WO2020124544A1 - 一种真空脱脂烧结炉及其使用方法 - Google Patents

一种真空脱脂烧结炉及其使用方法 Download PDF

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Publication number
WO2020124544A1
WO2020124544A1 PCT/CN2018/122642 CN2018122642W WO2020124544A1 WO 2020124544 A1 WO2020124544 A1 WO 2020124544A1 CN 2018122642 W CN2018122642 W CN 2018122642W WO 2020124544 A1 WO2020124544 A1 WO 2020124544A1
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Prior art keywords
graphite
box
port
material box
sintering
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PCT/CN2018/122642
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English (en)
French (fr)
Inventor
刘鹏
徐文立
胡芳
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宁波恒普真空技术有限公司
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Priority to PCT/CN2018/122642 priority Critical patent/WO2020124544A1/zh
Priority to JP2021536076A priority patent/JP7144617B2/ja
Priority to CN201880020622.7A priority patent/CN110603417B/zh
Publication of WO2020124544A1 publication Critical patent/WO2020124544A1/zh

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    • 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
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • 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
    • B22F3/1017Multiple heating or additional steps
    • B22F3/1021Removal of binder or filler
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B17/00Furnaces of a kind not covered by any preceding group
    • 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
    • Y02P10/10Reduction of greenhouse gas [GHG] emissions
    • Y02P10/143Reduction of greenhouse gas [GHG] emissions of methane [CH4]

Definitions

  • Graphite thermal field vacuum degreasing and sintering furnace is used to degrease and sinter metal powder embryo body.
  • the main components in the furnace are made of carbon fiber and graphite.
  • Graphite has excellent electrical conductivity, super heat resistance, high reliability and Lightweight and easy to process, long life and other advantages, it is one of the main materials of vacuum sintering furnace, but it also has the following problems:
  • Dust influence Graphite and carbon fiber are easy to generate dust. Graphite dust and carbon fiber dust will be brought into the bin with the air flow and attached to the product in the bin. The surface of the product is prone to defects during sintering, and the carbon content of the product is also With the increase, the performance of products with higher requirements made of stainless steel such as 316, 304, 316L, 17-4PH and other materials is reduced.
  • Leakage effect The leakage of the vacuum furnace is unavoidable, but the leakage is controlled at a low level, the air enters from the furnace door and other locations, and it is easy to contact with the sintered product and affect the performance of the product. The amount of leakage in different furnaces is different, resulting in differences between products sintered in different furnaces.
  • FIGS. 1 and 2 The structure of the existing vacuum degreasing and sintering furnace is shown in FIGS. 1 and 2.
  • the material box B1 is connected to the inner suction pipe B2, and the inner suction pipe B2 is connected to the vacuum pump B3.
  • the vacuum pump works, the pressure outside the tank is greater than the pressure inside the tank, the pressure difference promotes the unidirectional flow of gas, the gas outside the tank enters the tank from the gap between the tank door and the tank body, and the gas enters the tank. After passing the surface of the product, enter the inner suction tube B2.
  • the temperature of the heating material B4 is the highest, and the temperature of the outer wall of the bin B1 is increased by radiation.
  • the temperature of the bin is transmitted to the bin B1 on the one hand, and to the graphite column B8 and the graphite cover B9 on the other hand.
  • the temperature of the inner wall of the heat insulation tube B5 is higher, and the temperature of the outer wall is lower, so the temperature of each part in the furnace is different.
  • Thermocouple B6 monitors the temperature of the tank B1.
  • the temperature of the heating material B4 When the temperature of the tank B1 is controlled outside the hydrogen reaction sensitive area, such as 1300 °C, the temperature of the heating material B4 will be higher than 1300 °C, but the temperature near the insulation tube B5 graphite Then, in the hydrogen reaction sensitive area, hydrogen will react with the graphite parts in this temperature range, consuming parts.
  • the degreasing process is also very important for the quality of the product. If the degreasing is not clean, the size of the product will be large during subsequent sintering, the surface will be gray, and the performance will not meet the standard.
  • the scrap rate in the prior art is extremely high, and the only solution is to extend the degreasing time so that the binder in the product is discharged as much as possible.
  • the oxygen in the air reacts with the binder to accelerate the degreasing speed.
  • the main component of the binder is polymer plastics, such as PE, PP, etc. Plastics can be accelerated by adding oxygen at a temperature of about 200 °C.
  • the object of the present invention is to provide a vacuum degreasing and sintering furnace and a method for using the same to solve the above-mentioned problems in the prior art and improve the degreasing and sintering efficiency and product quality.
  • the present invention provides the following solutions:
  • the invention provides a vacuum degreasing and sintering furnace, which includes a furnace body and a carbon fiber heat insulation cylinder arranged inside the furnace body, and a graphite material box is provided inside the carbon fiber insulation cylinder;
  • the graphite material box is provided with an inner inflation port and an inner suction port, the inner inflation port communicates with an inner inflation tube, the inner suction port communicates with an inner suction tube, and both the inner inflation tube and the inner suction tube Extending through the carbon fiber heat insulation tube and the furnace body to the outside of the furnace;
  • the furnace body is provided with an outer inflation port and an outer suction port.
  • the outer inflation port communicates with an outer inflation tube
  • the outer suction port communicates with an outer suction tube.
  • the outer suction tube extends through the carbon fiber heat insulation cylinder Between the carbon fiber heat insulation barrel and the graphite box.
