CN111981847A - Pressure-assisted induction heating vacuum atmosphere flash sintering device - Google Patents
Pressure-assisted induction heating vacuum atmosphere flash sintering device Download PDFInfo
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any of groups F27B1/00 - F27B15/00
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/06—Induction heating, i.e. in which the material being heated, or its container or elements embodied therein, form the secondary of a transformer
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D9/00—Cooling of furnaces or of charges therein
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
- F27D2007/066—Vacuum
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D9/00—Cooling of furnaces or of charges therein
- F27D2009/0002—Cooling of furnaces
- F27D2009/001—Cooling of furnaces the cooling medium being a fluid other than a gas
- F27D2009/0013—Cooling of furnaces the cooling medium being a fluid other than a gas the fluid being water
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27M—INDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
- F27M2003/00—Type of treatment of the charge
- F27M2003/04—Sintering
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
本发明涉及新材料制备领域，提供了一种压力辅助感应加热真空气氛闪速烧结装置，包括炉体、压力***、闪烧***、感应加热***、冷却***和真空***；压力***包括上压头和可移动下压头，上电极及下电极分别设置在上压头和下压头的端部，为闪烧样品提供压力；闪烧***提供闪烧回路；感应加热***提供加热和保温；冷却***冷却炉体；真空***对炉体抽真空。本发明克服了传统闪速烧结技术中的固有缺点，可根据被闪烧结材料的电学性质灵活选择闪烧电源，来引发热失控，从而实现最大程度的致密化水平以及样品微观结构的精细调控，对于金属及陶瓷材料具有普适性；本发明可轻松实现闪烧过程的压力辅助，可为该研究领域提供一种新的制备手段。
The invention relates to the field of new material preparation, and provides a pressure-assisted induction heating vacuum atmosphere flash sintering device, comprising a furnace body, a pressure system, a flash sintering system, an induction heating system, a cooling system and a vacuum system; the pressure system includes an upper indenter The upper and lower electrodes are respectively arranged at the ends of the upper and lower indenters to provide pressure for the flash burning sample; the flash burning system provides a flash burning circuit; the induction heating system provides heating and heat preservation; cooling The system cools the furnace body; the vacuum system evacuates the furnace body. The invention overcomes the inherent shortcomings of the traditional flash sintering technology, and can flexibly select the flash sintering power source according to the electrical properties of the material to be flash sintered to induce thermal runaway, so as to achieve the maximum level of densification and fine control of the microstructure of the sample. It has universality for metal and ceramic materials; the invention can easily realize the pressure assistance of the flash burning process, and can provide a new preparation method for this research field.
Description
技术领域technical field
本发明涉及新材料制备技术领域，特别涉及一种压力辅助感应加热真空气氛闪速烧结装置。The invention relates to the technical field of new material preparation, in particular to a pressure-assisted induction heating vacuum atmosphere flash sintering device.
背景技术Background technique
自从2010年提出闪速烧结(或称为闪光烧结或闪烧)以来，其已经被应用于多种材料，包括离子导体，如氧化钇稳定氧化锆(YSZ)和钆掺杂二氧化铈(GDC)；半导体，如氧化锌(ZnO)和碳化硅(SiC)；以及某些类型的电子导体和绝缘体，例如Co2MnO4，钛酸锶(SrTiO3)和氧化铝(Al2O3)。与常规烧结工艺相比，闪速烧结最明显的优势在于它大大减少了陶瓷致密化所需的时间、温度和能量，意味着其在工业和环境效益方面具有重要的意义和应用前景。Since flash sintering (or flash sintering or flash sintering) was proposed in 2010, it has been applied to a variety of materials, including ionic conductors such as yttria-stabilized zirconia (YSZ) and gadolinium-doped ceria (GDC). ); semiconductors, such as zinc oxide (ZnO) and silicon carbide (SiC); and certain types of electronic conductors and insulators, such as Co2MnO4 , strontium titanate (SrTiO3 ) , and aluminum oxide ( Al2O3 ) . Compared with the conventional sintering process, the most obvious advantage of flash sintering is that it greatly reduces the time, temperature and energy required for ceramic densification, which means that it has important significance and application prospects in terms of industrial and environmental benefits.
近年来，采用新颖的实验装置来实现闪速烧结引起国际上科学界和技术界的关注，例如闪速放电等离子体烧结(FSPS)，闪速烧结锻造和非接触式闪速烧结。FSPS通过改造商业放电等离子体设备，通过施加极高的脉冲直流电，实现了极难烧结的高熔点碳化物、氮化物、硼化物的闪速烧结；非接触式闪速烧结采用等离子体作为电极，避免了电极和样品之间的物理接触，从而解决了常规闪速烧结方法中的存在的铂电极昂贵、电流不均匀流动产生热点等问题。这些新兴技术提供了闪速烧结扩展到工业应用的可能性。In recent years, the use of novel experimental setups to achieve flash sintering has attracted international scientific and technical attention, such as flash discharge plasma sintering (FSPS), flash sintering forging and non-contact flash sintering. FSPS realizes flash sintering of extremely difficult sintering high melting point carbides, nitrides and borides by transforming commercial discharge plasma equipment and applying extremely high pulsed direct current; non-contact flash sintering uses plasma as an electrode, The physical contact between the electrode and the sample is avoided, thereby solving the problems of expensive platinum electrodes and hot spots caused by uneven current flow in the conventional flash sintering method. These emerging technologies offer the possibility to expand flash sintering into industrial applications.
尽管如此，无论是常规的闪速烧结，还是采用这些新技术，都必须对生坯进行一系列预处理，以确保其具有足够的机械强度进行闪速烧结实验。这些预处理通常包括将粉末与粘结剂或烧结助剂混合、在常规炉中烧掉粘合剂或在FSPS情况下通过SPS进行预烧结。这些额外的预处理过程使闪速烧结失去了其节能和快速处理的固有优势，这与其发展的初衷背道而驰。Nonetheless, both conventional flash sintering and these new technologies require a series of pretreatments on the green body to ensure that it has sufficient mechanical strength for flash sintering experiments. These pretreatments typically include mixing the powder with a binder or sintering aid, burning off the binder in a conventional furnace or pre-sintering by SPS in the case of FSPS. These additional pretreatment processes make flash sintering lose its inherent advantages of energy saving and fast processing, which is contrary to the original intention of its development.
