CN1389317A - Stepped cooling and continuous casting method of massive amorphous alloy - Google Patents
Stepped cooling and continuous casting method of massive amorphous alloy Download PDFInfo
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Abstract
Description
技术领域：Technical field:
本发明涉及一种非晶合金连续铸造方法，尤其涉及一种大块非晶合金分步冷却连续铸造方法，属于金属材料铸造技术领域。The invention relates to a continuous casting method of an amorphous alloy, in particular to a stepwise cooling continuous casting method of a bulk amorphous alloy, which belongs to the technical field of metal material casting.
背景技术：Background technique:
与普通晶态合金相比，非晶合金具有许多优越的力学性能和物理化学性能，因此，三维方向尺寸均在1mm以上的块体铸造非晶合金自上世纪九十年代开发成功以来，受到了材料科学与工程界的广泛关注。不过，该类材料在铸造时仍要求有较高的冷却速度，其制备方法目前主要局限于整体液淬、铜模铸造、金属型高压铸造、真空吸铸、挤压铸造、电弧熔化随炉冷凝等(富莉，缓冷大块非晶合金的发展现状，金属功能材料，1998，增刊，p39-53)。Compared with ordinary crystalline alloys, amorphous alloys have many superior mechanical properties and physical and chemical properties. Therefore, bulk casting amorphous alloys with three-dimensional dimensions of more than 1 mm have been developed since the 1990s. extensive attention in the materials science and engineering community. However, this type of material still requires a high cooling rate during casting, and its preparation methods are currently mainly limited to overall liquid quenching, copper mold casting, metal high pressure casting, vacuum suction casting, squeeze casting, arc melting and furnace condensation etc. (Fu Li, Development Status of Slowly Cooled Bulk Amorphous Alloys, Metal Functional Materials, 1998, Supplement, p39-53).
个别研究者还对单向凝固大块非晶进行了实验。其实现手段之一是，在真空电弧炉的水冷坩锅上开一凹槽，放入合金料，在电弧从一端向另一端移动化料的同时，边熔化边凝固。另一种单向凝固非晶合金的方法，则是将置于柱形坩锅中的合金料在单向凝固炉中熔化，然后连同坩锅一起向下淬入冷却液中，在下降过程中逐渐完成合金液向非晶体的凝固(Z.P.Lu，T.T.Goh，Y.Li and S.C.Ng，Glass formation in La-based La-Al-Ni-Cu-(Co)alloys by Bridgmansolidification and their glass forming ability，Acta Materialia，1999，Vol.7，p2215-2224)。Individual researchers have also conducted experiments on unidirectionally solidified bulk amorphous. One of the means of realization is to open a groove on the water-cooled crucible of the vacuum electric arc furnace, put the alloy material in, and melt and solidify while the arc moves the material from one end to the other. Another method for one-way solidification of amorphous alloys is to melt the alloy material placed in a cylindrical crucible in a one-way solidification furnace, and then quench it together with the crucible into the cooling liquid. Gradually complete the solidification of alloy liquid to amorphous (Z.P.Lu, T.T.Goh, Y.Li and S.C.Ng, Glass formation in La-based La-Al-Ni-Cu-(Co)alloys by Bridgmansolidification and their glass forming ability, Acta Materialia, 1999, Vol. 7, p2215-2224).
事实上，与晶态材料不同，非晶形成过程中不产生凝固组织花样，相应不存在组织的取向问题，任何铸造方法得到的非晶在结构和性能上没有本质的区别，因此与其它大块非晶铸造方法相比，上述两种单向凝固技术并无多少优点，它们同样要求使用和铸件一样长的铸型。In fact, unlike crystalline materials, there is no solidification structure pattern during the formation of amorphous materials, and there is no problem with the orientation of the structure. The amorphous material obtained by any casting method has no essential difference in structure and performance, so it is different from other bulk materials. Compared with the amorphous casting method, the above two unidirectional solidification techniques do not have many advantages, and they also require the use of a mold as long as the casting.
