CN101306818A - A kind of preparation method and device of magnesium silicide - Google Patents
A kind of preparation method and device of magnesium silicide Download PDFInfo
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- 229910021338 magnesium silicide Inorganic materials 0.000 title claims abstract description 39
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000013021 overheating Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 4
- 239000000428 dust Substances 0.000 claims description 16
- 230000007704 transition Effects 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 230000005484 gravity Effects 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 abstract description 19
- 229910052749 magnesium Inorganic materials 0.000 abstract description 17
- 230000008569 process Effects 0.000 abstract description 7
- 238000003756 stirring Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000010419 fine particle Substances 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 7
- 229910019018 Mg 2 Si Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910017639 MgSi Inorganic materials 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 229910019752 Mg2Si Inorganic materials 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
本发明公开了一种硅化镁的制备方法与装置。该制备方法以当量配比的镁粉与硅粉为原料，在真空中或气体保护下，通过顶部连续给进原料，立式圆筒形反应器内连续搅动，使反应均匀充分，避免反应过热和镁蒸汽外逸。所述的装置主要采用立式圆筒形反应器代替水平式反应器，用顶部减速机带动螺旋片搅拌器搅动原料；该反应器外壁上部采用加热器加热，下部采用冷水套冷却，底部采用刮刀和孔板粉碎反应生成的硅化镁，反应器上侧与加料装置相连，下部与收料装置相连。反应完毕后，连续产物经过刮刀与孔板的粉碎作用，得到粒度细小、组成均匀、当量匹配的硅化镁粉末。本发明既可实现硅化镁的连续生产，还可提高原料转化率，减少过程中镁的消耗，同时降低能耗。
The invention discloses a preparation method and device of magnesium silicide. The preparation method uses magnesium powder and silicon powder in an equivalent ratio as raw materials. In vacuum or under the protection of gas, the raw materials are continuously fed through the top, and the vertical cylindrical reactor is continuously stirred to make the reaction uniform and sufficient to avoid overheating of the reaction. and magnesium vapor escape. The device mainly adopts a vertical cylindrical reactor instead of a horizontal reactor, and uses a top speed reducer to drive a spiral blade agitator to stir the raw materials; the upper part of the outer wall of the reactor is heated by a heater, the lower part is cooled by a cold water jacket, and the bottom part is cooled by a scraper. The magnesium silicide formed by the reaction with orifice plate pulverization, the upper side of the reactor is connected with the feeding device, and the lower part is connected with the receiving device. After the reaction is completed, the continuous product is pulverized by a scraper and an orifice plate to obtain a magnesium silicide powder with fine particle size, uniform composition and matching equivalent weight. The invention can not only realize the continuous production of magnesium silicide, but also improve the conversion rate of raw materials, reduce the consumption of magnesium in the process, and reduce energy consumption at the same time.
Description
技术领域 technical field
本发明涉及一种硅化镁的制备方法与装置。The invention relates to a preparation method and device of magnesium silicide.
背景技术 Background technique
硅化镁是一种重要的工业原料，广泛应用于制备硅烷气体、多晶硅、非晶硅薄膜、陶瓷材料及含硅纳米粉末等，对半导体微电子制造业、太阳电池制造业、材料镀层加工业和先进陶瓷有着越来越重要的作用。开发高效、高质量和低能耗的工业合成技术是硅化镁工艺的发展方向。Magnesium silicide is an important industrial raw material, which is widely used in the preparation of silane gas, polysilicon, amorphous silicon film, ceramic materials and silicon-containing nano-powder, etc. Advanced ceramics are playing an increasingly important role. The development of high-efficiency, high-quality and low-energy industrial synthesis technology is the development direction of magnesium silicide technology.
