CN116144956A - Production process and smelting equipment of a lithium-boron alloy strip - Google Patents
Production process and smelting equipment of a lithium-boron alloy stripDownload PDFInfo
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- GCICAPWZNUIIDV-UHFFFAOYSA-Nlithium magnesiumChemical compound[Li].[Mg]GCICAPWZNUIIDV-UHFFFAOYSA-N0.000claimsabstractdescription17
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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
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details specially adapted for crucible or pot furnaces
- F27B14/10—Crucibles
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C24/00—Alloys based on an alkali or an alkaline earth metal
- 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
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details specially adapted for crucible or pot furnaces
- F27B14/14—Arrangements of heating devices
- 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
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details specially adapted for crucible or pot furnaces
- F27B14/20—Arrangement of controlling, monitoring, alarm or like devices
- 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
- F27D27/00—Stirring devices for molten material
- 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
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details specially adapted for crucible or pot furnaces
- F27B2014/085—Preheating of the charge
- F27B2014/0856—Preheating of the crucible
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Abstract
Description
Translated fromChinese技术领域technical field
本发明涉及锂硼合金带生产技术领域，具体涉及一种锂硼合金带的生产工艺及熔炼设备。The invention relates to the technical field of production of lithium-boron alloy strips, in particular to a production process and smelting equipment of lithium-boron alloy strips.
背景技术Background technique
锂硼合金是一种理想的锂系热电池负极材料，具有高比能量、高比功率、低极化、电化学电位与纯锂相近、600℃以上仍能保持稳定结构等突出优点，用作热电池负极材料，可以显著提高热电池的比容量和比功率，相同容量的热电池体积和质量减小了10％～30％，有效地提高了热电池的性能，为热电池的更新换代提供了有效的材料保证。Lithium-boron alloy is an ideal negative electrode material for lithium-based thermal batteries. It has outstanding advantages such as high specific energy, high specific power, low polarization, electrochemical potential similar to pure lithium, and stable structure above 600 ° C. It is used as Thermal battery anode materials can significantly increase the specific capacity and specific power of thermal batteries. The volume and mass of thermal batteries with the same capacity are reduced by 10% to 30%, which effectively improves the performance of thermal batteries and provides a new source of energy for the replacement of thermal batteries. An effective material guarantee is provided.
锂硼合金熔炼过程中，要经历复杂的物理化学状态变化，原料配比、热控制和搅拌条件都会影响最后形成的相结构，容易出现夹杂、孔洞、偏析等多种缺陷，后续挤压或辊轧的生产方法会加剧内部成分偏聚、难以控制各部分锂含量的均匀性，从而导致同一批次之间热稳定性和放电容量的差异。During the smelting process of lithium-boron alloy, it has to undergo complex physical and chemical state changes. The ratio of raw materials, thermal control and stirring conditions will all affect the final phase structure, which is prone to various defects such as inclusions, holes, and segregation. Subsequent extrusion or roll The production method of rolling will aggravate the segregation of internal components, and it is difficult to control the uniformity of lithium content in each part, resulting in differences in thermal stability and discharge capacity between the same batch.
中国专利CN102851561A公开了一种锂硼合金生产工艺及其设备，将锂和硼混合后在高纯氩气气氛下升温至400℃搅拌反应2h，再升温至450℃形成合金熔体并浇铸到模具中，继续升温到650℃反应1h至硬化，将合金坯锭冷却至室温后进行脱模和包装。但是将硼粉直接加入锂中熔解，容易出现硼粉熔解不完全的现象，引起剧烈放热、反应速率和反应温度不可控，导致锂硼合金锭的锂含量不均匀，轧制生产的锂硼合金带锂含量偏差大，严重影响锂硼合金带的品质和收率。Chinese patent CN102851561A discloses a lithium-boron alloy production process and its equipment. Lithium and boron are mixed and heated to 400°C for 2 hours under high-purity argon atmosphere, then heated to 450°C to form an alloy melt and cast into a mold In the process, continue to raise the temperature to 650 ° C for 1 hour to harden, and then cool the alloy ingot to room temperature for demoulding and packaging. However, when boron powder is directly added to lithium for melting, it is prone to incomplete melting of boron powder, causing violent exotherm, uncontrollable reaction rate and reaction temperature, resulting in uneven lithium content in lithium-boron alloy ingots, and lithium-boron produced by rolling. The lithium content of the alloy strip has a large deviation, which seriously affects the quality and yield of the lithium-boron alloy strip.