相比之下，大块非晶合金若能实现连续铸造，就可简化铸型，显著提高生产效率。然而，常规连铸时，合金液是以一定的过热温度浇入冷凝器中的，冷凝器不仅要导出合金液自熔点温度降至玻璃转变温度时放出的热量，而且要导出从浇注温度降至熔点温度时的过热热量，由此显著影响了合金液在冷凝器中的冷却强度，使大块非晶合金的连铸变得非常困难。In contrast, if the continuous casting of large amorphous alloys can be realized, the casting mold can be simplified and the production efficiency can be significantly improved. However, during conventional continuous casting, the alloy liquid is poured into the condenser at a certain superheated temperature. The superheated heat at the melting point temperature significantly affects the cooling strength of the alloy liquid in the condenser, making continuous casting of bulk amorphous alloys very difficult.
发明内容：Invention content:
本发明的目的在于针对现有技术的不足，提供一种大块非晶合金分步冷却连续铸造方法，改变常规金属材料连铸时的冷却工艺，降低进入冷凝器的液态金属温度，实现大块非晶合金的连铸，经济地为非晶合金零件的制造提供坯料。The purpose of the present invention is to address the deficiencies of the prior art, to provide a step-by-step cooling continuous casting method for large amorphous alloys, to change the cooling process during continuous casting of conventional metal materials, to reduce the temperature of the liquid metal entering the condenser, and to achieve bulk amorphous alloys. The continuous casting of amorphous alloys economically provides blanks for the manufacture of amorphous alloy parts.
为实现这样的目的，本发明的技术方案中，采用了分步冷却的连续铸造方法，在连铸装置中增加了液流分散器，合金液在进入冷凝器之前，先经过液流分散器的冷却，再浇入铸型，进一步冷却到玻璃化转变温度以下，冷凝形成非晶。In order to achieve such purpose, in the technical scheme of the present invention, the continuous casting method of stepwise cooling is adopted, and the liquid flow disperser is added in the continuous casting device, and the alloy liquid passes through the liquid flow disperser before entering the condenser. Cool, then pour into the mold, further cool to below the glass transition temperature, and condense to form amorphous.
根据经典形核理论，过冷合金液形核的孕育时间随着过冷度的增大先缩短，后延长，即呈所谓的C曲线形状。合金液形成非晶的关键是要在C曲线的鼻尖温度Tn以上快速冷却，一旦合金液被成功过冷至Tn以下，对冷却强度的要求将迅速降低。形核C曲线的位置还和铸型对液态合金形核的触发能力有关。随着铸型触发形核能力的降低，C曲线右移，形成非晶的临界冷却速度降低。当非均质形核被完全抑制时，该临界冷却速度成数量级降低。依据这样的科学原理，本发明的具体连续铸造方法按如下步骤进行：According to the classical nucleation theory, the incubation time of supercooled alloy liquid nucleation first shortens and then prolongs with the increase of supercooling degree, which is in the shape of so-called C curve. The key to the formation of amorphous alloy liquid is to cool rapidly above the nose temperature Tn of the C curve. Once the alloy liquid is successfully supercooled to below Tn , the requirement for cooling intensity will decrease rapidly. The position of the nucleation C-curve is also related to the triggering ability of the casting mold to the nucleation of the liquid alloy. With the reduction of the ability of the mold to trigger nucleation, the C curve shifts to the right, and the critical cooling rate for the formation of amorphous decreases. This critical cooling rate decreases by orders of magnitude when heterogeneous nucleation is completely suppressed. According to such scientific principle, concrete continuous casting method of the present invention is carried out as follows:
第一步：将大块非晶合金料在坩锅中熔化、过热至其熔点温度以上200-300℃，并在该温度进行10-30分钟的保温处理。Step 1: Melt the bulk amorphous alloy material in a crucible, overheat it to 200-300°C above its melting point, and carry out heat preservation treatment at this temperature for 10-30 minutes.
合金在坩锅中进行熔化过热可采用电阻加热、感应加热或其它加热方式，为尽力减轻坩锅与合金液间的反应，坩锅材料应尽可能选用化学稳定性和热稳定性好的材料制造。The melting and overheating of the alloy in the crucible can use resistance heating, induction heating or other heating methods. In order to minimize the reaction between the crucible and the alloy liquid, the crucible material should be made of materials with good chemical and thermal stability as much as possible. .
