CN100441501C - System for preparing nanometer silicon nitride powder - Google Patents

System for preparing nanometer silicon nitride powder Download PDF

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CN100441501C
CN100441501C CN 02138263 CN02138263A CN100441501C CN 100441501 C CN100441501 C CN 100441501C CN 02138263 CN02138263 CN 02138263 CN 02138263 A CN02138263 A CN 02138263A CN 100441501 C CN100441501 C CN 100441501C
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CN1482059A (en
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张芬红
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张芬红
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Abstract

本发明公开一种采用等离子气相合成方法制备氮化硅纳米材料的生产系统,它包括等离子发生器和气相合成装置,气相合成装置产生的固态Si<sub>3</sub>N<sub>4</sub>和HCL进入分离器中,减压分散团聚颗粒,由捕集装置捕集收集成品Si<sub>3</sub>N<sub>4</sub>,等离子发生器采用旋转气流、阳极的机械结构及冷却水压缩,形成高速、稳定火焰的离子弧,由载气分配装置向反应室内沿反应室的腔壁自上而下提供环形载气,使产品颗粒未及时长大时被及时输送,由冷却和捕集装置完成Si<sub>3</sub>N<sub>4</sub>收集,从而得到纳米氮化硅陶瓷粉体。 The present invention discloses a method of using a plasma vapor-phase synthesis of nanomaterials prepared silicon production system, comprising a solid state Si plasma generator means and gas-phase synthesis, synthesis gas generating means <sub> 3 </ sub> N <sub> 4 </ sub> HCL and into the separator, the agglomerated particles dispersed under reduced pressure, collecting the finished product is collected by collecting means Si <sub> 3 </ sub> N <sub> 4 </ sub>, the plasma generator is a rotary airflow the anode of the mechanical structure and cooling water compressed to form a high-speed, stable plasma arc flame, providing an annular carrier gas chamber wall from top to bottom in the reaction chamber by a carrier gas reaction chamber dispensing device, so that the product particles are not grow in time when It is conveyed in time, done by cooling and trapping device Si <sub> 3 </ sub> N <sub> 4 </ sub> was collected to obtain silicon nitride ceramic nano-powder.

Description

制备纳米氮化硅粉体的系统 Nano Silicon Nitride Powder Systems

技术领域 FIELD

本发明公开一种采用采用等离子气相合成方法制备氮化硅纳米材料的生产系统。 The present invention discloses a preparation using silicon nitride using plasma vapor synthesis method nanomaterial production system. 背景技术 Background technique

氮化硅陶瓷粉体应用领域很广,如耐磨工具和零件, 一般耐热耐腐蚀部件,燃气轮机,柴油发动机、化工、国防及其它热装置。 Silicon nitride ceramic powder is very broad field of applications, such as wear-resistant tools and parts, generally heat and corrosion resistant member, gas turbines, diesel engines, chemical, defense and other thermal devices. 目前, 一般氮化硅粉体的制备是采用硅粉氮化的固相工艺,通过氮化产品的 At present, the silicon nitride powder is generally prepared using a solid phase nitriding process of silicon powder, nitriding by product

超细粉碎,要得到纳米(100〜10nm)级的氮化硅则需要采用激光诱导的新工艺,目前国内激光法制备氮化硅超细粉体规模较小且价格昂贵。 Ultrafine grinding, to obtain nanometer (100~10nm) grade silicon nitride you need to use laser-induced new technology, the current ultra-fine powder prepared silicon nitride small-scale and expensive laser domestic legal system. 为了克服激光法存在的不足,技术人员开始将精力集中在利用等离子弧合成纳米氮化硅陶瓷粉体的研究上,以期降低生产成本,虽然可以生产出合格的纳米氮化硅陶瓷粉体,现有技术仍然存在以下缺陷:(1) 作为气相合成纳米材料的能量提供者的等离子发生器存在着能量分散、速度慢、冲刷力不足的缺陷,以及弧焰不稳,从而影响制得的纳米氮化硅陶瓷粉体的产品质量;(2)作为纳米材料的气相合成的具体装置,现有技术无法实现使固态氮化硅和气态氯化氢反应后迅速离开反应区,容易造成颗粒长大,难以将粉体颗粒控制在纳米级U00〜20nm),从而影响制得的纳米氮化硅陶瓷粉体的产品质量,同时由于粉体不能及时迅速离开反应区,将出现产品大量附着在合成装置内。 To overcome the shortcomings of the laser method, the art began to focus on the study of the plasma arc Nanometer silicon nitride ceramic powder utilization, in order to reduce production costs, though it may produce qualified nanometer silicon nitride ceramic powder, now art still has the following defects: (1) a vapor phase synthesis of nanomaterials have energy plasma generator, there is an energy dispersion, slow erosion force is less than the defect, and the arc flame instability, thus affecting the prepared nano nitrogen silicon ceramic powder product quality; (2) the specific apparatus as a gas phase synthesis of nanomaterials, the prior art can not achieve the solid silicon and gaseous hydrogen chloride leaving the reaction zone after the reaction quickly, likely to cause particle growth, it is difficult to powder particles are controlled at the nanoscale U00~20nm), thus affecting the quality of the product obtained nanometer silicon nitride ceramic powder, because the powder can not be promptly while leaving the reaction zone, the large number of products in the synthesis means is attached. 发明内容 SUMMARY