基于闪速烧结技术在新材料制备领域的应用前景，相关科技论文和专利也相继被发表和申请。Based on the application prospects of flash sintering technology in the field of new material preparation, related scientific papers and patents have also been published and applied for.
专利(US9334194B2，US8940220B2)详细描述了陶瓷材料闪速烧结的内涵、操作方法以及基础研究设备；专利(EP2691551B1)报道了一种基于闪速烧结技术的复杂形状零部件的制造方法；专利(JP5562857B2)报道了一种基于闪速烧结技术的致密碘磷灰石的制备方法；专利(US9212424B1)报道了一种借助火焰加热实现闪速烧结的方法；专利(US20150329430A1)报道了一种基于闪速烧结技术的多层陶瓷的制备方法；专利(CN108558398A)报道了一种脉冲放电室温闪速烧结纳米陶瓷材料的方法；专利(CN106630974A)报道了一种在管式炉环境内低温快速烧结陶瓷的闪光烧结方法和制得的陶瓷及其装置；专利(CN108645204A，CN208419576U)报道了一种耦合热压烧结和闪烧技术的烧结炉；专利(CN210070583U)报道了一种耦合微波加热技术和闪烧技术的烧结炉。专利(CN110577399A)报道了一种基于感应加热的多场耦合闪速烧结***，其较为宏观的描述了各个模块的特点以及它们之间的相互作用关系，但并没有提及具体的设备结构，并且其仅可施加20～50MPa的压力，不满足一些需要施加较高压力的情况。专利(CN210070584U)报道了一种用于陶瓷晶体闪烧成型的烧结炉感应辅助加热装置，该装置同样使用感应加热作为闪烧样品的快速预热手段，同时施加一个轴向的压力，但该专利并没有对闪烧样品和模具的情况作出进一步的描述。然而，闪烧技术的关键在于迫使电流直接流过烧结体，引发热失控，从而提高物质的扩散速率，进而实现快速致密化。因此，样品、模具以及压头(又可作为电极)的相对空间位置格外重要，若是没有对其作出明确的规定，那么闪烧技术便无法得到有效应用。Patents (US9334194B2, US8940220B2) describe in detail the connotation, operation method and basic research equipment of flash sintering of ceramic materials; patent (EP2691551B1) reports a manufacturing method of complex-shaped parts based on flash sintering technology; patent (JP5562857B2) A preparation method of dense iodoapatite based on flash sintering technology is reported; patent (US9212424B1) reports a method for realizing flash sintering by means of flame heating; patent (US20150329430A1) reports a flash sintering technology-based method The preparation method of multilayer ceramics; the patent (CN108558398A) reported a method of pulse discharge room temperature flash sintering nano-ceramic materials; the patent (CN106630974A) reported a flash sintering method of low temperature rapid sintering of ceramics in a tube furnace environment and the obtained ceramic and its device; patent (CN108645204A, CN208419576U) reported a sintering furnace coupled with hot pressing sintering and flash sintering technology; patent (CN210070583U) reported a sintering furnace coupled with microwave heating technology and flash sintering technology . The patent (CN110577399A) reports a multi-field coupled flash sintering system based on induction heating, which describes the characteristics of each module and the interaction between them in a macroscopic manner, but does not mention the specific equipment structure, and It can only apply a pressure of 20 to 50 MPa, which does not meet some situations that require a higher pressure to be applied. Patent (CN210070584U) reports a sintering furnace induction-assisted heating device for flash-sintering and molding of ceramic crystals. The device also uses induction heating as a rapid preheating method for flash-sintered samples, and applies an axial pressure at the same time. The patent does not further describe the condition of the flashed samples and molds. The key to flash technology, however, is to force an electric current to flow directly through the sintered body, causing thermal runaway, which increases the rate of diffusion of the species, which in turn enables rapid densification. Therefore, the relative spatial position of the sample, the mold, and the indenter (which also acts as an electrode) is extremely important, and if it is not clearly defined, the flash technology cannot be effectively applied.
发明内容SUMMARY OF THE INVENTION
本发明所解决的技术问题：Technical problem solved by the present invention:
在闪速烧结过程中，样品的预热不需要用到上述专利中提到的较为复杂的设备并且消耗大量的能量，因为电流的不均匀性问题暂时无法在学术界或者技术界得到有效的解决，所以闪速烧结的样品通常很小，对于圆柱形样品而言直径和高度都在10mm左右，因此仅需要对样品实现有效的局部加热即可。本发明提出了一种无需任何预处理即可实施压力辅助闪速烧结的新***及方法。对于陶瓷样品(电阻温度系数为负)通过中频或者高频感应加热，可以将能量集中在“电极-样品-电极区域”或者“模具-样品区域”，从而实现超快且节能的局部加热，进而使陶瓷快达到闪烧温度；对于金属或类似金属的室温导电性良好的材料，利用特殊的模具和电极构造直接在室温下实现电阻加热，引发热失控实现闪烧。由此可以在压力的辅助下,在特殊构造的模具中原位闪烧松装粉末，无需对陶瓷生坯进行额外的预处理，压力最高可达2GPa，闪烧时间小于30s。本发明可用于各种陶瓷基、金属基先进材料的研究与生产。但基于传统核燃料工业的燃料芯块烧结工艺的局限性，本发明尤其适用于各种类型的核燃料芯块的闪速烧结制备。In the flash sintering process, the preheating of the sample does not require the complicated equipment mentioned in the above patent and consumes a lot of energy, because the problem of current non-uniformity cannot be effectively solved in the academic or technical circles. , so the flash sintered samples are usually very small, with a diameter and height of about 10 mm for cylindrical samples, so only effective localized heating of the sample is required. The present invention proposes a new system and method for implementing pressure-assisted flash sintering without any pretreatment. For ceramic samples (with a negative temperature coefficient of resistance), through intermediate frequency or high frequency induction heating, the energy can be concentrated in the "electrode-sample-electrode region" or "mold-sample region", so as to achieve ultra-fast and energy-saving local heating, and then Make the ceramic quickly reach the flash burning temperature; for materials with good room temperature conductivity of metals or similar metals, the special mold and electrode structure are used to directly achieve resistance heating at room temperature, causing thermal runaway to achieve flash burning. As a result, the loose powder can be flash-fired in-situ in a specially constructed mold with the aid of pressure, without additional pretreatment of the ceramic green body, the pressure can be up to 2GPa, and the flash-fire time is less than 30s. The invention can be used for research and production of various ceramic-based and metal-based advanced materials. However, based on the limitations of the fuel pellet sintering process in the traditional nuclear fuel industry, the present invention is especially suitable for the preparation of various types of nuclear fuel pellets by flash sintering.