第二步：提起坩锅柱塞，使合金液自坩锅底部的浇口流出，进入下方的液流分散器。在此合金液被分散成许多小的流股，在其下落过程中，与惰性气体进行强制换热，同时向外辐射传热，其温度被迅速冷却至Tn温度左右。Step 2: Lift the plunger of the crucible so that the alloy liquid flows out from the gate at the bottom of the crucible and enters the liquid flow distributor below. Here, the alloy liquid is dispersed into many small streams. During its falling, it conducts forced heat exchange with the inert gas, and at the same time radiates heat to the outside, and its temperature is rapidly cooled to about Tn temperature.
合金液的流量可通过调节柱塞的提起高度来控制。合金液冷却强度可通过调整惰性冷却气体的压力、温度或流动状态来控制。具体说，若要使合金液流较快降温，可以增大惰性气体的压力。由于大块非晶合金的化学活性一般较高，其铸造过程要在密闭的空间进行，当其中的气体压力增大后，金属液流与气体间的换热加强。更为有效的提高合金液流冷却速度的手段是增大惰性气体和合金液间的相对运动速度，即安装风扇，迫使气体进行强制对流。为保证合金液在到达冷凝器时的温度接近Tn，还可以适当增加液流分散器至冷凝器的距离，即延长液流束的散热时间来降低合金液的温度。液流分散器可采用耐火材料材质制成。The flow rate of the alloy liquid can be controlled by adjusting the lifting height of the plunger. The cooling strength of the alloy liquid can be controlled by adjusting the pressure, temperature or flow state of the inert cooling gas. Specifically, if the alloy liquid flow is to be cooled faster, the pressure of the inert gas can be increased. Because the chemical activity of bulk amorphous alloy is generally high, its casting process should be carried out in a closed space. When the gas pressure in it increases, the heat exchange between the metal liquid flow and the gas is strengthened. A more effective way to increase the cooling speed of the alloy liquid flow is to increase the relative movement speed between the inert gas and the alloy liquid, that is, to install a fan to force the gas to carry out forced convection. In order to ensure that the temperature of the alloy liquid when it reaches the condenser is close to T n , the distance from the liquid flow disperser to the condenser can be appropriately increased, that is, the cooling time of the liquid flow can be extended to reduce the temperature of the alloy liquid. The liquid flow disperser can be made of refractory material.
第三步：温度在Tn左右的低温合金液被浇入铸型，并被进一步冷却到玻璃化转变温度以下，冷凝形成非晶。为加强冷却，可用冷却液对已凝固相进行强制冷却。Step 3: The low-temperature alloy liquid with a temperature around Tn is poured into the mold, and is further cooled below the glass transition temperature, and condenses to form amorphous. In order to enhance the cooling, the solidified phase can be forced to cool with cooling liquid.
本发明用非晶材料制造冷凝器，或在晶态材料冷凝器的表面涂一层非晶涂料，这样可减轻或消除冷凝器对合金形核的触发作用，有利于提高非晶铸锭的截面尺寸。The present invention uses amorphous materials to manufacture condensers, or coats a layer of amorphous coating on the surface of crystalline material condensers, which can reduce or eliminate the triggering effect of condensers on alloy nucleation, and is conducive to improving the cross-section of amorphous ingots size.
本发明的液态合金在从液流分散器流出并下落的过程中，由于只是受到惰性冷却气体的作用，不和任何固态容器接触，避免了合金液以外的固相物质的触发形核作用，因此合金液在向Tn温度冷却的过程中不会发生结晶。而在流入冷凝器后，由于温度已接近或低于Tn，在相对低的冷却速度下即可形成非晶，因此最终能连续铸造出较大尺寸的非晶合金锭。In the process of flowing out and falling from the liquid flow disperser, the liquid alloy of the present invention is only subjected to the effect of the inert cooling gas and is not in contact with any solid container, thus avoiding the triggering nucleation of solid phase substances other than the alloy liquid, so The alloy liquid will not crystallize in the process of cooling to T n temperature. After flowing into the condenser, since the temperature is close to or lower than T n , amorphous alloys can be formed at a relatively low cooling rate, so larger-sized amorphous alloy ingots can finally be cast continuously.