本发明的目的在于提供一种弧焰能量集中、速度快、弧焰稳定的等离子源确保使原料充分参与反应,并且使所制得的产品处在纳米级时迅速离开反应区的制备纳米氮化硅粉体的系统。 Object of the present invention is to provide a flame arc energy concentration, fast, stable flame arc plasma source Nano ensure rapid nitridation reaction zone to leave when the feedstock sufficiently reacted, and the product obtained in the nanoscale silica fume system bodies.

一种制备纳米氮化硅粉体的系统,其特征在于-本发明包括等离子发生器,由工作气体Ar、 N2、 H2经起弧、转弧形成等离子弧,并保持等离子弧区域周围的还原性气氛; A process for preparing nano-silicon nitride powder system, characterized in that - the present invention comprises a plasma generator, a working gas Ar, N2, H2 by arcing, plasma arc into the arc transfer, hold, etc. and a reducing region surrounding the plasma arc atmosphere;

上述等离子发生器产生的等离子弧输至气相合成装置,反应气体SiCW和NH3经管路输入气相合成装置中,并保持物料平衡和反应温度环境; Plasma generator of the plasma arc gas-phase synthesis to the output means, the reaction gas and NH3 SiCW synthesis gas via line input means, maintaining the material balance and the reaction temperature environment;

上述气相合成装置产生的固态SisN4和HCL进入分离器中,减压分散团聚颗粒; Solid SisN4 above synthesis gas generating means HCL and into the separator, the agglomerated particles dispersed under reduced pressure;

上述物料通过引风装置引导经冷却管路进入捕集装置捕集收集成品Si3N4; It said material by introducing air into the cooling circuit through the guide means trap collecting trap apparatus of Si3N4 finished;

所述的等离子发生器包括阳极体,其管腔中设置有彼此配合用于产生等离子弧的阳极部件、阴极部件,所述的阳极部件内部有供等离子弧通过的管状空腔,其一端为锥孔状并与阴级部件的锥状端部构成间隙配合,另一端与气相合成装置相连;靠近阳极部件、阴极部件的配合位置处设有能包附在等离子弧周围并以气旋方式输入起弧、转弧气体的气旋装置;在上述的阳极部件的管状空腔周围设有冷却水腔; The plasma generator comprising an anode body, which is provided with a lumen anode member cooperate with each other for generating a plasma arc, the cathode component, an anode tubular member inside said cavity for plasma arc through which a tapered end a hole shape and constitutes a clearance fit with the tapered end portion of the female member of the class, the other end is connected to vapor phase synthesis means; fitting at a position close to the anode member, the cathode member is provided around the package can be attached to the plasma arc and the arcing in a cyclonic manner input , transfer means arc gas cyclone; a cooling water chamber above the cavity around the tubular anode member;

所述的气相合成装置包括一个由石墨管件制成的内壁呈文氏结构腔体的反应室,其外部设有由夹层套管构成的冷却腔,夹层套管上设有便于同等离子体发生器相连的连接部件,位于连接部件一端的反应室腔室的上端与等离子体发生器的等离子弧输出通路连通,反应室上还设有原料输入管路,所述的反应室的上端设有载气输入通路,该通路与反应室的上部设置的载气分配装置相通,该载气分配装置与反应室之间设有沿反应室的内壁自上而下进入反应室内部的载气通路; Said combining means comprises a vapor phase reaction chamber's inner wall submission of the chamber is made of a graphite tube, which is provided with an external cooling chamber formed of a laminated casing, it is provided to facilitate plasma generator is connected with the sleeve on the interlayer plasma arc plasma generator output path of the upper end of the reaction chamber chamber connecting member, the connecting member is located at one end of the communication and the like, is also provided on the reaction chamber conduit feedstock input, the upper end of the reaction chamber is provided with a carrier gas input means the upper portion of the carrier gas dispensing passageway is provided with a reaction chamber communicating with the carrier gas passage from top to bottom along the inner wall of the reaction chamber into the interior of the reaction chamber, the carrier gas between the reaction chamber and the dispensing means;

所述的阳极部件内部的管状空腔大致为台阶状的圆柱形空腔, 靠近锥孔的部位为小直径细长孔段,上述的管状空腔周围的冷却水腔与阳极体上设置的冷却水通路连通; The interior of the anode tubular member is substantially hollow stepped cylindrical cavity, close to the tapered bore portion of the elongated small diameter bore section, provided on said cooling water chamber with the cooling cavity surrounding the tubular anode body water communicating passageway;