传统硅化镁的合成方法是将硅粉与镁粉按比例混合，在氢气氛或真空下加热到500～650℃左右，使其发生反应，生成硅化镁粉末，反应式为：The traditional synthesis method of magnesium silicide is to mix silicon powder and magnesium powder in proportion, and heat them to about 500-650°C in hydrogen atmosphere or vacuum to make them react to produce magnesium silicide powder. The reaction formula is:
2Mg+Si→Mg2Si+77.4kJ2Mg+Si→Mg 2 Si+77.4kJ
由于合成硅化镁的反应是一个是放热反应，在用大型固定床装置中合成硅化镁时，就会碰到一个严重的问题，即物料反应放热引起高温，物料会自动升温到650～800℃。这时生成的产品呈粘结块状，组成偏离Mg2Si。从而导致用这种组成偏离原料制备硅烷的收率偏低。同时，大型固定床装置一般是间隙式的生产方式，即它需要装料、加热、保温、冷却和取料等过程，生产效率较低，能耗较大，产物结块严重，处理困难，劳保条件差。Because the reaction of synthesizing magnesium silicide is an exothermic reaction, when synthesizing magnesium silicide in a large fixed bed device, a serious problem will be encountered, that is, the exothermic reaction of the material will cause a high temperature, and the material will automatically heat up to 650-800 ℃. At this time, the resulting product is in the form of a cohesive block, and its composition deviates from Mg 2 Si. As a result, the yield of silane prepared from raw materials deviated from this composition is low. At the same time, large-scale fixed bed devices are generally intermittent production methods, that is, they require processes such as charging, heating, heat preservation, cooling, and reclaiming, with low production efficiency, high energy consumption, serious product agglomeration, difficult handling, and labor insurance. poor condition.
相对间隙生产方式，硅化镁连续合成法更具有优势。德国专利1143190提出了连续合成硅化镁的方法。一个方案是卧式螺旋推进反应器，在水平的反应管内混合料由旋转的螺旋推进器向前输送，一边搅拌一边通过加热区。另一个方案是延转管式，反应管稍倾斜，物料靠反应管道转动，一面拌和一面通过加热区。在连续炉中硅镁混合料通过热区，传热和传质较均匀，因反应热引起过热的问题得到缓解，从而使生产硅烷的收率提高。但是，由于以上两个方案均基本使用了水平的反应管，反应管上部没有物料填充，从而引起镁蒸气外泄，造成镁的损耗。在此类卧式反应器中的物料配比，镁必需过量3～10％，不但造成镁的浪费，而且蒸发的镁在反应管内部件表面上结晶会妨碍机构的正常运转。因此，装置的产量和产品质量受到限制。Compared with the intermittent production method, the continuous synthesis method of magnesium silicide has more advantages. German patent 1143190 proposes a method for continuously synthesizing magnesium silicide. One solution is a horizontal screw propulsion reactor, in which the mixed material is conveyed forward by a rotating screw propeller in a horizontal reaction tube, and passes through the heating zone while stirring. Another solution is the extension tube type, the reaction tube is slightly inclined, the material is rotated by the reaction tube, and the material passes through the heating zone while stirring. In the continuous furnace, the silicon-magnesium mixture passes through the hot zone, the heat transfer and mass transfer are relatively uniform, and the problem of overheating caused by the reaction heat is alleviated, thereby increasing the yield of silane production. However, since the above two schemes basically use horizontal reaction tubes, there is no material filling in the upper part of the reaction tubes, which will cause the leakage of magnesium vapor and cause the loss of magnesium. In the proportioning of materials in this type of horizontal reactor, the magnesium must be in excess of 3-10%, which not only causes the waste of magnesium, but also the crystallization of evaporated magnesium on the surface of the inner part of the reaction tube will hinder the normal operation of the mechanism. Therefore, the yield and product quality of the device are limited.
发明内容 Contents of the invention
为了克服背景技术存在的问题，本发明的目的在于提供一种硅化镁的制备方法与装置。In order to overcome the problems in the background technology, the object of the present invention is to provide a method and device for preparing magnesium silicide.