发明内容Contents of the invention
针对锂硼合金生产工艺中硼粉熔解不完全剧烈放热、反应速率和反应温度不可控的技术问题，本发明提供一种锂硼合金带的生产工艺和熔炼设备。Aiming at the technical problems of incomplete melting of boron powder and violent heat release, uncontrollable reaction rate and reaction temperature in the production process of lithium-boron alloy, the invention provides a production process and smelting equipment of lithium-boron alloy strip.
第一方面，本发明提供一种锂硼合金带的生产工艺，以质量百分比计，原料包括硼粉20％～50％、碳化锂粉末0.2％～1％、锂50％～80％、镁2％～6％；具体包括如下步骤：In the first aspect, the present invention provides a production process of a lithium-boron alloy strip. In terms of mass percentage, the raw materials include 20% to 50% of boron powder, 0.2% to 1% of lithium carbide powder, 50% to 80% of lithium,
(1)将硼粉和碳化锂粉末混合后，球磨至粒度为50～100μm的混合粉末，加入预热料仓内预热至200℃；(1) After mixing boron powder and lithium carbide powder, ball mill to a mixed powder with a particle size of 50-100 μm, add it to the preheating silo and preheat to 200°C;
(2)向熔炼坩埚中加入锂，加热至400～440℃，锂完全熔化后加入镁，搅拌30～60min，形成表面光亮无杂质的锂-镁熔体；(2) Add lithium to the melting crucible, heat to 400-440°C, add magnesium after the lithium is completely melted, and stir for 30-60 minutes to form a lithium-magnesium melt with a bright surface and no impurities;
(3)将锂-镁熔体升温至440～460℃，将预热好的混合粉末加入锂-镁熔体中，继续搅拌至熔体变黏：(3) Raise the temperature of the lithium-magnesium melt to 440-460°C, add the preheated mixed powder into the lithium-magnesium melt, and continue stirring until the melt becomes viscous:
(4)将熔体全部倒入提前预热到440～460℃的固化坩埚，以1℃/min的速率升温到500～560℃，熔炼至熔体完全固化，得到锂硼合金块，停止加热，随炉降温至250℃；(4) Pour all the melt into a solidification crucible preheated to 440-460°C in advance, heat up to 500-560°C at a rate of 1°C/min, and melt until the melt is completely solidified to obtain a lithium-boron alloy block, and stop heating , with the furnace cooling down to 250°C;
(5)将锂硼合金块从固化坩埚中取出，自然冷却至室温，密封包装；(5) Take out the lithium-boron alloy block from the solidified crucible, cool it down to room temperature naturally, and seal it;
(6)将锂硼合金块放入辊轧机进行多辊连轧，得到锂硼合金带，切边后收卷。(6) Put the lithium-boron alloy block into a rolling mill for multi-roll continuous rolling to obtain a lithium-boron alloy strip, which is wound after trimming.
熔炼过程中，将硼粉和碳化锂粉末制成混合粉末并提前预热，有助于硼粉的完全熔解，避免硼粉与锂-镁熔体反应剧烈放热，使反应速率和反应温度可控，进而得到锂含量均匀的熔体，固化生成Li7B6+Li相均匀的锂硼合金块。During the smelting process, boron powder and lithium carbide powder are made into mixed powder and preheated in advance, which is helpful for the complete melting of boron powder, avoiding the violent exothermic reaction between boron powder and lithium-magnesium melt, and making the reaction rate and reaction temperature possible. control, and then obtain a melt with uniform lithium content, and solidify to form a lithium-boron alloy block with uniform Li7 B6 +Li phase.