液流分散器构成本发明的重要环节。由于合金液温度在降低到Tn温度时，粘度很大，流动能力极差，在以集中的流股进入到铸型中时不易完整地充满铸型。使用了液流分散器后，在设计上保证从分散器排出的流束的截面形状与铸锭横截面相近，就可克服低温合金液充型能力差的问题。当非晶铸锭为圆筒、圆柱这样的回旋体时，可以让分散器在浇注过程中进行旋转，由此可进一步改善冷凝器中各处液面高度的均匀性。The liquid flow disperser forms an important part of the present invention. Since the temperature of the alloy liquid is lowered to the Tn temperature, the viscosity is very high, and the flow ability is extremely poor, and it is difficult to completely fill the mold when it enters the mold as a concentrated stream. After the liquid flow disperser is used, the design ensures that the cross-sectional shape of the stream discharged from the disperser is similar to the cross-section of the ingot, so that the problem of poor mold filling ability of the low-temperature alloy liquid can be overcome. When the amorphous ingot is a rotating body such as a cylinder or a cylinder, the disperser can be rotated during the pouring process, thereby further improving the uniformity of the liquid level in the condenser.
液流分散器还可用来控制进入冷凝器的液态金属的流量。若要提高连铸速度，可以适当增大分散器流出孔的总截面积，并通过增大坩锅柱塞的开启程度来提高进入分散器中的合金液的流量。Liquid flow dispersers can also be used to control the flow of liquid metal into the condenser. To increase the continuous casting speed, the total cross-sectional area of the outlet holes of the disperser can be appropriately increased, and the flow rate of the alloy liquid entering the disperser can be increased by increasing the opening degree of the crucible plunger.
本发明工艺方法简单，不需很多的设备投入，却具有显著的效果，实现了大块非晶合金的连续铸造，所制备的非晶具有和铜模重力铸造非晶相当的力学和物理化学性能。The process method of the invention is simple, does not require a lot of equipment investment, but has remarkable effects, realizes the continuous casting of bulk amorphous alloys, and the prepared amorphous has mechanical and physical and chemical properties equivalent to those of copper mold gravity casting amorphous .
使用本发明连铸方法生产的非晶合金锭，可用作制造单件、小批量非晶合金零件的坯料，由此显著缩短零件的生产周期，节约昂贵的模具制造费用。该类非晶合金坯料还可重新加热到过冷液相区，进行轧制或挤压成形，得到非晶板材、线材，或尺寸更大、形状更为复杂的其它非晶材质的零件。The amorphous alloy ingot produced by the continuous casting method of the invention can be used as a blank for manufacturing single-piece and small-batch amorphous alloy parts, thereby significantly shortening the production cycle of parts and saving expensive mold manufacturing costs. This type of amorphous alloy billet can also be reheated to the supercooled liquid phase region for rolling or extrusion forming to obtain amorphous plates, wires, or other amorphous parts with larger sizes and more complex shapes.
附图说明及具体实施方式：Description of drawings and specific implementation methods:
为更好地理解本发明的技术方案，以下结合附图及具体实施例作进一步描述。In order to better understand the technical solution of the present invention, further description will be made below in conjunction with the accompanying drawings and specific embodiments.
图1为本发明采用的连铸装置结构示意图。Fig. 1 is a structural schematic diagram of the continuous casting device adopted in the present invention.
如图所示，本发明的连铸装置在现有装置的基础上增加了一个液流分散器4，坩锅1的外面有加热元件3，坩锅1内的中间置有可调节流量的柱塞2，坩锅1的下方有一个液流分散器4，液流分散器4下方有充有冷却液7的冷凝器6。As shown in the figure, the continuous casting device of the present invention adds a liquid flow disperser 4 on the basis of the existing device. There is a heating element 3 on the outside of the crucible 1, and a column with an adjustable flow rate is placed in the middle of the crucible 1. There is a liquid flow diffuser 4 under the plug 2 and the crucible 1, and a condenser 6 filled with cooling liquid 7 is arranged under the liquid flow diffuser 4.
合金在坩锅1中熔化过热(电阻加热、感应加热或其它加热方式均可)，浇入耐火材料材质的液流分散器4，其流量可通过调节柱塞2的提起高度来控制。合金液在经过液流分散器4后被分成许多细的流股，这样的流股在自由下落的过程中被冷却，冷却强度通过调整惰性冷却气体的种类、温度或流量来控制，保证合金液在到达冷凝器6时的温度接近Tn。低温合金液在冷凝器6中完成向非晶体的转变，铸成非晶连铸件8。The alloy is melted and overheated in the crucible 1 (resistance heating, induction heating or other heating methods are acceptable), and poured into the liquid flow distributor 4 made of refractory material, and its flow rate can be controlled by adjusting the lifting height of the plunger 2 . The alloy liquid is divided into many fine streams after passing through the liquid flow disperser 4, and such streams are cooled in the process of free fall, and the cooling intensity is controlled by adjusting the type, temperature or flow of the inert cooling gas to ensure that the alloy liquid The temperature on reaching the condenser 6 is close to T n . The low-temperature alloy liquid is transformed into amorphous in the condenser 6 and cast into an amorphous continuous casting 8 .