申请人根据多年研究发现，硅化镁合成时，首先是镁的升华，然后气态的镁与硅粉固体作用，镁原子由硅粉表面向内部扩散，最后形成硅化镁。由于放热反应使物料温度骤然升高，高温下硅化镁不稳定以及高温下镁容易蒸发，使合成过程复杂化。合成时物料的实际温度对硅化镁品质有十分重要影响。实际合成反应有如下可能的可逆过程：According to years of research, the applicant found that when magnesium silicide is synthesized, magnesium is first sublimated, then gaseous magnesium interacts with silicon powder solids, magnesium atoms diffuse from the surface of silicon powder to the inside, and finally magnesium silicide is formed. Due to the exothermic reaction, the temperature of the material rises suddenly, the magnesium silicide is unstable at high temperature, and the magnesium is easy to evaporate at high temperature, which complicates the synthesis process. The actual temperature of the material during synthesis has a very important influence on the quality of magnesium silicide. The actual synthesis reaction has the following possible reversible process:
2Mg+Si→Mg2Si (2)2Mg+Si→Mg 2 Si (2)
Mg2Si→MgSi+Mg (3) Mg2Si →MgSi+Mg (3)
2MgSi→Mg2Si+Si (4)2MgSi→ Mg2Si +Si (4)
MgSi→Mg+Si (5)MgSi→Mg+Si (5)
500℃开始反应以明显的速度开始按(2)式进行，产物是Mg2Si。高于700℃时因镁蒸发，(3)式的分解过程开始占优势。温度愈高，加热时间愈长，分解得愈多。生成的中间化合物MgSi不稳定，在700℃以下时，如(4)，转化成Mg2Si，同时析出硅。高于1100℃时按(5)式进一步分解为硅和镁。所以高温下合成的硅化镁中，Mg2Si的含量少，析出的游离镁、游离硅较多。而目前硅化镁的制备装置还不能解决合成过程中过热问题与镁蒸汽外逸的问题。The reaction starts at 500°C and proceeds according to formula (2) at an obvious speed, and the product is Mg 2 Si. When the temperature is higher than 700°C, the decomposition process of formula (3) begins to dominate due to the evaporation of magnesium. The higher the temperature, the longer the heating time and the more decomposition. The generated intermediate compound MgSi is unstable, and when the temperature is below 700°C, as in (4), it will be transformed into Mg 2 Si, and silicon will be precipitated at the same time. When it is higher than 1100°C, it will be further decomposed into silicon and magnesium according to formula (5). Therefore, in the magnesium silicide synthesized at high temperature, the content of Mg 2 Si is small, and the precipitated free magnesium and free silicon are more. However, the current preparation device for magnesium silicide cannot solve the problem of overheating and the escape of magnesium vapor during the synthesis process.
本发明解决其技术问题采用的技术方案是：The technical scheme that the present invention solves its technical problem adopts is:
一、一种硅化镁的制备方法：One, a kind of preparation method of magnesium silicide:
1)将硅粉与镁粉按照质量比1∶1.5～2.3的比例混合，加入过渡料斗后，抽真空或充入保护气体，再将其放入上料斗；1) Mix silicon powder and magnesium powder according to the mass ratio of 1:1.5-2.3, add them into the transition hopper, vacuumize or fill them with protective gas, and then put them into the upper hopper;
2)由螺旋推进器给立式圆筒形反应器连续加料；2) The vertical cylindrical reactor is continuously fed by the screw propeller;
3)原料通过立式圆筒形反应器的螺旋片搅拌器搅动，让其经过反应器上部的热场，该热场控制的温度范围为500～650℃，此时硅粉与镁粉发生反应生成硅化镁，同时放出热量；3) The raw materials are stirred by the helical blade agitator of the vertical cylindrical reactor, and let them pass through the thermal field on the upper part of the reactor. The temperature range controlled by the thermal field is 500-650°C, and the silicon powder and the magnesium powder react at this time Magnesium silicide is generated and heat is released at the same time;
4)刚生成的硅化镁在重力作用下，进入反应器下部的冷水套冷却，防止反应过热；4) The magnesium silicide just generated enters the cold water jacket in the lower part of the reactor to cool under the action of gravity to prevent overheating of the reaction;
5)最后通过刮刀与孔板，将粉体磨碎后，送入收料斗，并通过出料斗取出最终产物。5) Finally, through the scraper and the orifice plate, the powder is ground, sent into the receiving hopper, and the final product is taken out through the discharging hopper.