针对现有技术的不足，本发明采用如下技术方案：For the deficiencies in the prior art, the present invention adopts the following technical solutions:
一种压力辅助感应加热真空气氛闪速烧结装置，主要用于多种核燃料芯块的闪速烧结制备，所述多种核燃料芯块的材料包括二氧化铀、碳化铀、氮化铀、硅化铀，以及以它们为基体的复合材料，是一种全新的核燃料芯块烧结方法。所述装置包括炉体、压力***、闪烧***、感应加热***、冷却***和真空***；A pressure-assisted induction heating vacuum atmosphere flash sintering device is mainly used for the flash sintering preparation of various nuclear fuel pellets, the materials of which include uranium dioxide, uranium carbide, uranium nitride, and uranium silicide , and the composite materials based on them, is a brand-new nuclear fuel pellet sintering method. The device includes a furnace body, a pressure system, a flash burning system, an induction heating system, a cooling system and a vacuum system;
所述压力***包括相对于炉体顶部固定设置的上压头，及可移动下压头；上压头端部设置上电极，下压头端部设置下电极；所述上压头、下压头相对运动时带动所述上电极、下电极为闪烧样品提供压力；The pressure system includes an upper indenter fixed relative to the top of the furnace body, and a movable lower indenter; an upper electrode is arranged at the end of the upper indenter, and a lower electrode is arranged at the end of the lower indenter; the upper indenter, the lower indenter When the head moves relatively, the upper electrode and the lower electrode are driven to provide pressure for the flash burning sample;
所述闪烧***包括闪烧电源、闪烧模具、所述上电极及所述下电极；所述闪烧***为所述闪烧样品提供闪烧回路；The flash burning system includes a flash burning power source, a flash burning mold, the upper electrode and the lower electrode; the flash burning system provides a flash burning circuit for the flash burning sample;
所述感应加热***用于为闪烧样品加热及保温；所述感应加热***设置在所述炉体内；The induction heating system is used for heating and maintaining the flash burning sample; the induction heating system is arranged in the furnace body;
所述冷却***，用于冷却所述炉体；the cooling system for cooling the furnace body;
所述真空***，用于对所述炉体内部抽真空。The vacuum system is used for evacuating the inside of the furnace body.
进一步的，压头与电极之间采用螺纹连接固定，或者直接将电极嵌套于压头端部中心的孔内固定；Further, the indenter and the electrode are fixed by screw connection, or the electrode is directly embedded in the hole in the center of the end of the indenter to be fixed;
炉体外设置压力框架，上压头顶端与上电极板下平面接触将所述上电极引出炉体，上电极板上平面与压力框架上固定的压力传感器之间采用玻纤板或聚四氟乙烯板绝缘；A pressure frame is set outside the furnace, and the top of the upper indenter is in contact with the lower plane of the upper electrode plate to lead the upper electrode out of the furnace body. Glass fiber plate or PTFE is used between the plane of the upper electrode plate and the pressure sensor fixed on the pressure frame. board insulation;
可移动下压头通过伺服电缸驱动，可移动下压头底端与下电极板上平面接触将所述下电极引出炉体，下电极板与伺服电缸之间采用玻纤板或聚四氟乙烯板绝缘；下压头与炉体之间采用动密封(例如油封)。The movable lower pressure head is driven by the servo electric cylinder. The bottom end of the movable lower pressure head is in plane contact with the lower electrode plate to lead the lower electrode out of the furnace body. The glass fiber plate or polytetrafluoroethylene is used between the lower electrode plate and the servo electric cylinder. Insulation with vinyl fluoride plate; dynamic seal (such as oil seal) is used between the lower pressure head and the furnace body.
进一步的，上压头、下压头采用水冷，与炉体之间采用具有一定力学性能的玻纤板或聚四氟材料绝缘。Further, the upper pressure head and the lower pressure head are water-cooled, and glass fiber board or PTFE material with certain mechanical properties is used for insulation between the upper pressure head and the furnace body.
进一步的，所述伺服电缸(0～20T)加压、卸压、位移控制速率可调，恒压力模式、自定义压力模式(可设定加载曲线)可选。Further, the servo electric cylinder (0-20T) can be pressurized, relieved, and the displacement control rate is adjustable, and the constant pressure mode and the custom pressure mode (the loading curve can be set) are optional.
进一步的，所述炉体为卧式圆筒，圆筒筒壁为水冷双层不锈钢结构。Further, the furnace body is a horizontal cylinder, and the cylinder wall is a water-cooled double-layer stainless steel structure.
进一步的，所述炉体对应设置有前门和后门，前门设置观察窗或辐射测温窗，后门设置有热电偶、真空抽气口和真空测量装置。Further, the furnace body is correspondingly provided with a front door and a back door, the front door is provided with an observation window or a radiation temperature measurement window, and the back door is provided with a thermocouple, a vacuum exhaust port and a vacuum measurement device.
进一步的，作为本发明的创新点之一，所述闪烧模具为中空圆柱形，具有3层结构，中空部分放置闪烧样品；所述闪烧模具的最外层为耐高温绝热材料，用于降低闪烧模具内部的温度梯度，次外层为耐高温金属基材料(在闪烧压力较高的条件下使用)，又如高强度石墨(在闪烧压力较低的条件下使用)，次外层用于承受闪烧压力(即使最内层破裂也不影响其承压)，并能被感应加热作为发热体，从而传导加热闪烧样品，使其达到闪烧温度，灵活选择次外层材料，可施加高达2GPa的闪烧压力，可提供高达1500℃的闪烧温度；最内层为耐高温绝缘材料，用于闪烧样品与次外层在闪烧温度下的电绝缘(即使最内层破裂也不影响闪烧样品与次外层的电绝缘)，保证闪烧电源的电流全部通过闪烧样品，从而达到闪烧的目的；所述闪烧模具由耐高温模具座支撑，用于减小闪烧模具与下压头的热传导作用，上压头在闪烧过程中不与闪烧模具接触，避免电流通过闪烧模具。Further, as one of the innovative points of the present invention, the flash-burning mold is a hollow cylinder with a three-layer structure, and a flash-burning sample is placed in the hollow part; In order to reduce the temperature gradient inside the flash burning mold, the secondary outer layer is a high temperature resistant metal base material (used under the condition of high flash burning pressure), such as high-strength graphite (used under the condition of low flash burning pressure), The secondary outer layer is used to withstand the flash burning pressure (even if the innermost layer is broken, it will not affect its bearing pressure), and can be heated by induction as a heating element, so as to conduct heating of the flash burning sample to reach the flash burning temperature, and the secondary outer layer can be selected flexibly. Layer material, can apply flash pressure up to 2GPa, can provide flash temperature up to 1500 ℃; the innermost layer is a high temperature resistant insulating material, which is used for the electrical insulation of the flash sample and the sub-outer layer at the flash temperature (even if The rupture of the innermost layer does not affect the electrical insulation of the flash burning sample and the sub-outer layer), ensuring that the current of the flash burning power supply all passes through the flash burning sample, so as to achieve the purpose of flash burning; the flash burning mold is supported by a high temperature resistant mold base, It is used to reduce the heat conduction between the flash-burning die and the lower indenter. The upper indenter does not contact the flash-burning die during the flash-burning process to avoid current passing through the flash-burning die.