进一步的，步骤(3)中，加入混合粉末的质量为锂-镁熔体质量的30％～50％。Further, in step (3), the mass of the mixed powder added is 30%-50% of the mass of the lithium-magnesium melt.
进一步的，步骤(3)中，搅拌速度为200～600rpm，搅拌时间为60～240min。Further, in step (3), the stirring speed is 200-600 rpm, and the stirring time is 60-240 min.
进一步的，步骤(6)中，控制每一道次轧制量在10％～20％之间。Further, in step (6), the rolling amount of each pass is controlled between 10% and 20%.
进一步的，步骤(1)至步骤(5)在水氧含量＜0.1ppm、高纯氩气氛的手套箱内进行，步骤(6)的轧制过程在露点温度低于-45℃的干燥室内实施。Further, steps (1) to (5) are carried out in a glove box with a water oxygen content of <0.1ppm and a high-purity argon atmosphere, and the rolling process of step (6) is carried out in a drying room with a dew point temperature lower than -45°C .
第二方面，本发明提供一种用于上述生产工艺的锂硼合金熔炼设备，包括手套箱，手套箱内设置有两台独立控温炉体，两台独立控温炉体上分别设置有熔炼坩埚和固化坩埚，熔炼坩埚和固化坩埚内分别设置有搅拌装置，熔炼坩埚上部还设置有预热料仓。In the second aspect, the present invention provides a lithium-boron alloy smelting equipment used in the above-mentioned production process, including a glove box, two independent temperature-controlled furnace bodies are arranged in the glove box, and two independent temperature-controlled furnace bodies are respectively equipped with smelting The crucible, the solidifying crucible, the melting crucible and the solidifying crucible are respectively provided with stirring devices, and the upper part of the melting crucible is also provided with a preheating bin.
进一步的，预热料仓设置为不锈钢材质，加热方式为电加热，可加热温度为100～300℃。Further, the preheating bin is made of stainless steel, the heating method is electric heating, and the heating temperature is 100-300°C.
进一步的，独立控温炉体内设置有温控系统，温控系统的测温元件为热电偶。Further, a temperature control system is installed in the body of the independent temperature control furnace, and the temperature measuring element of the temperature control system is a thermocouple.
进一步的，独立控温炉体的加热方式为电磁感应加热或电阻加热。Further, the heating method of the independently temperature-controlled furnace body is electromagnetic induction heating or resistance heating.
进一步的，熔炼坩埚和固化坩埚为铁素体不锈钢材质。Further, the melting crucible and the solidification crucible are made of ferritic stainless steel.
本发明的有益效果在于：The beneficial effects of the present invention are:
本发明提供的锂硼合金带的生产工艺通过加入碳化锂粉末，使硼粉与锂镁熔体不产生剧烈放热，反应速率与反应温度可控，得到锂含量均匀的锂硼合金块，熔炼完成后无需后续复杂的加工处理即可直接进行下一步辊轧工序。制得的锂硼合金带均匀性有所提高、同一批次不同部位锂含量偏差控制在1％以内，表面质量好、无夹杂和变色，收率高，操作简便，能实现连续生产，无需额外增加大型挤压或墩压设备，降低了生产成本，提高了劳动效率。The production process of the lithium-boron alloy strip provided by the present invention adds lithium carbide powder so that the boron powder and the lithium-magnesium melt do not generate violent exothermic heat, the reaction rate and reaction temperature are controllable, and a lithium-boron alloy block with uniform lithium content is obtained, which is smelted After completion, the next rolling process can be directly carried out without subsequent complicated processing. The uniformity of the prepared lithium-boron alloy strips is improved, the deviation of lithium content in different parts of the same batch is controlled within 1%, the surface quality is good, there is no inclusion and discoloration, the yield is high, the operation is simple, and continuous production can be realized without additional Adding large-scale extrusion or pier pressing equipment reduces production costs and improves labor efficiency.