所述的保护气体为氢气或氩气。The protective gas is hydrogen or argon.
二、一种硅化镁的制备装置：Two, a preparation device of magnesium silicide:
本发明包括立式圆筒形反应器、螺旋片搅拌器、两个减速机、加热器、冷水套、刮刀、孔板、收料斗、螺旋推进器、出料斗、上料斗、过渡料斗、三个粉尘过滤器、二个机械真空泵、九个阀门、视镜和氮气瓶；过渡料斗的出口经第一阀门接上料斗，上料斗的出口接螺旋推进器；立式圆筒形反应器的外圆柱面上端包覆加热器，下端包覆冷水套，内部配有螺旋片搅拌器、刮刀和孔板，顶部配有视镜；螺旋片搅拌器和螺旋推进器分别采用减速机驱动；立式圆筒形反应器通过第二粉尘过滤器与第七阀门，与第一机械真空泵相连；立式圆筒形反应器底部通过刮刀和孔板与收料斗相连，收料斗与出料斗通过第二阀门相连；出料斗通过第三粉尘过滤器和第八阀门与氮气瓶相连；过渡料斗通过第一粉尘过滤器和第六阀门与第二机械真空泵相连，并经第四阀门接第三粉尘过滤器，收料斗、上料斗和过渡料斗上，分别接有第三阀门、第五阀门和第五阀门。The invention includes a vertical cylindrical reactor, a spiral blade agitator, two reducers, a heater, a cold water jacket, a scraper, an orifice plate, a receiving hopper, a screw propeller, a hopper, an upper hopper, a transition hopper, three Dust filter, two mechanical vacuum pumps, nine valves, sight glass and nitrogen cylinder; the outlet of the transition hopper is connected to the hopper through the first valve, and the outlet of the upper hopper is connected to the screw propeller; the outer cylinder of the vertical cylindrical reactor The upper end of the surface is covered with a heater, and the lower end is covered with a cold water jacket. The interior is equipped with a spiral blade agitator, a scraper and an orifice plate, and the top is equipped with a sight glass; the spiral blade agitator and the screw propeller are respectively driven by a reducer; the vertical cylinder The cylindrical reactor is connected with the seventh valve through the second dust filter, and connected with the first mechanical vacuum pump; the bottom of the vertical cylindrical reactor is connected with the receiving hopper through the scraper and the orifice plate, and the receiving hopper is connected with the discharging hopper through the second valve; The discharge hopper is connected to the nitrogen cylinder through the third dust filter and the eighth valve; the transition hopper is connected to the second mechanical vacuum pump through the first dust filter and the sixth valve, and connected to the third dust filter through the fourth valve, and the receiving hopper , the upper hopper and the transition hopper are respectively connected with a third valve, a fifth valve and a fifth valve.
本发明与背景技术相比，具有的有益效果如下：Compared with the background technology, the present invention has the following beneficial effects:
(1)本发明可现实加料、反应和收料等步骤的连续化生产，无需硅化镁间隙式生产法的装料、加热、保温、冷却和取料等过程，生产效率提高，能耗降低。(1) The present invention can realize the continuous production of steps such as feeding, reacting and receiving materials, and does not need the processes of charging, heating, heat preservation, cooling and retrieving materials of the magnesium silicide batch production method, the production efficiency is improved, and the energy consumption is reduced.