  • the graphite material box is provided with an air guide device and several layers of material plates, the air guide device is located between the inner inflation port and the material plate, and the air guide device is provided with The air guide holes of each layer of the material board.
  • the inner inflation port is provided at both ends of the graphite box, the inner suction port is located in the middle of the graphite box; or the inner inflation port is located in the middle of the graphite box,
  • the inner suction port is provided at both ends of the graphite box; or the inner inflation port is provided at one end of the graphite box, and the inner suction port is provided at the other end of the graphite box.
  • the inner suction pipe is sequentially connected with a first pressure sensor, a first flow regulating valve and a vacuum pump, the first pressure sensor is used to detect the internal pressure of the graphite hopper, and the outer suction pipe is sequentially connected with A second flow regulating valve and the vacuum pump are provided with a second pressure sensor for detecting the external pressure of the graphite box on the furnace body.
  • a third flow regulating valve and a third pressure sensor are also connected to the inner suction pipe between the inner suction port and the first pressure sensor.
  • a plurality of graphite heating rods are evenly distributed between the carbon fiber heat insulation cylinder and the graphite material box, and a plurality of thermocouples are provided on the graphite material box, and the thermocouple is used to detect the graphite material The temperature of the corresponding area of the box.
  • the inner suction port is provided on the lower side of the graphite material box
  • a pressure dividing valve is provided on the graphite material box on the lower side of the material plate at the bottom
  • the middle of the upper side of the graphite material box Or the material box cover is provided at both ends.
  • a mass flow meter is respectively arranged on the inner inflation tube and the outer inflation tube.
  • the invention also provides a method for using the vacuum degreasing sintering furnace as described in any one of the above technical solutions,
  • the temperature inside the graphite feed box is controlled, the external gas filling tube is used to fill the outer gas body into the furnace outside the graphite material box, and the inner gas filling tube is used to fill the internal gas filling degreasing process gas into the graphite material box.
  • the air flow rate of the inner inflation port and the inner suction port and the outer inflation port and the outer suction port make the external pressure of the graphite material box greater than the internal pressure, and the binder vapor inside the graphite material box will not diffuse to the outside of the graphite material box;
  • control the temperature inside the graphite box use the outer inflation tube to fill the furnace outside the graphite box, and use the inner inflation tube to fill the graphite box with inner sintering process gas, by adjusting The air flow rate of the inner inflation port and the inner suction port and the outer inflation port and the outer suction port make the external pressure of the graphite material box equal to, slightly greater than or slightly less than the internal pressure, and the pollution gas outside the graphite material box will not diffuse into the graphite material box Inside, to ensure that the atmosphere inside the graphite box is pure, and the internal sintering process gas inside the graphite box will not diffuse to the outside of the graphite box.
  • the internal degreasing process gas is water vapor, air, hydrogen, inert gas, carbon dioxide, carbon monoxide, methane, propane, acetylene, oxygen or ammonia gas, or a mixed gas of at least two of the above gases;
  • the sintering process gas is hydrogen, inert gas, carbon dioxide, carbon monoxide, methane, propane, acetylene, oxygen, or ammonia, or a mixed gas of at least two of the above gases;
  • the outer inflatable body is inert gas or hydrogen or hydrogen and inert Mixed gas of gas; when the outer suction pipe is closed, the outer inflatable body can be drawn out through the inner suction pipe through the partial pressure valve without passing through the product.
  • the vacuum degreasing and sintering furnace of the present invention is mainly filled with process gas in the graphite material box, and supplemented by inert gas outside the graphite material box to isolate the atmosphere inside and outside the graphite material box and form a relatively independent and pure
  • the space reduces various impure atmospheres and pollutants outside the graphite material box into the graphite material box and affects the sintering of the product, which improves the product quality.
  • the invention can prevent the adhesive vapor from leaking out and polluting the furnace during degreasing, and also draw out the impure atmosphere outside the graphite material box through the external exhaust port, which reduces the pollution degree in the furnace and also prolongs the vacuum degreasing.
  • the service life of the sintering furnace can prevent the adhesive vapor from leaking out and polluting the furnace during degreasing, and also draw out the impure atmosphere outside the graphite material box through the external exhaust port, which reduces the pollution degree in the furnace and also prolongs the vacuum degreasing.
  • the present invention makes it possible to use hydrogen in high-temperature sintering and oxygen in low-temperature degreasing through the different settings of the inside and outside atmosphere of the graphite box, and solve the technical problems that those skilled in the art have been eager to solve, thereby reducing the time of degreasing and sintering. , Improve production speed, and improve product performance and quality.
  • Figure 1 is a system diagram of the existing vacuum degreasing sintering furnace
  • FIG. 2 is a front sectional view of a conventional vacuum degreasing sintering furnace
  • Figure 3 is a graph of the reaction effect of graphite rods fed with hydrogen at a gradual temperature
  • FIG. 4 is a system diagram of the vacuum degreasing sintering furnace of the present invention.
  • 1-furnace body 2-carbon fiber heat insulation tube, 3-graphite feed box, 4-inner inflation port, 5-inner exhaust port, 6-inner inflation tube, 7-inner exhaust tube, 8-outer inflation port, 9-outer suction port, 10-outer inflation tube, 11-outer suction tube, 12-air guide, 13-plate, 14-first pressure sensor, 15-first flow regulating valve, 16-vacuum pump, 17- Second flow regulating valve, 18-second pressure sensor, 19-third flow regulating valve, 20-third pressure sensor, 21-graphite heating rod, 22-thermocouple, 23-partial pressure valve, 24-top box Cover, 25-mass flow meter.