进一步的，闪烧样品直径最大尺寸可达30mm，高度视闪烧电源参数而定。Further, the maximum diameter of the flash burning sample can reach 30mm, and the height depends on the parameters of the flash burning power supply.
进一步的，所述闪烧模具的最外层材料为多孔莫来石或碳毡；次外层材料为高速钢、硬质合金或高强度石墨；最内层材料为氧化铝或氮化硼陶瓷。Further, the material of the outermost layer of the flash burning mold is porous mullite or carbon felt; the material of the second outer layer is high-speed steel, cemented carbide or high-strength graphite; the material of the innermost layer is alumina or boron nitride ceramics .
进一步的，作为本发明的创新点之一，所述闪烧电源可根据被闪烧材料的电学性质选择，以引发最大程度的热失控，实现闪烧，如室温导电性良好的金属材料选择低电压、大电流脉冲电源；预热后具有一定导电性的氧化物陶瓷材料选择高电压、小电流的直流恒流电源。闪烧电源通过导线和上电极板、下电极板连接形成闪烧回路。Further, as one of the innovative points of the present invention, the flash burning power source can be selected according to the electrical properties of the flash burning material, so as to induce thermal runaway to the greatest extent and realize flash burning. Voltage, high current pulse power supply; select high voltage, low current DC constant current power supply for oxide ceramic materials with certain conductivity after preheating. The flash burning power supply is connected with the upper electrode plate and the lower electrode plate through the wire to form a flash burning circuit.
进一步的，所述感应加热***包括感应加热电源(例如参数为：10～30kW，15～80kHz)和感应加热线圈，所述感应加热线圈由绝缘柱固定于炉体上，并通过电机引出装置与水冷电缆相连；闪烧样品、闪烧模具、感应加热线圈同轴心线设置，使闪烧电流与感应线圈磁感线方向平行，防止电流路径受到干扰，感应加热恒温区尺寸例如为
进一步的，所述冷却***采用水冷***，水冷***由各种管道阀等相关装置组成，具有断水声光报警自动切断电源功能。Further, the cooling system adopts a water cooling system, and the water cooling system is composed of various pipeline valves and other related devices, and has the function of automatically cutting off the power supply by sound and light alarm when water is cut off.
进一步的，所述真空***由油旋片泵、电磁控制阀(防止因突然停电机械泵油倒灌)、真空计、真空管道和真空阀组成，抽速240L/min，工作真空度≤50Pa(视材料放气有变化)；炉体预抽真空后保持真空状态或充保护性气氛。Further, the vacuum system is composed of an oil rotary vane pump, an electromagnetic control valve (to prevent the mechanical pump from being poured back due to sudden power failure), a vacuum gauge, a vacuum pipeline and a vacuum valve, the pumping speed is 240L/min, and the working vacuum is ≤50Pa (depending on the situation). Material outgassing changes); the furnace body is pre-evacuated and kept in a vacuum state or filled with a protective atmosphere.
进一步的，所述上压头、下压头采用高强度石墨块或硬质合金制造，直径为80～100mm，用于施加压力，同时作为连接闪烧回路的导体。Further, the upper indenter and the lower indenter are made of high-strength graphite blocks or cemented carbide, with a diameter of 80-100 mm, for applying pressure and as conductors for connecting the flashing circuit.
进一步的，作为本发明的创新点之一，所述上电极、下电极材质为磁性钢、石墨、高速钢、硬质合金、铜基合金、钼基合金、钨基合金中的一种或任两种组成的复合电极，电极连接压头将压力传到闪烧样品上实现压力辅助，同时作为将闪烧样品连入闪烧回路的导体；所述上电极、下电极和闪烧样品的接触区域处于感应线圈中心位置，接触闪烧样品的上电极和下电极的端部区域被感应加热的效果最显著，在不使用次外层的作为发热体的情况下，电极可单独作为发热体用于闪烧样品的传导加热；所述复合电极采用由带有磁性的金属材料(如磁性钢、部分高速钢)和耐高温高强度金属基材料(如部分高速钢、硬质合金、钼基合金、钨基合金)堆叠组成，带有磁性的金属材料用于提供电极与闪烧样品接触区域的高效的感应加热，耐高温高强度金属基材料用于承受较高的闪烧压力。Further, as one of the innovative points of the present invention, the material of the upper electrode and the lower electrode is one or any of magnetic steel, graphite, high-speed steel, cemented carbide, copper-based alloy, molybdenum-based alloy, and tungsten-based alloy. A composite electrode with two compositions, the electrode is connected to the pressure head to transmit the pressure to the flash burning sample to achieve pressure assistance, and at the same time acts as a conductor connecting the flash burning sample into the flash burning circuit; the contact between the upper electrode, the lower electrode and the flash burning sample The area is located in the center of the induction coil, and the end areas of the upper and lower electrodes that contact the flash burning sample are most significantly heated by induction. In the case of not using the sub-outer layer as a heating element, the electrodes can be used alone as a heating element. Conductive heating for flash burning samples; the composite electrode is made of magnetic metal materials (such as magnetic steel, part of high-speed steel) and high-temperature resistant and high-strength metal-based materials (such as part of high-speed steel, cemented carbide, molybdenum-based alloys) , tungsten-based alloy) stack, the magnetic metal material is used to provide efficient induction heating of the contact area between the electrode and the flash burning sample, and the high temperature resistant and high-strength metal base material is used to withstand higher flash burning pressure.