(2)跟水平反应器或近水平反应器相比，本发明采用的立式圆筒形反应器，可有效防止镁蒸汽的外逸，有效节约镁的用量，同时避免蒸发的镁在反应管内部件表面上结晶会妨碍机构的正常运转。(2) compared with horizontal reactor or nearly horizontal reactor, the vertical cylindrical reactor that the present invention adopts can effectively prevent the escaping of magnesium vapor, effectively save the consumption of magnesium, and avoid the magnesium that evaporates in reaction tube simultaneously Crystallization on the surface of the component can prevent the proper functioning of the mechanism.
(3)本发明采用的立式圆筒形反应器，设计了上部的加热区与下部的冷却区，使反应产生的热量随着硅化镁被带入下部的冷却区冷却，有效防止因反应热产生的过热问题，避免产物结块和副反应的发生，从而保证质量。(3) The vertical cylindrical reactor adopted in the present invention is designed with an upper heating zone and a lower cooling zone, so that the heat generated by the reaction is brought into the lower cooling zone along with the magnesium silicide for cooling, effectively preventing the reaction heat from The resulting overheating problem avoids product agglomeration and side reactions, thereby ensuring quality.
附图说明 Description of drawings
图1是本发明的结构示意图。Fig. 1 is a structural schematic diagram of the present invention.
图2是实施例1所得硅化镁产物的XRD图谱。Fig. 2 is the XRD spectrum of the magnesium silicide product obtained in Example 1.
图中：1.立式圆筒形反应器，2.螺旋片搅拌器，3a、3b.减速机，4.加热器，5.冷水套，6.刮刀，7.孔板，8.收料斗，9.螺旋推进器，10.出料斗，11.上料斗，12.过渡料斗，13a～13c.粉尘过滤器，14a、14b.机械真空泵，15a～15i.阀门，16.视镜，17.氮气瓶In the figure: 1. Vertical cylindrical reactor, 2. Spiral blade agitator, 3a, 3b. Reducer, 4. Heater, 5. Cooling water jacket, 6. Scraper, 7. Orifice plate, 8. Hopper , 9. Screw propeller, 10. Out hopper, 11. Upper hopper, 12. Transition hopper, 13a～13c. Dust filter, 14a, 14b. Mechanical vacuum pump, 15a～15i. Valve, 16. Sight glass, 17. nitrogen bottle
具体实施方式 Detailed ways
如图1所示，本发明包括立式圆筒形反应器1，螺旋片搅拌器2，两个减速机3a、3b，加热器4，冷水套5，刮刀6，孔板7、收料斗8，螺旋推进器9，出料斗10，上料斗11，过渡料斗12，三个粉尘过滤器13a～13c，二个机械真空泵14a、14b，九个阀门15a～15i，视镜16和氮气瓶17；过渡料斗12的出口经第一阀门15a接上料斗11，上料斗11的出口接螺旋推进器9；立式圆筒形反应器1的外圆柱面上端包覆加热器4，下端包覆冷水套5，内部配有螺旋片搅拌器2、刮刀6和孔板7，顶部配有视镜16；螺旋片搅拌器2和螺旋推进器9分别采用减速机3a、3b驱动；立式圆筒形反应器1通过第二粉尘过滤器13b与第七阀门15g，与第一机械真空泵14a相连；立式圆筒形反应器1底部通过刮刀6和孔板7与收料斗8相连，收料斗8与出料斗10通过第二阀门15b相连；出料斗10通过第三粉尘过滤器13c和第八阀门15h与氮气瓶17相连；过渡料斗12通过第一粉尘过滤器13a和第六阀门15f与第二机械真空泵14b相连，并经第四阀门15d接第三粉尘过滤器13c，收料斗8、上料斗11和过渡料斗12上，分别接有第三阀门15c、第五阀门15e和第五阀门15i。As shown in Figure 1, the present invention comprises a vertical
本发明具体实施步骤如下：The specific implementation steps of the present invention are as follows:
(1)将硅粉与镁粉按照规定比例混合，搅拌；(1) Mix silicon powder and magnesium powder according to the specified ratio, and stir;