  • the purpose of the present invention is to provide a vacuum degreasing and sintering furnace and its use method to solve the above-mentioned problems in the prior art and improve the degreasing and sintering efficiency and product quality.
  • this embodiment provides a vacuum degreasing sintering furnace, including a furnace body 1 and a carbon fiber heat insulation tube 2 disposed inside the furnace body 1, a graphite material box is provided inside the carbon fiber heat insulation tube 2 3.
  • a material box upper cover 24 is provided in the middle of the upper side of the graphite material box 3.
  • a number of graphite heating rods 21 are evenly distributed between the carbon fiber heat insulation cylinder 2 and the graphite material box 3 along the circumferential direction.
  • the graphite material box 3 is provided with a plurality of thermocouples 22 on the upper and lower sides, respectively, and the thermocouples 22 are used to detect the graphite material. The temperature of the upper and lower sides of the box 3.
  • the graphite feed box 3 is provided with an inner inflation port 4 and an inner suction port 5, the inner inflation port 4 communicates with an inner inflation tube 6, the inner inflation tube 6 is used to feed process gas into the graphite feed box 3, and the inner suction port 5 communicates There is an inner suction tube 7, the inner inflation tube 6 and the inner suction tube 7 extend through the carbon fiber insulation tube 2 and the furnace body 1 to the outside of the furnace; the furnace body 1 is provided with an outer inflation port 8 and an outer suction port 9, the outer inflation port 8 is connected with an outer inflation tube 10, which is used to pour inert gas between the furnace body 1 and the carbon fiber heat insulation tube 2, the outer suction port 9 is connected with an outer suction tube 11, the outer suction tube 11 penetrates the carbon fiber insulation
  • the barrel 2 extends between the carbon fiber heat insulation barrel 2 and the graphite bin 3.
  • the inner inflation port 4 is provided at both ends of the upper side of the graphite feed box 3, the inner suction port 5 is provided at the middle of the lower side of the graphite feed box 3; the outer inflation port 8 is provided at the upper side of the furnace body 1, the outer The exhaust port 9 is provided on the lower side of the furnace body 1.
  • the process gas enters the graphite feed box 3 through the inner inflation tube 6.
  • the gas flow passes through the product and is drawn out from the inner exhaust tube 7.
  • the inert gas enters the furnace through the outer inflation tube 10.
  • the external suction pipe 11 is drawn out, forming different effects of the atmosphere inside and outside the graphite box 3 as shown in FIG. 9.
  • the graphite material box 3 is provided with a gas guide device 12 and a plurality of material plates 13.
  • the material plate 13 is a multi-layer double-row arrangement.
  • the material plate 13 is provided with a ceramic plate for placing a product embryo, and the gas guide device 12 Located between the inner inflation port 4 and the material plate 13, an air guide device 12 is provided on both outer sides of the double-row material plate 13 respectively.
  • the air guide device 12 may be plate-shaped or tubular, and is provided with a passage leading to each layer of material The gas guide holes of the plate 13 allow the process gas to enter the layers uniformly.
  • a mass flow meter 25 is provided on the inner inflation tube 6 and the outer inflation tube 10 respectively;
  • the first pressure sensor 14, the first flow regulating valve 15 and the vacuum pump 16 constitute a degreasing pipeline system, and are connected with the inner suction tube 7 Connected, when the degreasing process is carried out, the first flow regulating valve 15 is opened, and the first pressure sensor 14 is used to detect the internal pressure of the graphite feed box 3; the outer suction pipe 11 is in turn communicated with the second flow regulating valve 17 and the vacuum pump 16, furnace
  • the body 1 is provided with a second pressure sensor 18 for detecting the external pressure of the graphite tank 3.
  • the first flow regulating valve 15 and the second flow regulating valve 17 By adjusting the flow rates of the two mass flow meters 25, the first flow regulating valve 15 and the second flow regulating valve 17, the internal pressure and the external pressure of the graphite hopper 3 can be adjusted, and can be passed through the first pressure sensor 14 and The second pressure sensor 18 performs real-time monitoring.
  • the inner suction pipe 7 is also connected with a third flow regulating valve 19 and a third pressure sensor 20 for performing a partial pressure sintering process.
  • This embodiment also provides a method for using the above vacuum degreasing sintering furnace.
  • the temperature inside the graphite feed box 3 is controlled, and the outer gas filling tube 10 is used to fill the furnace outside the graphite feed box 3 with an inert gas, such as Nitrogen or argon is used to fill the graphite material box 3 with the degassing process gas through the inner inflation tube 6.
  • an inert gas such as Nitrogen or argon
  • the degreasing process gas is generally selected as an inert gas, or oxygen-containing media such as steam or air can also be used, and hydrogen can also be used to improve degreasing Rate, when the oxygen-containing medium gas is selected, it should be noted that the temperature of the graphite feed box 3 is not higher than 300 °C, preferably about 200 °C, in order to avoid the sensitive temperature of the reaction between oxygen and graphite, by adjusting the inner inflation port 4 and the inner pumping
  • the air flow of the gas port 5 and the outer inflation port 8 and the outer suction port 9 makes the external pressure of the graphite material box 3 greater than the internal pressure, and the binder vapor inside the graphite material box 3 will not diffuse to the outside of the graphite material box 3 and pollute the furnace
  • the inner wall of the furnace body 1, carbon fiber heat insulation tube 2 and graphite pieces Such as the inner wall of the furnace body 1, carbon fiber heat insulation tube 2 and graphite pieces.