进一步的，所述装置还包括控制***，所述控制***采用PLC和高精度数字仪表组合，真彩触摸屏作为人机交互界面，集成操作按钮，并将控制指令和工艺参数下达到PCL控制器和温控表，显示各种工艺过程信息(如：温度、压力、位移和设备工作状态等)并做记录，可以实现手动和自动控制。Further, the device also includes a control system, the control system adopts a combination of PLC and high-precision digital instruments, a true color touch screen is used as a human-computer interaction interface, integrated operation buttons, and the control instructions and process parameters are downloaded to the PCL controller and the PCL controller. The temperature control table displays and records various process information (such as temperature, pressure, displacement and equipment working status, etc.), and can realize manual and automatic control.
本发明的有益效果为：不仅克服了传统闪速烧结技术中的固有缺点，还集成了闪速放电等离子烧结设备的功能，能够以一种更简单的、更紧凑的配置实现国内外学者提出的大部分闪速烧结工艺。同时，可根据被闪烧结材料的电学性质灵活选择闪烧电源，来引发热失控，从而实现最大程度的致密化水平以及样品微观结构的精细调控，对于金属及陶瓷材料具有普适性。并且压力辅助闪速烧结属于目前闪烧学术界和技术界的最新研究方向之一，有望进一步降低闪烧温度和致密化时间。而本发明可轻松实现闪烧过程的压力辅助，可为该研究领域提供一种新的制备手段。此外，本发明在核燃料工业也具有巨大的应用潜力。The beneficial effect of the invention is that it not only overcomes the inherent shortcomings of the traditional flash sintering technology, but also integrates the functions of the flash discharge plasma sintering equipment, so that the proposed method proposed by scholars at home and abroad can be realized in a simpler and more compact configuration. Most flash sintering processes. At the same time, the flash sintering power source can be flexibly selected according to the electrical properties of the flash sintered material to induce thermal runaway, so as to achieve the maximum densification level and fine control of the microstructure of the sample, which is universal for metal and ceramic materials. And pressure-assisted flash sintering is one of the latest research directions in the current flash sintering academic and technical fields, and it is expected to further reduce the flash sintering temperature and densification time. The invention can easily realize the pressure assistance of the flash burning process, and can provide a new preparation method for this research field. In addition, the present invention also has great application potential in the nuclear fuel industry.
附图说明Description of drawings
图1所示为本发明实施例一种压力辅助感应加热真空气氛闪速烧结装置的结构示意图。FIG. 1 is a schematic structural diagram of a pressure-assisted induction heating vacuum atmosphere flash sintering device according to an embodiment of the present invention.
图2所示为实施例中炉体及各***之间的连接关系示意图。FIG. 2 is a schematic diagram showing the connection relationship between the furnace body and each system in the embodiment.
图3所示为闪烧模具示意图。Figure 3 shows a schematic diagram of the flash-burning mold.
图4所示为实施例中复合电极示意图。FIG. 4 is a schematic diagram of the composite electrode in the embodiment.
图5所示为实施例1、2、3、4的样品外观图示及其扫描电镜图片；其中(a)实施例1；(b)实施例2；(c)实施例3；(d)实施例4。Figure 5 shows the appearance diagram of the samples of Examples 1, 2, 3, and 4 and their SEM pictures; (a) Example 1; (b) Example 2; (c) Example 3; (d) Example 4.
图6所示为实施例5、6、7、8的样品外观图示及其扫描电镜图片；其中(a)实施例5；(b)实施例6；(c)实施例7；(d)实施例8。Figure 6 shows the appearance diagram of the samples of Examples 5, 6, 7, and 8 and their SEM pictures; (a) Example 5; (b) Example 6; (c) Example 7; (d) Example 8.
图7所示为实施例9、10、11、12的样品外观图片及其扫描电镜图片；其中(a)实施例9；(b)实施例10；(c)实施例11；(d)实施例12。Figure 7 shows the sample appearance pictures of Examples 9, 10, 11 and 12 and their SEM pictures; (a) Example 9; (b) Example 10; (c) Example 11; (d) Example Example 12.
其中：1-压力传感器；2-上绝缘板；3-上电极板；4-压力框架；5-导线；6-闪烧电源；7-闪烧模具；8-(可移动)下压头；9-下绝缘板；10-伺服电缸；11-下电极板；12-耐高温模具座；13-下电极；14-闪烧样品；15-感应加热电源；16-感应加热线圈；17-上电极；18-炉体；19-上压头；20-后门；21-规管座；22-热电偶；23-真空泵连接座；24-前门；25-观察窗(辐射测温窗)；26-(闪烧模具)最外层；27-(闪烧模具)次外层；28-(闪烧模具)最内层；29-耐高温高强度金属基材料；30-带磁性的金属材料。Among them: 1- pressure sensor; 2- upper insulating plate; 3- upper electrode plate; 4- pressure frame; 5- wire; 6- flash burning power supply; 7- flash burning mold; 8- (removable) lower pressure head; 9- Lower insulating plate; 10- Servo electric cylinder; 11- Lower electrode plate; 12- High temperature mold base; 13- Lower electrode; 14- Flash burning sample; 15- Induction heating power supply; 16- Induction heating coil; 17- Upper electrode; 18-furnace body; 19-upper pressure head; 20-back door; 21-gauge tube seat; 22-thermocouple; 23-vacuum pump connection seat; 24-front door; 25-observation window (radiation temperature measurement window); 26-(flash-burning mold) outermost layer; 27-(flash-burning mold) secondary outer layer; 28-(flash-burning mold) innermost layer; 29-high temperature resistant and high-strength metal base material; 30-magnetic metal material .
具体实施方式Detailed ways
下文将结合具体附图详细描述本发明具体实施例。应当注意的是，下述实施例中描述的技术特征或者技术特征的组合不应当被认为是孤立的，它们可以被相互组合从而达到更好的技术效果。Hereinafter, specific embodiments of the present invention will be described in detail with reference to the accompanying drawings. It should be noted that the technical features or combinations of technical features described in the following embodiments should not be considered isolated, and they can be combined with each other to achieve better technical effects.