(2)对整个系统经多次氮气吹扫和抽真空，最终保持真空状态，如果需要氢气或氩气保护，抽真空后，充入氢气或氩气；(2) The whole system is purged and vacuumed several times with nitrogen gas, and the vacuum state is finally maintained. If hydrogen or argon protection is required, after vacuuming, fill it with hydrogen or argon;
(3)开始对加热器4开始加热，并对冷水套5通冷却水，开启立式圆筒形反应器1顶部的减速机3a，使立式圆筒形反应器1的螺旋片搅拌器2的螺旋片向上推动；(3) start heating to
(4)关闭阀门15a，将上述原料放入过渡料斗12后，密封；(4) close the valve 15a, after putting the above-mentioned raw materials into the
(5)打开真空泵14b和阀门15f，开始对过渡料斗12抽真空，抽完真空后，关闭阀门15f；(5)
(6)打开阀门15a，将原料放入上料斗11后，开启螺旋推进器9的减速机3b，开始对立式圆筒形反应器1加料；(6) Open valve 15a, after raw material is put into
(7)原料在立式圆筒形反应器1的加热器4产生的热场区反应生成硅化镁，进入冷水套5冷却区冷却；(7) The raw material reacts to generate magnesium silicide in the thermal field area produced by the
(8)通过视镜16观察立式圆筒形反应器1，待立式圆筒形反应器已满，先停止减速机3b，继续反应。(8) Observe the vertical
(9)停止减速机3a后，并让其反转，开始收料。(9) After stopping the
实施例1：Example 1:
硅粉与镁粉按照质量比为1∶1.7的比例混合后，倒入本发明的制备装置中，立式圆筒形反应器加热区的温度控制在550℃。最终得到了硅化镁产物，如图2所示是它的XRD图谱，该图谱中所有XRD衍射峰均与硅化镁的标准卡片35-0773吻合，说明产物为纯度较高的硅化镁。Silicon powder and magnesium powder are mixed according to the mass ratio of 1:1.7, and then poured into the preparation device of the present invention, and the temperature in the heating zone of the vertical cylindrical reactor is controlled at 550°C. The magnesium silicide product was finally obtained, and its XRD spectrum is shown in Figure 2. All the XRD diffraction peaks in the spectrum are consistent with the standard card 35-0773 of magnesium silicide, indicating that the product is magnesium silicide with high purity.
实施例2：Example 2:
硅粉与镁粉按照质量比为1∶1.5的比例混合后，倒入本发明的制备装置中，立式圆筒形反应器加热区的温度控制在650℃。最终得到了硅化镁产物。Silicon powder and magnesium powder are mixed according to the mass ratio of 1:1.5, and then poured into the preparation device of the present invention, and the temperature of the heating zone of the vertical cylindrical reactor is controlled at 650°C. Finally, a magnesium silicide product is obtained.
实施例3：Example 3:
硅粉与镁粉按照质量比为1∶2.3的比例混合后，倒入本发明的制备装置中，立式圆筒形反应器加热区的温度控制在500℃。最终得到了硅化镁产物。Silicon powder and magnesium powder are mixed according to the mass ratio of 1:2.3, and then poured into the preparation device of the present invention, and the temperature in the heating zone of the vertical cylindrical reactor is controlled at 500°C. Finally, a magnesium silicide product is obtained.
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| CN101928005A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Reaction device for continuously synthesizing magnesium silicide |
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| CN1027439C (en) * | 1991-12-14 | 1995-01-18 | 浙江大学 | A kind of method of manufacturing magnesium silicide |
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