  • the temperature inside the graphite feed box 3 is controlled, and the furnace outside the graphite feed box 3 is filled with an inert gas, such as nitrogen or argon, using the outer inflation tube 10, and the graphite feed box 3 is used with the inner inflation tube 6
  • an inert gas such as nitrogen or argon
  • the interior is filled with sintering process gas.
  • the sintering process gas is generally selected as inert gas, and hydrogen can also be used.
  • the temperature of the graphite feed box 3 is not less than 1200 °C, preferably 1300 °C, by adjusting the internal inflation
  • the air flow rate of the port 4 and the inner suction port 5 and the outer inflation port 8 and the outer suction port 9 make the external pressure of the graphite material box 3 equal to, slightly greater or slightly less than the internal pressure, and the slightly larger and slightly smaller means the graphite material box 3
  • the internal and external pressure difference is less than the maximum pressure that the graphite box 3 can withstand under the premise of sealing.
  • the pollutant gas outside the graphite box 3 will not diffuse into the graphite box 3, Ensure that the atmosphere inside the graphite feed box 3 is pure, and the sintering process gas inside the graphite feed box 3 will not diffuse outside the graphite feed box 3 and cause loss of furnace parts such as the carbon fiber heat insulation cylinder 2 and graphite pieces.
  • the inner inflation port 4 is provided in the middle of the upper side of the graphite feed box 3, and the inner suction port 5 is provided at both ends of the lower side of the graphite feed box 3 in two rows
  • An air guiding device 12 is respectively provided at the adjacent end of the material plate 13, the upper cover 24 of the material box is provided at both ends of the upper side of the graphite material box 3, and the external air extraction port 9 is provided at the lower side of the furnace body 1.
  • the inner inflation port 4 is provided at one end on the upper side of the graphite box 3, such as the right end, and the inner suction port 5 is provided at the other end under the graphite box 3
  • the material plate 13 is provided in multiple layers. Only the right end of the material plate 13 is provided with a gas guide device 12, and the external air extraction port 9 is provided at the lower side of the furnace body 1.