附图说明Description of drawings
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，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，对于本领域普通技术人员而言，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。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, for those of ordinary skill in the art, In other words, other drawings can also be obtained from these drawings on the premise of not paying creative work.
图1是本申请实施例中锂硼合金熔炼设备的结构示意图。Fig. 1 is a schematic structural diagram of a lithium-boron alloy smelting equipment in an embodiment of the present application.
其中，1、手套箱；2、炉体；3、热电偶；4、熔炼坩埚；5、固化坩埚；6、搅拌装置；7、预热料仓。Among them, 1. Glove box; 2. Furnace body; 3. Thermocouple; 4. Melting crucible; 5. Solidifying crucible; 6. Stirring device; 7. Preheating bin.
具体实施方式Detailed ways
为了使本技术领域的人员更好地理解本发明中的技术方案，下面将结合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做出创造性劳动前提下所获得的所有其他实施例，都应当属于本发明保护的范围。In order to enable those skilled in the art to better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings. Obviously, the described embodiments are only a part of the present invention Examples, not all examples. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts shall fall within the protection scope of the present invention.
实施例1Example 1
一种锂硼合金熔炼设备，包括手套箱1，手套箱1内设置有两台独立控温的炉体2，炉体2加热方式为变频电阻式加热丝加热，炉体2内部采用陶瓷作为保温材质。炉体2内部的温控系统通过热电偶3探测炉体中心温度，根据预设参数自动调节加热功率，实现温度控制。两台独立控温的炉体2上分别设置有熔炼坩埚4和固化坩埚5，熔炼坩埚4和固化坩埚5均为铁素体不锈钢材质。熔炼坩埚4和固化坩埚5内分别设置有搅拌装置6，熔炼坩埚4上部还设置有预热料仓7。A lithium-boron alloy smelting equipment, including a
使用上述锂硼合金熔炼设备和辊轧机生产锂硼合金带，生产工艺包括如下步骤：Using the above-mentioned lithium-boron alloy smelting equipment and rolling mill to produce lithium-boron alloy strips, the production process includes the following steps:
(1)将提前干燥称重的43g硼粉和1g碳化锂粉末混合均匀，球磨粒度为50～100μm的混合粉末，加入预热料仓预热至200℃；(1) Mix 43g of boron powder and 1g of lithium carbide powder that have been dried and weighed in advance and mix evenly, ball mill the mixed powder with a particle size of 50-100μm, add it to the preheating silo and preheat to 200°C;
(2)在水氧含量＜0.1ppm、高纯氩气氛的手套箱内，称取58g锂，放入熔炼坩埚内，440℃保温，锂完全熔化后加入4g镁，并安装搅拌装置，搅拌30min得到表面光亮无杂质的锂-镁熔体；(2) In a glove box with a water oxygen content of <0.1ppm and a high-purity argon atmosphere, weigh 58g of lithium, put it into a melting crucible, keep it warm at 440°C, add 4g of magnesium after the lithium is completely melted, install a stirring device, and stir for 30 minutes Obtain a lithium-magnesium melt with a bright surface and no impurities;
(3)将预热好的混合粉末投入锂-镁熔体中，继续搅拌，搅拌速度为200rpm，当熔体出现变黏情况时提出搅拌桨，搅拌时间为60min；(3) Put the preheated mixed powder into the lithium-magnesium melt and continue to stir at a stirring speed of 200rpm. When the melt becomes viscous, raise the stirring paddle for 60 minutes;
(4)固化坩埚提前预热到440℃，将熔体全部倒入固化坩埚，然后以1℃/min的速率将固化坩埚升温到560℃，保温直到熔体完全固化，得到锂硼合金块，停止加热，随炉降温至250℃；(4) Preheat the solidified crucible to 440°C in advance, pour all the melt into the solidified crucible, then raise the temperature of the solidified crucible to 560°C at a rate of 1°C/min, keep warm until the melt is completely solidified, and obtain a lithium-boron alloy block, Stop heating and cool down to 250°C with the furnace;
(5)将锂硼合金块磕出，在手套箱内自然冷却到常温，真空密封包装，转移到露点-45℃的干燥间内；(5) Knock out the lithium-boron alloy block, cool it naturally in a glove box to normal temperature, pack it in a vacuum seal, and transfer it to a drying room with a dew point of -45°C;
(6)根据产品要求，将锂硼合金块放入辊轧机进行多辊连轧，控制每一道次轧制量在10％，经过15道次轧得到厚度为0.6mm±0.03mm锂硼合金带，切边并收卷。(6) According to the product requirements, put the lithium-boron alloy block into the rolling mill for multi-roll continuous rolling, control the rolling volume of each pass at 10%, and obtain a lithium-boron alloy strip with a thickness of 0.6mm±0.03mm after 15 passes , trimmed and rolled.