如图1所示，本发明实施例一种压力辅助感应加热真空气氛闪速烧结装置，包括炉体18、压力***、闪烧***、感应加热***、冷却***和真空***；所述压力***包括相对于炉体18顶部固定设置的上压头19，及可移动下压头8及伺服电缸10；上压头19端部设置上电极17，下压头8端部设置下电极13；所述伺服电缸10带动下压头8运动；上压头19、下压头8相对运动时带动所述上电极17、下电极13为闪烧样品14提供压力；所述闪烧***包括闪烧电源6、闪烧模具7、所述上电极17及所述下电极13；所述闪烧***为所述闪烧样品14提供闪烧回路；所述感应加热***用于为闪烧样品14加热及保温；所述感应加热***设置在所述炉体18内；所述冷却***，用于冷却所述炉体18；所述真空***，用于对所述炉体18内部抽真空。As shown in FIG. 1, a pressure-assisted induction heating vacuum atmosphere flash sintering device according to an embodiment of the present invention includes a
优选的，上压头19固定于炉顶，通过上电极板3(钨铜板)将上电极17引出炉体，上电极板3与压力框架4上固定的压力传感器1之间采用上绝缘板2绝缘；可移动下压头8通过下电极板11将下电极13引出炉体，并与伺服电缸10连接；可移动下压头8与炉体18之间采用动密封；下电极板11通过下绝缘板9与压力框架4以及伺服电缸10隔热绝缘。闪烧样品14及模具7与感应线圈16同轴心线放置，以使闪烧电流与感应线圈16磁感线方向平行，防止电流路径受到干扰；闪烧模具7由耐高温模具座12支撑。感应线圈通过电极引出装置与感应加热电源15上的水冷电缆相连。闪烧电源6通过导线5和上电极板3、下电极板11连接形成闪烧回路。Preferably, the
优选的，如图2所示，双层水冷炉体18设有前门24、后门20。前门24设置有观察窗25(测温窗)，后门20设置有规管座21(用于放置真空测量规管)、热电偶22(可通过接触测量模具或电极上任意一点温度)、真空泵连接座23。Preferably, as shown in FIG. 2 , the double-layer water-cooled
优选的，闪烧模具7结构如图3所示，为中空圆柱形，具有3层结构，中空部分放置闪烧样品14，最外层26为耐高温绝热材料(如多孔莫来石或碳毡等)，用于降低闪烧模具内部的温度梯度；次外层27为耐高温金属基材料或石墨，如高速钢、硬质合金等(在闪烧压力较高的条件下使用)，又如高强度石墨等(在闪烧压力较低的条件下使用)，次外层27用于承受闪烧压力(即使最内层28破裂也不影响其承压)，并能被感应加热作为发热体，从而传导加热闪烧样品，使其达到闪烧温度，灵活选择次外层27材料，可施加高达2GPa的闪烧压力，可提供高达1500℃的闪烧温度；最内层28为耐高温绝缘材料(如氧化铝、氮化硼陶瓷等)，用于闪烧样品14与次外层27在闪烧温度下的电绝缘(即使最内层28破裂也不影响闪烧样品14与次外层27的电绝缘)，保证闪烧电源的电流全部通过闪烧样品14，从而达到闪烧的目的；所述闪烧模具7由耐高温模具座12支撑，用于减小闪烧模具7与下压头8的热传导作用，上压头19在闪烧过程中不与闪烧模具7接触，避免电流通过闪烧模具7。闪烧样品14直径最大尺寸可达30mm，高度视闪烧电源6参数而定。电极13、17可采用单一结构的只含一种材料的整体电极，也可采用如图4所示的复合结构电极由耐高温高强度金属基材料29(部分高速钢、硬质合金、钼基合金、钨基合金)和带有磁性的金属材料30(如磁性钢、部分高速钢)堆叠组成，带有磁性的金属材料30用于提供电极与样品接触区域的高效的感应加热，耐高温高强度金属基材料29用于承受较高的闪烧压力。Preferably, the structure of the
优选的，闪烧模具7结构如图3所示，最外层26为耐高温绝热材料(如多孔莫来石或碳毡等)；次外层27为耐高温金属基材料或石墨，如高速钢、硬质合金等(在承压较高的条件下使用)，又如高强度石墨等(在承压较低时使用，同时作为发热筒，可提供800～1500℃的预热温度)；最内层28为耐高温绝缘材料(如氧化铝、氮化硼陶瓷等)。闪烧样品直径最大尺寸可达30mm，高度视闪烧电源参数而定。电极13、17可采用单一结构的只含一种材料的整体电极，也可采用如图4所示的复合结构电极，由高温强度金属基材料29(如纯钨、高速钢、硬质合金等)和带磁性的金属材料30(如碳钢等)组成。这种复合结构电极可以更好地集中感应加热能量并具有较好的高温承压能力。Preferably, the structure of the flash-burning
实施例1Example 1
本实施例为商用ZnO粉末的压力辅助闪速烧结。感应加热预热温度设定为770℃，压力为26MPa，样品直径为6.4mm。闪烧电源采用一台低功率脉冲直流电源，初始电场强度约为80V/cm,频率1000Hz，脉宽128μs。本实施例将闪烧电流设置为0A(即不打开闪烧电源)，在预热温度及恒定压力下保温30s，样品外观照片及微观结构如图5中(a)所示，其致密度为71.1％，晶粒尺寸为130.1nm。This example is pressure-assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature was set to 770 °C, the pressure was 26 MPa, and the sample diameter was 6.4 mm. The flash burning power supply adopts a low-power pulsed DC power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128μs. In this example, the flash burning current is set to 0A (that is, the flash burning power supply is not turned on), and the temperature is kept for 30s under the preheating temperature and constant pressure. 71.1%, the grain size is 130.1nm.
实施例2Example 2
本实施例为商用ZnO粉末的压力辅助闪速烧结。感应加热预热温度设定为770℃，压力为26MPa，样品直径为6.4mm。闪烧电源采用一台低功率脉冲直流电源，初始电场强度约为80V/cm,频率1000Hz，脉宽128μs。本实施例将闪烧电流设置为50A，在预热温度及恒定压力下打开电源，30s后立即关闭，样品外观照片及微观结构如图5中(b)所示，其致密度为77.3％，晶粒尺寸为200.7nm。This example is pressure-assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature was set to 770 °C, the pressure was 26 MPa, and the sample diameter was 6.4 mm. The flash burning power supply adopts a low-power pulsed DC power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128μs. In this example, the flash current is set to 50A, the power is turned on at the preheating temperature and constant pressure, and turned off immediately after 30s. The appearance photo and microstructure of the sample are shown in (b) in Figure 5, and the density is 77.3%. The grain size is 200.7 nm.
