and arranging the small end of the truncated cone shape joint tube close to one side of the waveguide tube, arranging the large end of the truncated cone shape joint tube close to one side of the furnace body and arranging the furnace body into a round cylinder body and arranging the furnace body horizontally, the invention can control the constant temperature field of microwaves at a hearth in the furnace body, namely, the mixture in the hearth can be uniformly heated and sintered in the environment of the constant temperature field, thereby further improving the quality of products. Through setting up locking mechanism, can realize locking and unblock fast to the furnace gate, further improve work efficiency.
The term "plurality" as used in this embodiment means the number of "two or more". The above embodiments are only for illustrating the present invention, not for limiting the present invention, and various changes and modifications may be made by one skilled in the relevant art without departing from the spirit and scope of the present invention, so that all equivalent technical solutions shall fall within the scope of the present invention, which is defined by the claims.

Claims (5)

1. The utility model provides a many atmospheres microwave sintering stove, includes furnace body, its characterized in that: the multi-atmosphere microwave sintering furnace further comprises a waveguide tube arranged on the top of the furnace body and a vacuum pipeline arranged on the side part of the furnace body, one end of the vacuum pipeline is connected with a vacuum source through a valve I, the other end of the vacuum pipeline is communicated with the inside of the furnace body, one end of the waveguide tube is connected with a microwave source, the other end of the waveguide tube is communicated with the inside of the furnace body, and a drainage tube with a valve II is further arranged at the bottom of the furnace body;
the furnace body comprises a round cylinder body with one end closed and the other end open and a furnace door arranged on the open end of the round cylinder body; the circular cylinder body is horizontally arranged, the other end of the vacuum pipeline is connected to the closed end of the circular cylinder body, and a locking mechanism for locking the furnace door on the open end of the circular cylinder body is further arranged between the furnace door and the open end of the circular cylinder body;
the locking mechanism comprises a locking wedge block I and a pressing sleeve body; the first locking wedge block is fixedly connected to the periphery of the opening end of the circular cylinder body, and the compressing sleeve body comprises a sleeve body, a second locking wedge block arranged on one end of the sleeve body and a pressing block arranged on the other end of the sleeve body; when in locking, the rotating sleeve body drives the sleeve body to move through the matching of the locking wedge block I and the locking wedge block II, so that the furnace door is pressed on the opening end of the circular cylinder body by utilizing the pressing block on the sleeve body; when the door is unlocked, the sleeve body is reversely rotated through the matching of the first locking wedge block and the second locking wedge block, so that the pressing block on the sleeve body is loosened to press the door.
2. The multi-atmosphere microwave sintering furnace according to claim 1, wherein: one end of the waveguide tube is connected with a microwave source, and the other end of the waveguide tube is communicated with the inside of the furnace body through a joint tube; and a glass partition plate is arranged between the waveguide tube and the joint tube, and the inner cavity of the waveguide tube is separated from the inner cavity of the joint tube by the glass partition plate.
3. The multi-atmosphere microwave sintering furnace according to claim 2, wherein: the joint pipe is in a truncated cone shape, the small end of the truncated cone-shaped joint pipe is close to one side of the waveguide tube, and the large end of the truncated cone-shaped joint pipe is close to one side of the furnace body.
4. The multi-atmosphere microwave sintering furnace according to claim 1, wherein: the first locking wedge block and the second locking wedge block comprise an annular body and a plurality of wedge blocks which are sequentially arranged on one side part of the annular body along the circumferential direction of the annular body; the inclined surfaces of the plurality of wedge blocks in the locking wedge block I are matched and contacted with the inclined surfaces of the plurality of wedge blocks in the locking wedge block II, and when the locking wedge block I is locked, the rotating sleeve body drives the sleeve body to axially move along the sleeve body through the matching of the inclined surfaces of the plurality of wedge blocks in the locking wedge block I and the inclined surfaces of the plurality of wedge blocks in the locking wedge block II, so that the furnace door is pressed on the opening end of the circular cylinder body by utilizing the pressing block on the sleeve body; when the furnace door is in the unlocking state, the sleeve body is reversely moved along the axial direction of the sleeve body by the combination of the plurality of wedge blocks in the locking wedge block I and the plurality of wedge blocks in the locking wedge block II, so that the pressing block on the sleeve body is loosened to press the furnace door.
5. The multi-atmosphere microwave sintering furnace according to claim 4, wherein: the pressing blocks are arranged in a plurality, and the pressing blocks are sequentially arranged at the other end of the sleeve body along the circumferential direction of the sleeve body; the furnace door is round, and a plurality of protruding blocks are sequentially arranged on the periphery of the round furnace door along the circumferential direction of the round furnace door; when in locking, the pressing blocks on the pressing sleeve body are respectively contacted with the convex blocks on the furnace door, so that the furnace door is pressed on the opening end of the round cylinder body.
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