将锂硼合金带分切成所需规格的锂硼合金片材产品，取样检测产品的化学成分、尺寸、物相组成、密度、外观质量、热稳定性、放电性能，均合格通过；其中，锂含量测定结果在54.3％～55.1％范围内。Cut the lithium-boron alloy strip into lithium-boron alloy sheet products of required specifications, and take samples to test the chemical composition, size, phase composition, density, appearance quality, thermal stability, and discharge performance of the product, all of which are qualified; among them, The lithium content measurement results are in the range of 54.3% to 55.1%.
实施例2Example 2
使用实施例1中的锂硼合金熔炼设备和辊轧机生产锂硼合金带，生产工艺包括如下步骤：Use the lithium-boron alloy smelting equipment and rolling mill in
1)将提前干燥称重的32g硼粉和0.5g碳化锂粉末混合均匀，球磨粒度为50～100μm的混合粉末，加入预热料仓预热至200℃；1) Mix 32g of boron powder and 0.5g of lithium carbide powder that have been dried and weighed in advance, evenly, ball mill the mixed powder with a particle size of 50-100μm, and add it to the preheating silo to preheat to 200°C;
(2)在水氧含量＜0.1ppm、高纯氩气氛的手套箱内，称取75g锂，放入熔炼坩埚内，420℃保温，锂完全熔化后加入6g镁，并安装搅拌装置，搅拌60min得到表面光亮无杂质的锂-镁熔体；(2) In a glove box with a water oxygen content of <0.1ppm and a high-purity argon atmosphere, weigh 75g of lithium, put it into a melting crucible, keep it warm at 420°C, add 6g of magnesium after the lithium is completely melted, install a stirring device, and stir for 60 minutes Obtain a lithium-magnesium melt with a bright surface and no impurities;
(3)将预热好的混合粉末投入锂-镁熔体中，继续搅拌，搅拌速度为400rpm，当熔体出现变黏情况时提出搅拌桨，搅拌时间为80min；(3) Put the preheated mixed powder into the lithium-magnesium melt and continue to stir at a stirring speed of 400rpm. When the melt becomes viscous, raise the stirring paddle for 80 minutes;
(4)固化坩埚提前预热到420℃，将熔体全部倒入固化坩埚，然后以1℃/min的速率将固化坩埚升温到540℃，保温直到熔体完全固化，得到锂硼合金块，停止加热，随炉降温至250℃；(4) Preheat the solidified crucible to 420°C in advance, pour all the melt into the solidified crucible, then raise the temperature of the solidified crucible to 540°C at a rate of 1°C/min, keep warm until the melt is completely solidified, and obtain a lithium-boron alloy block, Stop heating and cool down to 250°C with the furnace;
(5)将锂硼合金块磕出，在手套箱内自然冷却到常温，真空密封包装，转移到露点-45℃的干燥间内；(5) Knock out the lithium-boron alloy block, cool it naturally in a glove box to normal temperature, pack it in a vacuum seal, and transfer it to a drying room with a dew point of -45°C;
(6)根据产品要求，将锂硼合金块放入辊轧机进行多辊连轧，控制每一道次轧制量在15％，经过12道次轧得到厚度为0.6mm±0.03mm锂硼合金带，切边并收卷。(6) According to the product requirements, put the lithium-boron alloy block into the rolling mill for multi-roll continuous rolling, control the rolling volume of each pass at 15%, and obtain a lithium-boron alloy strip with a thickness of 0.6mm±0.03mm after 12 passes , trimmed and rolled.