  • FIG. 8 The difference between this embodiment and the first embodiment is that when the external suction pipe 11 is closed, a pressure dividing valve 23 can be provided on the graphite material box 3 under the bottommost material plate 13 23 is close to the inner suction port 5. Due to the obstruction of the upper side material plate 13, the contaminated gas that enters the graphite hopper 3 through the partial pressure valve 23 will be directly discharged through the inner suction port 5 without contaminating the embryo body of the product. The same technical effect.

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Abstract

一种真空脱脂烧结炉及其使用方法,涉及粉末冶金、粉末陶瓷烧结等制造专用设备技术领域,石墨料箱(3)上设有内充气口(4)和内抽气口(5),内充气口(4)连通有内充气管(6),内抽气口(5)连通有内抽气管(7),炉体(1)上设有外充气口(8)和外抽气口(9),外充气口(8)连通有外充气管(10),外抽气口(9)连通有外抽气管(11)。所述真空脱脂烧结炉以向石墨料箱(3)内充工艺气体为主,以向石墨料箱(3)外充惰性气体为辅,将石墨料箱(3)内外气氛隔离,减少石墨料箱(3)外各种不纯气氛和污染物进入石墨料箱(3)而影响产品的烧结,提高了产品质量和生产速度,减少了炉内的污染程度,延长了真空脱脂烧结炉的使用寿命,并使得高温烧结时氢气的使用和低温脱脂时氧的使用成为可能。

Description

一种真空脱脂烧结炉及其使用方法 技术领域
本发明涉及粉末冶金及粉末陶瓷烧结等制造专用设备技术领域,特别是涉及一种真空脱脂烧结炉及其使用方法。
背景技术
石墨热场真空脱脂烧结炉用于对金属粉末胚体进行脱脂和烧结处理,炉内主要部件均是由碳纤维与石墨制成,石墨因具有优异的电导率、超耐热性、高可靠性及轻巧易于加工、寿命长等优点,是真空烧结炉的主要材料之一,但同时也存在如下问题:
1.粉尘影响:石墨和碳纤维容易生成粉尘,石墨粉尘、碳纤维粉尘会随气流带入料箱内,附着在料箱内产品上,在烧结时产品表面容易产生缺陷,而产品中的碳含量也随之增高,使要求较高的由不锈钢如316、304、316L、17-4PH等材料制成的产品性能下降。
2.水份影响:当炉门打开时,空气中的水份会进入炉内,进入到碳纤维隔热筒中,在真空高温下,水份会变成蒸汽跑出来,水分使产品表面氧化,轻微的出现发黄,严重的出现发灰、发蓝的现象。
3.泄漏影响:真空炉的泄漏是无法避免的,只是将泄漏控制在较低的水平,空气从炉门等位置进入,容易与烧结的产品接触而影响产品的性能。不同炉子的泄漏量不同,造成不同炉子烧结的产品之间存在差异。
4.新物质的污染影响:陶瓷板(承烧板)是放置产品的中介物,没有陶瓷板,产品就直接烧融(如PM、MIM产品),所以又是烧结的必用承烧部件。但陶瓷板与石墨料板直接接触,会产生碳热还原反应,生成Al和Al 2O 3等新物质附着在产品表面上,在炉内抽真空或冷却等工艺时,料箱上盖打开,生成的新物质会跑到料箱外部去,进入到碳纤维隔热筒中,或附着在炉内壁上污染隔热筒,在下一炉工艺运行环节中又跑到料箱内,如此循环,达到一定量时,会沉积在产品表面,造成产品表面不良,并影响产品性能。
5.粘结剂污染的影响:真空环境有利于粘结剂的气化,但也容易使粘 结剂扩散,脱脂时,粘结剂会从产品中脱出变成蒸气并扩散,部分会泄漏到料箱外部去,进入到碳纤维隔热筒中,或附着在炉内壁上,污染炉内。在烧结工艺时,粘结剂蒸气又会被载流气体带入料箱内污染产品,影响产品尺寸与性能。
现有的真空脱脂烧结炉的炉内结构如图1和图2所示,料箱B1与内抽管B2连接,内抽管B2与真空泵B3连接,在脱脂和烧结工艺时,工艺气体充入炉内,真空泵工作,料箱外压力大于料箱内压力,压力差促使气体单向流动,料箱外气体从料箱门与料箱体之间的缝隙进入料箱,气体进入料箱内,经过产品表面,再进入内抽管B2。公开号为CN103264163A,公开日为2013年5月6日的中国发明专利申请公开了一种金属粉末注射成形真空脱脂烧结炉定向气流装置,门板上装有进气装置,当料箱内外压差达到一定值时,进气阀打开,使气流从门板处进入,流经产品表面,进入到内抽管。在现有技术中,气体将料箱外部空间的气氛及污染物带入料箱,并流经产品。气氛中包括泄漏的空气、沉积在保温碳纤维隔热筒中的水、碳等气氛;污染物包括粉尘,氧化铝或氧化硅等污染物。料箱内产品被污染,就会有缺陷,浓度高的碳气氛会使产品增碳,空气会使产品氧化,氧化铝或氧化硅会使产品变形,尺寸不均等。
此外,还存在工艺气体被限制使用的问题,由于氢气的热传导率非常好,在室温下是氮气的7倍,可将产品胚体迅速加热,且能与高分子反应,加速分解粘结剂中的高分子有机物,所以氢气经常应用于烧结炉的脱脂工艺中,提高脱脂速率。又因其在金属中的扩散速率相当快,对氧化物的还原能力强,所以氢气又是一种非常理想的烧结工艺气体。
高温烧结使用氢气的目的在于:氢气与碳反应,可将以下产生的碳,游离碳,产品中的碳脱除:
1.使用石墨热场高温烧结时,由于整体碳势较高,烧结低碳不锈钢时,碳含量超标,如316L,使用石墨热场碳含量在0.04%以下比较困难。
2.由低温热脱脂时,残留在热场的碳,在高温烧结时挥发出来形成游离碳,游离碳会使产品渗碳或局部渗碳。
3.金属粉末制成时,表面会形成一层氧化层,如果氧化层不去除,在烧结时会阻碍扩散,使产品无法达到致密,使用氢气可以使氧化碳还原。
但是行业内,氢气在石墨热场的烧结工艺中是被限制使用的。因为氢气与碳在敏感温度区(1000℃~1200℃)会发生反应。现有的真空脱脂烧结炉中的零部件不管是料箱B1还是隔热筒B5都是碳制成。实验表明,石墨棒在渐变温度下通入氢气,氢气与石墨在之间会发生反应,消耗石墨件,如图3所示。所以在现有技术的石墨热场的烧结工艺中是不允许通入氢气的。并且仅在敏感温度区外向炉内通入氢气也是不可行的。因为料箱外圈有发热材B4(石墨电极棒、石墨加热棒和石墨连接片)用以加热料箱B1,发热材B4外圈有碳纤维的隔热筒B5,用以维持料箱B1热量不流失。石墨立柱B8用以支撑石墨的料箱B1,石墨的内抽管B2用以连接真空管道系统和料箱B1,确保气流走向。炉内料箱B1外部有这么多石墨件,加上炉体B7的夹套中通有冷却水,所以炉内从料箱B1到炉内壁(由内到外)的温度也各不相同,其中,发热材B4的温度最高,通过辐射使料箱B1外壁温度升高,料箱温度一方面传导到料箱B1内,一方面传导到石墨立柱B8和石墨上盖B9等石墨件上。隔热筒B5内壁温度较高,而外壁温度又较低,所以炉内各部件温度都不同。热电偶B6监控的是料箱B1的温度,当料箱B1温度控制在氢气反应敏感区外,如1300℃,则发热材B4温度会高于1300℃,但靠近隔热筒B5石墨件的温度则在氢气反应敏感区内,氢气会与此温度区间的石墨件反应,损耗零部件。
脱脂工艺对于产品的质量也很重要,脱脂如果脱不干净,后续烧结时,产品尺寸偏大,表面会发灰,性能不达标。现有技术中报废率极高,解决办法只有加长脱脂时间,使产品中的粘结剂尽可能的排出。而在低温下,空气中的氧与粘结剂反应,可加快脱脂速度,(粘结剂主要成份为高分子塑料,如PE、PP等,塑料在200℃左右温度下加入氧,可加速塑料燃烧)但目前真空脱脂烧结炉技术中,氧是限制使用的,因为在300℃以上氧会与石墨发生反应,从而损耗石墨件。此外,同氢气限制使用一样,就算将料箱温度控制在200℃左右,氧充入炉内,在进入料箱前,会经过不同温度区域,对反应区域的石墨件和隔热筒会有反应,特别是发热材,温度比料箱温度高,损耗较大。
发明内容
本发明的目的是提供一种真空脱脂烧结炉及其使用方法,以解决上 述现有技术存在的问题,提高脱脂烧结效率和产品的质量。
为实现上述目的,本发明提供了如下方案:
本发明提供了一种真空脱脂烧结炉,包括炉体和设置于所述炉体内部的碳纤维隔热筒,所述碳纤维隔热筒内部设有石墨料箱;
所述石墨料箱上设有内充气口和内抽气口,所述内充气口连通有内充气管,所述内抽气口连通有内抽气管,所述内充气管和所述内抽气管均贯穿所述碳纤维隔热筒和所述炉体延伸至炉外;
所述炉体上设有外充气口和外抽气口,所述外充气口连通有外充气管,所述外抽气口连通有外抽气管,所述外抽气管贯穿所述碳纤维隔热筒延伸至所述碳纤维隔热筒与所述石墨料箱之间。
优选地,所述石墨料箱内设有导气装置和若干层料板,所述导气装置位于所述内充气口与所述料板之间,所述导气装置上设有分别通向每层所述料板的导气孔。
优选地,所述内充气口设置在所述石墨料箱的两端,所述内抽气口设置在所述石墨料箱的中间;或所述内充气口设置在所述石墨料箱的中间,所述内抽气口设置在所述石墨料箱的两端;或所述内充气口设置在所述石墨料箱的一端,所述内抽气口设置在所述石墨料箱的另一端。
优选地,所述内抽气管依次连通有第一压力传感器、第一流量调节阀和真空泵,所述第一压力传感器用于检测所述石墨料箱的内部压力,所述外抽气管依次连通有第二流量调节阀和所述真空泵,所述炉体上设有用于检测所述石墨料箱的外部压力的第二压力传感器。
优选地,所述内抽气口与所述第一压力传感器之间的所述内抽气管还连通有第三流量调节阀和第三压力传感器。
优选地,所述碳纤维隔热筒与所述石墨料箱之间均布有若干个石墨发热棒,所述石墨料箱上设有若干个热电偶,所述热电偶用于检测所述石墨料箱对应区域的温度。
优选地,所述内抽气口设置在所述石墨料箱的下侧,最底层的所述料板下侧的所述石墨料箱上设有分压阀,所述石墨料箱上侧的中间或两端设有料箱上盖。
优选地,所述内充气管和所述外充气管上分别设有一质量流量计。
本发明还提供了如上述技术方案中任一项所述的真空脱脂烧结炉的使用方法,
在进行脱脂工艺时,控制石墨料箱内部的温度,利用外充气管向石墨料箱外部的炉内充入外充气体,利用内充气管向石墨料箱内部充入内充脱脂工艺气体,通过调节内充气口和内抽气口以及外充气口和外抽气口的气流量,使石墨料箱的外部压力大于内部压力,石墨料箱内部的粘结剂蒸气不会扩散到石墨料箱外部;
在进行烧结工艺时,控制石墨料箱内部的温度,利用外充气管向石墨料箱外部的炉内充入外充气体,利用内充气管向石墨料箱内部充入内充烧结工艺气体,通过调节内充气口和内抽气口以及外充气口和外抽气口的气流量,使石墨料箱的外部压力等于、稍大于或稍小于内部压力,石墨料箱外部的污染气体不会扩散进入石墨料箱内部,保证石墨料箱内部的气氛纯净,石墨料箱内部的内充烧结工艺气体也不会扩散到石墨料箱外部。
优选地,所述内充脱脂工艺气体为水蒸气、空气、氢气、惰性气体、二氧化碳、一氧化碳、甲烷、丙烷、乙炔、氧气或氨气,或者是至少两种上述气体的混合气体;所述内充烧结工艺气体为氢气、惰性气体、二氧化碳、一氧化碳、甲烷、丙烷、乙炔、氧气或氨气,或者是至少两种上述气体的混合气体;所述外充气体为惰性气体或氢气或氢气与惰性气体的混合气体;在外抽气管关闭时,所述外充气体能够通过分压阀经由内抽气管抽出,而不经过产品。