实施例3Example 3
本实施例为商用ZnO粉末的压力辅助闪速烧结。感应加热预热温度设定为770℃，压力为26MPa，样品直径为6.4mm。闪烧电源采用一台低功率脉冲直流电源，初始电场强度约为80V/cm,频率1000Hz，脉宽128μs。本实施例将闪烧电流设置为100A，在预热温度及恒定压力下打开电源，30s后立即关闭，样品外观照片及微观结构如图5中(c)所示，其致密度为91.9％，晶粒尺寸为687.5nm。This example is pressure-assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature was set to 770 °C, the pressure was 26 MPa, and the sample diameter was 6.4 mm. The flash burning power supply adopts a low-power pulsed DC power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128μs. In this example, the flash current is set to 100A, the power is turned on at the preheating temperature and constant pressure, and turned off immediately after 30s. The grain size is 687.5 nm.
实施例4Example 4
本实施例为商用ZnO粉末的压力辅助闪速烧结。感应加热预热温度设定为770℃，压力为26MPa，样品直径为6.4mm。闪烧电源采用一台低功率脉冲直流电源，初始电场强度约为80V/cm,频率1000Hz，脉宽128μs。本实施例将闪烧电流设置为150A，在预热温度及恒定压力下打开电源，30s后立即关闭，样品外观照片及微观结构如图5中(d)所示，其致密度为95.2％，晶粒尺寸为912.4nm。This example is pressure-assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature was set to 770 °C, the pressure was 26 MPa, and the sample diameter was 6.4 mm. The flash burning power supply adopts a low-power pulsed DC power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128μs. In this example, the flash current is set to 150A, the power is turned on at the preheating temperature and constant pressure, and turned off immediately after 30s. The appearance photo and microstructure of the sample are shown in (d) in Figure 5. The grain size is 912.4 nm.
实施例5Example 5
由于核燃料，如二氧化铀(UO2)等在实验室使用的限制，本实施例采用商用纳米CeO2粉末来模拟纳米结构二氧化铀燃料芯块的压力辅助闪速烧结制备。感应加热预热温度设定为750℃，压力为810MPa，样品直径为6.0mm。闪烧电源采用一台低功率直流恒流电源，初始电场强度约为500V/cm。本实施例将闪烧电流设置为0A(即不打开闪烧电源)，在预热温度及恒定压力下保温3min，样品外观照片及微观结构如图6中(a)所示，其致密度为91.2％，晶粒尺寸小于100nm。Due to the limited use of nuclear fuels such as uranium dioxide (UO 2 ) in the laboratory, commercial nano-CeO 2 powder is used in this example to simulate the pressure-assisted flash sintering of nano-structured uranium dioxide fuel pellets. The induction heating preheating temperature was set to 750 °C, the pressure was 810 MPa, and the sample diameter was 6.0 mm. The flash burning power supply adopts a low-power DC constant current power supply, and the initial electric field intensity is about 500V/cm. In this example, the flash burning current is set to 0A (that is, the flash burning power supply is not turned on), and the temperature is kept at a preheating temperature and a constant pressure for 3 minutes. The appearance photo and microstructure of the sample are shown in (a) in Figure 6. 91.2%, the grain size is less than 100nm.
实施例6Example 6
由于核燃料，如二氧化铀(UO2)等在实验室使用的限制，本实施例采用商用纳米CeO2粉末来模拟纳米结构二氧化铀燃料芯块的压力辅助闪速烧结制备。感应加热预热温度设定为750℃，压力为810MPa，样品直径为6.0mm。闪烧电源采用一台低功率直流恒流电源，初始电场强度约为500V/cm。本实施例将闪烧电流设置为1A，在预热温度及恒定压力下打开电源，电流达到峰值1s后立即关闭电源，整个过程持续约3min，样品外观照片及微观结构如图6中(b)所示，其致密度为92.5％，晶粒尺寸小于100nm。Due to the limited use of nuclear fuels such as uranium dioxide (UO 2 ) in the laboratory, commercial nano-CeO 2 powder is used in this example to simulate the pressure-assisted flash sintering of nano-structured uranium dioxide fuel pellets. The induction heating preheating temperature was set to 750 °C, the pressure was 810 MPa, and the sample diameter was 6.0 mm. The flash burning power supply adopts a low-power DC constant current power supply, and the initial electric field intensity is about 500V/cm. In this example, the flash current is set to 1A, the power is turned on at the preheating temperature and constant pressure, and the power is turned off immediately after the current reaches the peak value for 1s. The whole process lasts about 3min. As shown, its density is 92.5% and the grain size is less than 100 nm.
实施例7Example 7
由于核燃料，如二氧化铀(UO2)等在实验室使用的限制，本实施例采用商用纳米CeO2粉末来模拟纳米结构二氧化铀燃料芯块的压力辅助闪速烧结制备。感应加热预热温度设定为750℃，压力为810MPa，样品直径为6.0mm。闪烧电源采用一台低功率直流恒流电源，初始电场强度约为500V/cm。本实施例将闪烧电流设置为1A，在预热温度及恒定压力下打开电源，电流达到峰值5s后立即关闭电源，整个过程持续约3min，样品外观照片及微观结构如图6中(c)所示，其致密度为94.7％，晶粒尺寸小于100nm。Due to the limited use of nuclear fuels such as uranium dioxide (UO 2 ) in the laboratory, commercial nano-CeO 2 powder is used in this example to simulate the pressure-assisted flash sintering of nano-structured uranium dioxide fuel pellets. The induction heating preheating temperature was set to 750 °C, the pressure was 810 MPa, and the sample diameter was 6.0 mm. The flash burning power supply adopts a low-power DC constant current power supply, and the initial electric field intensity is about 500V/cm. In this example, the flash current is set to 1A, the power is turned on at the preheating temperature and constant pressure, and the power is turned off immediately after the current reaches the peak value for 5s. The whole process lasts about 3min. The appearance photo and microstructure of the sample are shown in Figure 6(c) As shown, its density is 94.7% and the grain size is less than 100 nm.