将锂硼合金带冲切出所需规格的锂硼合金圆片产品，取样检测产品的化学成分、尺寸、物相组成、密度、外观质量、热稳定性、放电性能，均合格通过；其中，锂含量测定结果均在65.7％～66.3％范围内。Die-cut lithium-boron alloy strips into required specifications of lithium-boron alloy disc products, and take samples to test the chemical composition, size, phase composition, density, appearance quality, thermal stability, and discharge performance of the products, all of which are qualified; among them, The measured results of lithium content were all in the range of 65.7%-66.3%.
实施例3Example 3
使用实施例1中的锂硼合金熔炼设备和辊轧机生产锂硼合金带，生产工艺包括如下步骤：Use the lithium-boron alloy smelting equipment and rolling mill in
1)将提前干燥称重的38g硼粉和0.7g碳化锂粉末混合均匀，球磨粒度为50～100μm的混合粉末，加入预热料仓预热至200℃；1) Mix 38g of boron powder and 0.7g of lithium carbide powder that have been dried and weighed in advance, evenly, ball mill the mixed powder with a particle size of 50-100μm, and add it to the preheating silo to preheat to 200°C;
(2)在水氧含量＜0.1ppm、高纯氩气氛的手套箱内，称取72g锂，放入熔炼坩埚内，400℃保温，锂完全熔化后加入4g镁，并安装搅拌装置，搅拌60min得到表面光亮无杂质的锂-镁熔体；(2) In a glove box with a water oxygen content of <0.1ppm and a high-purity argon atmosphere, weigh 72g of lithium, put it into a melting crucible, keep it warm at 400°C, add 4g of magnesium after the lithium is completely melted, install a stirring device, and stir for 60 minutes Obtain a lithium-magnesium melt with a bright surface and no impurities;
(3)将预热好的混合粉末投入锂-镁熔体中，继续搅拌，搅拌速度为400rpm，当熔体出现变黏情况时提出搅拌桨，搅拌时间为100min；(3) Put the preheated mixed powder into the lithium-magnesium melt, continue to stir, the stirring speed is 400rpm, when the melt becomes viscous, the stirring paddle is raised, and the stirring time is 100min;
(4)固化坩埚提前预热到400℃，将熔体全部倒入固化坩埚，然后以1℃/min的速率将固化坩埚升温到520℃，保温直到熔体完全固化，得到锂硼合金块，停止加热，随炉降温至250℃；(4) Preheat the solidified crucible to 400°C in advance, pour all the melt into the solidified crucible, then raise the temperature of the solidified crucible to 520°C at a rate of 1°C/min, keep warm until the melt is completely solidified, and obtain a lithium-boron alloy block, Stop heating and cool down to 250°C with the furnace;
(5)将锂硼合金块磕出，在手套箱内自然冷却到常温，真空密封包装，转移到露点-45℃的干燥间内；(5) Knock out the lithium-boron alloy block, cool it naturally in a glove box to normal temperature, pack it in a vacuum seal, and transfer it to a drying room with a dew point of -45°C;
(6)根据产品要求，将锂硼合金块放入辊轧机进行多辊连轧，控制每一道次轧制量在20％，经过10道次轧得到厚度为0.6mm±0.03mm锂硼合金带，切边并收卷。(6) According to the product requirements, put the lithium-boron alloy block into the rolling mill for multi-roll continuous rolling, control the rolling volume of each pass at 20%, and obtain a lithium-boron alloy strip with a thickness of 0.6mm±0.03mm after 10 passes , trimmed and rolled.