本发明相对于现有技术取得了以下技术效果:
本发明的真空脱脂烧结炉以向石墨料箱内充工艺气体为主,以向石墨料箱外充惰性气体为辅,使石墨料箱内外气氛隔离,使石墨料箱内形成一个相对独立纯净的空间,减少了石墨料箱外各种不纯气氛和污染物进入石墨料箱而影响产品的烧结,提高了产品质量。
本发明通过压力差的设置可防止脱脂时的粘接剂蒸汽外泄污染炉内,还将石墨料箱外不纯的气氛由外抽气口抽出,减少炉内的污染程度,也延长了真空脱脂烧结炉的使用寿命。
本发明通过石墨料箱内外气氛的不同设置,使得高温烧结时氢气的使用和低温脱脂时氧的使用成为可能,解决了本领域技术人员一直迫切希望 解决的技术问题,从而缩短了脱脂烧结的时间,提高了生产速度,并提高了产品的性能和质量。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1为现有真空脱脂烧结炉的系统图;
图2为现有真空脱脂烧结炉的主视剖视图;
图3为石墨棒在渐变温度下通入氢气的反应效果图;
图4本发明真空脱脂烧结炉的系统图;
图5为实施例一的主视剖视图;
图6为实施例二的主视剖视图;
图7为实施例三的主视剖视图;
图8为实施例四的主视剖视图;
图9为发明真空脱脂烧结炉的气氛效果图;
其中:1-炉体,2-碳纤维隔热筒,3-石墨料箱,4-内充气口,5-内抽气口,6-内充气管,7-内抽气管,8-外充气口,9-外抽气口,10-外充气管,11-外抽气管,12-导气装置,13-料板,14-第一压力传感器,15-第一流量调节阀,16-真空泵,17-第二流量调节阀,18-第二压力传感器,19-第三流量调节阀,20-第三压力传感器,21-石墨发热棒,22-热电偶,23-分压阀,24-料箱上盖,25-质量流量计。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有付出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明的目的是提供一种真空脱脂烧结炉及其使用方法,以解决上述现有技术存在的问题,提高脱脂烧结效率和产品的质量。
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合附图和具体实施方式对本发明作进一步详细的说明。
实施例一
如图4-图5所示:本实施例提供了一种真空脱脂烧结炉,包括炉体1和设置于炉体1内部的碳纤维隔热筒2,碳纤维隔热筒2内部设有石墨料箱3,石墨料箱3上侧的中间设有料箱上盖24。碳纤维隔热筒2与石墨料箱3之间沿周向均布有若干个石墨发热棒21,石墨料箱3上侧和下侧分别设有若干个热电偶22,热电偶22分别用于检测石墨料箱3上侧和下侧的温度。
石墨料箱3上设有内充气口4和内抽气口5,内充气口4连通有内充气管6,内充气管6用于向石墨料箱3内部通入工艺气体,内抽气口5连通有内抽气管7,内充气管6和内抽气管7均贯穿碳纤维隔热筒2和炉体1延伸至炉外;炉体1上设有外充气口8和外抽气口9,外充气口8连通有外充气管10,外充气管10用于向炉体1和碳纤维隔热筒2之间冲入惰性气体,外抽气口9连通有外抽气管11,外抽气管11贯穿碳纤维隔热筒2延伸至碳纤维隔热筒2与石墨料箱3之间。在本实施例中,内充气口4设置在石墨料箱3上侧的两端,内抽气口5设置在石墨料箱3下侧的中间;外充气口8设置在炉体1上侧,外抽气口9设置在炉体1下侧,工艺气体通过内充气管6进入石墨料箱3内,气流流经产品,由内抽气管7抽出,同时惰性气体通过外充气管10进入炉内,由外抽气管11抽出,形成如图9所示的石墨料箱3内外气氛不同的效果。
进一步地,石墨料箱3内设有导气装置12和若干层料板13,料板13为多层双列设置,料板13上设有用于放置产品胚体的陶瓷板,导气装置12位于内充气口4与料板13之间,双列料板13的两外侧分别设有一导气装置12,导气装置12可为板状或管状,且其上设有分别通向每层料板13的导气孔,使工艺气体可均匀地进入到各层。
如图4所示,内充气管6和外充气管10上分别设有一质量流量计25;第一压力传感器14、第一流量调节阀15和真空泵16构成脱脂管道系统,并与内抽气管7连通,当进行脱脂工艺时,第一流量调节阀15打开,第一压力传感器14用于检测石墨料箱3的内部压力;外抽气管11依次连通 有第二流量调节阀17和真空泵16,炉体1上设有用于检测石墨料箱3的外部压力的第二压力传感器18。通过调节两个质量流量计25、第一流量调节阀15和第二流量调节阀17的流量大小,可调节石墨料箱3的内部压力和外部压力大小,并可分别通过第一压力传感器14和第二压力传感器18进行实时监测。内抽气管7还连通有第三流量调节阀19和第三压力传感器20,用于进行分压烧结工艺。
本实施例还提供了上述真空脱脂烧结炉的使用方法,在进行脱脂工艺时,控制石墨料箱3内部的温度,利用外充气管10向石墨料箱3外部的炉内充入惰性气体,如氮气或氩气,利用内充气管6向石墨料箱3内部充入脱脂工艺气体,脱脂工艺气体一般选为惰性气体,也可以选用水蒸气或空气等含氧介质,还可选用氢气以提高脱脂速率,当选用含氧介质气体时,要注意控制石墨料箱3的温度不高于300℃,优选为200℃左右,以避开氧与石墨反应敏感温度,通过调节内充气口4和内抽气口5以及外充气口8和外抽气口9的气流量,使石墨料箱3的外部压力大于内部压力,石墨料箱3内部的粘结剂蒸气不会扩散到石墨料箱3外部而污染炉内的如炉体1内壁、碳纤维隔热筒2和石墨件。