本发明的一个实施例，采用如图1所示的大块非晶合金连续铸造装置，进行了Zr55Al10Cu30Ni5、Zr60Al10Cu15Ni10Pd5和Zr41.2Ti13.8Cu12.5Ni10Be22.5合金的连铸。合金的熔化和浇注过程在相对压力为5×10-6Pa的惰性高纯氩气体的保护下进行。合金首先在刚玉质坩锅中以高频感应加热方式进行熔化、保温，底注进入石英玻璃材质的多孔分散器，其孔径为3毫米。合金液在此被分散形成流束后下落浇入黄铜基质、表面涂有非晶涂层的冷凝器中。冷凝器中通水冷却，同时用镓铟合金液对已凝部分进行冷却，使大块非晶合金过冷液体在冷凝器中完成向非晶的转变。为使冷凝器中各处液面尽可能均匀一致，试验中始终使分散器处于缓慢转动状态。利用该方法，最终获得了直径30mm、长500mm的Zr55Al10Cu30Ni5、Zr60Al10Cu15Ni10Pd5和Zr41.2Ti13.8Cu12.5Ni10Be22.5非晶合金棒。In one embodiment of the present invention, using the bulk amorphous alloy continuous casting device shown in Figure 1, Zr 55 Al 10 Cu 30 Ni 5 , Zr 60 Al 10 Cu 15 Ni 10 Pd 5 and Zr 41.2 Ti 13.8 Cu 12.5 Continuous casting of Ni 10 Be 22.5 alloy. The melting and pouring process of the alloy is carried out under the protection of an inert high-purity argon gas with a relative pressure of 5×10 -6 Pa. The alloy is first melted and kept warm in a corundum crucible by means of high-frequency induction heating, and the bottom injection enters a porous disperser made of quartz glass with a pore diameter of 3 mm. The alloy liquid is dispersed to form a stream and then poured down into the brass-based condenser with an amorphous coating on the surface. Water is passed through the condenser for cooling, and at the same time, the condensed part is cooled with gallium-indium alloy liquid, so that the supercooled liquid of the bulk amorphous alloy completes the transformation to amorphous in the condenser. In order to make the liquid level in the condenser as uniform as possible, the disperser was always in a slow rotating state during the test. Using this method, Zr 55 Al 10 Cu 30 Ni 5 , Zr 60 Al 10 Cu 15 Ni 10 Pd 5 and Zr 41.2 Ti 13.8 Cu 12.5 Ni 10 Be 22.5 amorphous alloy rods with a diameter of 30 mm and a length of 500 mm were finally obtained.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325206C (en) * | 2003-05-09 | 2007-07-11 | 燕山大学 | Continuous manufacture process of massive non-crystal alloy casting |
| CN105014027A (en) * | 2015-08-21 | 2015-11-04 | 天津市中重科技工程有限公司 | Molten steel pre-cooling device for high speed continuous casting machine |
| CN108286068A (en) * | 2017-01-09 | 2018-07-17 | 赛峰集团 | The equipment for manufacturing part by implementing Bridgman method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325206C (en) * | 2003-05-09 | 2007-07-11 | 燕山大学 | Continuous manufacture process of massive non-crystal alloy casting |
| CN105014027A (en) * | 2015-08-21 | 2015-11-04 | 天津市中重科技工程有限公司 | Molten steel pre-cooling device for high speed continuous casting machine |
| CN105014027B (en) * | 2015-08-21 | 2017-03-22 | 天津市中重科技工程有限公司 | Molten steel pre-cooling device for high speed continuous casting machine |
| CN108286068A (en) * | 2017-01-09 | 2018-07-17 | 赛峰集团 | The equipment for manufacturing part by implementing Bridgman method |
| CN108286068B (en) * | 2017-01-09 | 2021-02-26 | 赛峰集团 | Device for producing a part by implementing the Bridgman method |
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