将锂硼合金带冲切出所需规格的锂硼合金圆片产品，取样检测产品的化学成分、尺寸、物相组成、密度、外观质量、热稳定性、放电性能，均合格通过；其中，锂含量测定结果均在71.6％～72.3％范围内。Die-cut lithium-boron alloy strips into required specifications of lithium-boron alloy disc products, and take samples to test the chemical composition, size, phase composition, density, appearance quality, thermal stability, and discharge performance of the products, all of which are qualified; among them, The lithium content determination results were all in the range of 71.6%-72.3%.
对比例comparative example
使用实施例1中的锂硼合金熔炼设备和辊轧机生产锂硼合金带，生产工艺包括如下步骤：Use the lithium-boron alloy smelting equipment and rolling mill in
(1)将68g锂和32g硼粉混合放入熔炼坩埚400℃保温，并搅拌反应60min，升温至450℃，得到熔体；(1) Mix 68g of lithium and 32g of boron powder into a melting crucible to keep warm at 400°C, and stir for 60 minutes, then heat up to 450°C to obtain a melt;
(2)固化坩埚提前预热到450℃，将熔体全部倒入固化坩埚，升温至650℃，保温反应60min至固化，得到锂硼合金块，停止加热，随炉降温至250℃；(2) Preheat the solidification crucible to 450°C in advance, pour all the melt into the solidification crucible, raise the temperature to 650°C, keep it warm for 60 minutes until solidification, and obtain a lithium-boron alloy block, stop heating, and cool down to 250°C with the furnace;
(3)将锂硼合金块磕出，在手套箱内自然冷却到常温，真空密封包装，转移到露点-45℃的干燥间内；(3) Knock out the lithium-boron alloy block, cool it naturally in a glove box to room temperature, pack it in a vacuum seal, and transfer it to a drying room with a dew point of -45°C;
(6)根据产品要求，将锂硼合金块放入辊轧机进行多辊连轧，控制每一道次轧制量在20％，经过10道次轧得到厚度为0.6mm±0.03mm锂硼合金带。(6) According to the product requirements, put the lithium-boron alloy block into the rolling mill for multi-roll continuous rolling, control the rolling volume of each pass at 20%, and obtain a lithium-boron alloy strip with a thickness of 0.6mm±0.03mm after 10 passes .
该锂硼合金带边缘开裂严重，表面不平整，出现变色和夹杂，需要切除的边缘较宽，将锂硼合金带分切成片材，取样检测片材的化学成分，锂含量的范围为63.4％～79.2％。The edge of the lithium-boron alloy strip is severely cracked, the surface is uneven, discoloration and inclusions appear, and the edge to be cut is wide. The lithium-boron alloy strip is cut into sheets, and the chemical composition of the sheet is tested by sampling. The lithium content ranges from 63.4 %~79.2%.
尽管通过结合附图并优选实施例的方式对本发明进行了详细描述，但本发明并不限于此。在不脱离本发明的精神和实质的前提下，本领域普通技术人员可以对本发明的实施例进行各种等效的修改或替换，而这些修改或替换都应在本发明的涵盖范围内/任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。Although the present invention has been described in detail with reference to the accompanying drawings and preferred embodiments, the present invention is not limited thereto. Without departing from the spirit and essence of the present invention, those skilled in the art can make various equivalent modifications or replacements to the embodiments of the present invention, and these modifications or replacements should be within the scope of the present invention/any Those skilled in the art can easily think of changes or substitutions within the technical scope disclosed in the present invention, and all should be covered within the protection scope of the present invention.
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