在进行烧结工艺时,控制石墨料箱3内部的温度,利用外充气管10向石墨料箱3外部的炉内充入惰性气体,如氮气或氩气,利用内充气管6向石墨料箱3内部充入烧结工艺气体,烧结工艺气体一般选为惰性气体,也可选用氢气,当选用氢气时,要注意控制石墨料箱3的温度不低于1200℃,优选为1300℃,通过调节内充气口4和内抽气口5以及外充气口8和外抽气口9的气流量,使石墨料箱3的外部压力等于、稍大于或稍小于内部压力,稍大、稍小是指石墨料箱3的内外压力差小于石墨料箱3在保证密封的前提下能够承受的最大压力,由于石墨料箱3具有一定的密封性,石墨料箱3外部的污染气体不会扩散进入石墨料箱3内部,保证石墨料箱3内部的气氛纯净,石墨料箱3内部的烧结工艺气体也不会扩散到石墨料箱3外部而损耗炉内零件如碳纤维隔热筒2和石墨件。
实施例二
如图6所示:本实施例与实施例一的区别在于:内充气口4设置在石墨料箱3上侧的中间,内抽气口5设置在石墨料箱3下侧的两端,两列料 板13相邻的一端分别设有一导气装置12,料箱上盖24设置在石墨料箱3上侧的两端,外抽气口9设置在炉体1下侧。其余技术特征和使用方法参见实施例一即可。
实施例三
如图7所示:本实施例与实施例一的区别在于:内充气口4设置在石墨料箱3上侧的一端,如右端,内抽气口5设置在石墨料箱3下侧的另一端,如左端,料板13为多层设置,仅在料板13右端设有导气装置12,外抽气口9设置在炉体1下侧。其余技术特征和使用方法参见实施例一即可。
实施例四
如图8所示:本实施例与实施例一的区别在于:当外抽气管11关闭,可在最底层的料板13下侧的石墨料箱3上设有分压阀23,分压阀23靠近内抽气口5,由于上侧料板13的阻隔,通过分压阀23进入到石墨料箱3中的污染气体会直接通过内抽气口5排出而不会污染产品的胚体,实现基本相同的技术效果。
本说明书中应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想;同时,对于本领域的一般技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处。综上所述,本说明书内容不应理解为对本发明的限制。

Claims (10)

  1. 一种真空脱脂烧结炉,其特征在于:包括炉体和设置于所述炉体内部的碳纤维隔热筒,所述碳纤维隔热筒内部设有石墨料箱;
    所述石墨料箱上设有内充气口和内抽气口,所述内充气口连通有内充气管,所述内抽气口连通有内抽气管,所述内充气管和所述内抽气管均贯穿所述碳纤维隔热筒和所述炉体延伸至炉外;
    所述炉体上设有外充气口和外抽气口,所述外充气口连通有外充气管,所述外抽气口连通有外抽气管,所述外抽气管贯穿所述碳纤维隔热筒延伸至所述碳纤维隔热筒与所述石墨料箱之间。
  2. 根据权利要求1所述的真空脱脂烧结炉,其特征在于:所述石墨料箱内设有导气装置和若干层料板,所述导气装置位于所述内充气口与所述料板之间,所述导气装置上设有分别通向每层所述料板的导气孔。
  3. 根据权利要求1或2所述的真空脱脂烧结炉,其特征在于:所述内充气口设置在所述石墨料箱的两端,所述内抽气口设置在所述石墨料箱的中间;或所述内充气口设置在所述石墨料箱的中间,所述内抽气口设置在所述石墨料箱的两端;或所述内充气口设置在所述石墨料箱的一端,所述内抽气口设置在所述石墨料箱的另一端。
  4. 根据权利要求1所述的真空脱脂烧结炉,其特征在于:所述内抽气管依次连通有第一压力传感器、第一流量调节阀和真空泵,所述第一压力传感器用于检测所述石墨料箱的内部压力,所述外抽气管依次连通有第二流量调节阀和所述真空泵,所述炉体上设有用于检测所述石墨料箱的外部压力的第二压力传感器。
  5. 根据权利要求4所述的真空脱脂烧结炉,其特征在于:所述内抽气口与所述第一压力传感器之间的所述内抽气管还连通有第三流量调节阀和第三压力传感器。
  6. 根据权利要求1所述的真空脱脂烧结炉,其特征在于:所述碳纤维隔热筒与所述石墨料箱之间均布有若干个石墨发热棒,所述石墨料箱上设有若干个热电偶,所述热电偶用于检测所述石墨料箱对应区域的温度。
  7. 根据权利要求2所述的真空脱脂烧结炉,其特征在于:所述内抽气 口设置在所述石墨料箱的下侧,最底层的所述料板下侧的所述石墨料箱上设有分压阀,所述石墨料箱上侧的中间或两端设有料箱上盖。
  8. 根据权利要求1所述的真空脱脂烧结炉,其特征在于:所述内充气管和所述外充气管上分别设有一质量流量计。
  9. 如权利要求1-8中任一项所述的真空脱脂烧结炉的使用方法,其特征在于:在进行脱脂工艺时,控制石墨料箱内部的温度,利用外充气管向石墨料箱外部的炉内充入外充气体,利用内充气管向石墨料箱内部充入内充脱脂工艺气体,通过调节内充气口和内抽气口以及外充气口和外抽气口的气流量,使石墨料箱的外部压力大于内部压力,石墨料箱内部的粘结剂蒸气不会扩散到石墨料箱外部;
    在进行烧结工艺时,控制石墨料箱内部的温度,利用外充气管向石墨料箱外部的炉内充入外充气体,利用内充气管向石墨料箱内部充入内充烧结工艺气体,通过调节内充气口和内抽气口以及外充气口和外抽气口的气流量,使石墨料箱的外部压力等于、稍大于或稍小于内部压力,石墨料箱外部的污染气体不会扩散进入石墨料箱内部,保证石墨料箱内部的气氛纯净,石墨料箱内部的内充烧结工艺气体也不会扩散到石墨料箱外部。
  10. 根据权利要求9所述的真空脱脂烧结炉,其特征在于:所述内充脱脂工艺气体为水蒸气、空气、氢气、惰性气体、二氧化碳、一氧化碳、甲烷、丙烷、乙炔、氧气或氨气,或者是至少两种上述气体的混合气体;所述内充烧结工艺气体为氢气、惰性气体、二氧化碳、一氧化碳、甲烷、丙烷、乙炔、氧气或氨气,或者是至少两种上述气体的混合气体;所述外充气体为惰性气体或氢气或氢气与惰性气体的混合气体;在外抽气管关闭时,所述外充气体能够通过分压阀经由内抽气管抽出,而不经过产品。
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