实施例8Example 8
由于核燃料，如二氧化铀(UO2)等在实验室使用的限制，本实施例采用商用纳米CeO2粉末来模拟纳米结构二氧化铀燃料芯块的压力辅助闪速烧结制备。感应加热预热温度设定为750℃，压力为810MPa，样品直径为6.0mm。闪烧电源采用一台低功率直流恒流电源，初始电场强度约为500V/cm。本实施例将闪烧电流设置为1A，在预热温度及恒定压力下打开电源，电流达到峰值10s后立即关闭电源，整个过程持续约3min，样品外观照片及微观结构如图6中(d)所示，其致密度为96.5％，晶粒尺寸小于100nm。Due to the limited use of nuclear fuels such as uranium dioxide (UO 2 ) in the laboratory, commercial nano-CeO 2 powder is used in this example to simulate the pressure-assisted flash sintering of nano-structured uranium dioxide fuel pellets. The induction heating preheating temperature was set to 750 °C, the pressure was 810 MPa, and the sample diameter was 6.0 mm. The flash burning power supply adopts a low-power DC constant current power supply, and the initial electric field intensity is about 500V/cm. In this example, the flash current is set to 1A, the power is turned on at the preheating temperature and constant pressure, and the power is turned off immediately after the current reaches the peak value for 10s. The whole process lasts about 3min. The appearance photo and microstructure of the sample are shown in Figure 6(d) As shown, the density is 96.5% and the grain size is less than 100 nm.
实施例9Example 9
本实施例为商用雾化Al-12Si粉末的压力辅助闪速烧结。该粉末在室温下便具有良好的导电性，因此采用一台大功率脉冲直流电源来强制引发热失控，实现闪烧，无需采用感应加热预热。压力为631MPa，样品直径为10.5mm，初始电场强度约为10V/cm,频率30kHz，脉宽100μs。本实施例将闪烧电流设置为1200A，在室温及恒定压力下打开电源，1s后立即关闭，样品外观照片及微观结构如图7中(a)所示，其致密度为93.0％,硬度为66HV。This example is pressure-assisted flash sintering of commercial atomized Al-12Si powder. The powder has good electrical conductivity at room temperature, so a high-power pulsed DC power supply is used to force thermal runaway to achieve flash burn without induction heating. The pressure is 631MPa, the sample diameter is 10.5mm, the initial electric field strength is about 10V/cm, the frequency is 30kHz, and the pulse width is 100μs. In this example, the flash current is set to 1200A, the power is turned on at room temperature and constant pressure, and immediately turned off after 1 s. The appearance photo and microstructure of the sample are shown in (a) in Figure 7. The density is 93.0% and the hardness is 66HV.
实施例10Example 10
本实施例为商用雾化Al-12Si粉末的压力辅助闪速烧结。该粉末在室温下便具有良好的导电性，因此采用一台大功率脉冲直流电源来强制引发热失控，实现闪烧，无需采用感应加热预热。压力为631MPa，样品直径为10.5mm，初始电场强度约为10V/cm,频率30kHz，脉宽100μs。本实施例将闪烧电流设置为1200A，在室温及恒定压力下打开电源，10s后立即关闭，样品外观照片及微观结构如图7中(b)所示，其致密度为97.9％,硬度为98HV。This example is pressure-assisted flash sintering of commercial atomized Al-12Si powder. The powder has good electrical conductivity at room temperature, so a high-power pulsed DC power supply is used to force thermal runaway to achieve flash burn without induction heating. The pressure is 631MPa, the sample diameter is 10.5mm, the initial electric field strength is about 10V/cm, the frequency is 30kHz, and the pulse width is 100μs. In this example, the flash current is set to 1200A, the power is turned on at room temperature and constant pressure, and turned off immediately after 10s. The appearance photo and microstructure of the sample are shown in (b) in Figure 7. The density is 97.9% and the hardness is 98HV.
实施例11Example 11
本实施例为商用雾化Al-12Si粉末的压力辅助闪速烧结。该粉末在室温下便具有良好的导电性，因此采用一台大功率脉冲直流电源来强制引发热失控，实现闪烧，无需采用感应加热预热。压力为631MPa，样品直径为10.5mm，初始电场强度约为10V/cm,频率30kHz，脉宽100μs。本实施例将闪烧电流设置为1200A，在室温及恒定压力下打开电源，20s后立即关闭，样品外观照片及微观结构如图7中(c)所示，其致密度为99.8％,硬度为81HV。This example is pressure-assisted flash sintering of commercial atomized Al-12Si powder. The powder has good electrical conductivity at room temperature, so a high-power pulsed DC power supply is used to force thermal runaway to achieve flash burn without induction heating. The pressure is 631MPa, the sample diameter is 10.5mm, the initial electric field strength is about 10V/cm, the frequency is 30kHz, and the pulse width is 100μs. In this example, the flashing current is set to 1200A, the power is turned on at room temperature and constant pressure, and immediately turned off after 20s. The appearance photo and microstructure of the sample are shown in (c) in Figure 7. The density is 99.8% and the hardness is 81HV.
实施例12Example 12
本实施例为商用雾化Al-12Si粉末的压力辅助闪速烧结。该粉末在室温下便具有良好的导电性，因此采用一台大功率脉冲直流电源来强制引发热失控，实现闪烧，无需采用感应加热预热。压力为631MPa，样品直径为10.5mm，初始电场强度约为10V/cm,频率30kHz，脉宽100μs。本实施例将闪烧电流设置为1200A，在室温及恒定压力下打开电源，30s后立即关闭，样品外观照片及微观结构如图7中(d)所示，其致密度为98.3％,硬度为101HV。This example is pressure-assisted flash sintering of commercial atomized Al-12Si powder. The powder has good electrical conductivity at room temperature, so a high-power pulsed DC power supply is used to force thermal runaway to achieve flash burn without induction heating. The pressure is 631MPa, the sample diameter is 10.5mm, the initial electric field strength is about 10V/cm, the frequency is 30kHz, and the pulse width is 100μs. In this example, the flash current is set to 1200A, the power is turned on at room temperature and constant pressure, and immediately turned off after 30s. The appearance photo and microstructure of the sample are shown in (d) in Figure 7. The density is 98.3%, and the hardness is 101HV.
本文虽然已经给出了本发明的几个实施例，但是本领域的技术人员应当理解，在不脱离本发明精神的情况下，可以对本文的实施例进行改变。上述实施例只是示例性的，不应以本文的实施例作为本发明权利范围的限定。Although several embodiments of the present invention have been presented herein, those skilled in the art should understand that changes may be made to the embodiments herein without departing from the spirit of the present invention. The above-mentioned embodiments are only exemplary, and the embodiments herein should not be construed as limiting the scope of the rights of the present invention.
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