所述的气旋装置包括一个旋气套管,其管壁上设有连通套管内外的通孔,通孔的外端与起弧、转弧气体的气源管路连通,通孔的内端沿旋气套管内壁的切线方向引入; The cyclone apparatus comprises a rotating air tube, which communicates with inside and outside wall of the through hole on the sleeve, the outer end of the through hole arcing, arc gas transfer conduit communicating gas source, the inner end of the through-hole gas is introduced into a spin along the inner wall of the sleeve in the tangential direction;

所述的载气分配装置包括一个与载气输入通路相通的位于等离子入口周围的环状载气腔,环状载气腔与载气通路连通,所述的载气通路是由环状的圆盘与反应室的腔壁之间以环形间隙方式配合形成的。 Said dispensing means comprising a carrier gas input communicating passage positioned around the plasma chamber inlet annular carrier gas with a carrier gas, the carrier gas communication with the annular chamber with a carrier gas passage, a carrier gas passage is a circular ring-shaped a reaction chamber between the disc and the chamber wall to form an annular gap fit manner.

由上述技术方案可知,本发明在结构上采用了三级联合压縮的方案,即提供旋转气流的方式压縮、阳极部件的机械结构压縮及冷却水压縮,通过上述三级压縮的方案使所产生的等离子弧被有效的压縮集中,从而形成高速、稳定火焰的等离子弧,为制备高质量的纳米氮化 Seen from the above technical solution, the present invention is employed in the structure of the joint three compression programs, providing a compression manner of the whirling airflow, the mechanical structure of the anode member and the cooling water of the compressed compression, the compression by the above three program enables the generated plasma arc concentration is effectively compressed, so as to form a high speed, a stable flame, plasma arc, to prepare a high-quality nitride nano

硅陶瓷粉体提供了可靠的能源保障;另外,由上述发生器提供的等离子弧利用所提供的能量,在反应内使原料能够进行最大量的反应,并由载气分配装置向反应室内沿反应室的腔壁自上而下提供环形的载气,在环形载气和快速等离子弧的双重作用下,使产品颗粒未及时长大时被及时输送,并在高速气流的带动下进入冷却系统,而不会附着在反应室的腔壁上,产生的固态Si3N4和HCL经分离器中减压分散团聚颗粒,再由冷却和捕集装置完成Si3N4收集,从而得到纳米氮化硅陶瓷粉体。 Silicon ceramic powder to provide a reliable energy security; In addition, the plasma arc generator provided by the use of the energy provided by the feedstock in the reaction can be carried out a maximum amount of the reaction, by means of carrier gas into the reaction chamber along a dispensing Reaction providing an annular chamber cavity wall from top to bottom of the carrier gas, the dual role of the carrier gas and the annular plasma arc flash, so that the product particles are not promptly conveyed in time grow up, and into the cooling system driven by the high velocity gas stream, without adhering chamber wall of the reaction chamber, and the resulting solid Si3N4 HCL separated agglomerated particles dispersed at reduced pressure, and then cooling is done by collecting and trapping device Si3N4, silicon nitride ceramic powder to obtain nanometer. 附图说明 BRIEF DESCRIPTION

图1是本发明的系统示意图; 1 is a system schematic of the present invention;

图2是本发明中等离子弧发生器和气相合成装置的结构示意图; FIG 2 is a schematic view of a plasma arc generator and a middle gas-phase synthesis apparatus of the present invention;

图3是阳极体的结构示意图; FIG 3 is a schematic view of the anode body;

图4是图3中A—A剖视图; FIG 4 FIG. 3 is a sectional view of A-A;

图5是旋气套管的结构示意图; FIG 5 is a schematic view of the rotating inlet sleeve;

图6是图5中A—A剖视图; FIG 6 is an A-A sectional view of the;

图7是图5中B—B剖视图; 7 is a sectional view B-B in FIG. 5;

图8是图2中的A—A剖视图; FIG 8 is a cross-sectional view A-A in FIG 2;

图9是原料输入管路的结构示意图; 9 is a schematic view of the input feed line;

图IO是分离器的结构示意图。 FIG IO is a schematic view of the separator. 具体实施方式 Detailed ways

以下结合附图和实施例对本发明作进一步的说明。 Hereinafter, the present invention will be further described in conjunction with the accompanying drawings and embodiments.

如图1,本发明包括等离子发生器,由工作气体Ar、 N2、 H2经起弧、转弧形成等离子弧,并保持等离子弧区域周围的还原性气氛; 1, the present invention comprises a plasma generator, a working gas Ar, N2, H2 by arcing, plasma arc into the arc transfer, and the like to maintain a reducing atmosphere surrounding the plasma arc region;

上述等离子发生器产生的等离子弧输至气相合成装置,反应气体 The plasma generator is a plasma arc input to the gas-phase synthesis means, the reaction gas

7SiCL4和NH3经管路输入气相合成装置中,并保持物料平衡和反应温度环境; 7SiCL4 and NH3 synthesis gas via line input means, maintaining the material balance and the reaction temperature environment;

上述气相合成装置产生的固态Si3N4和HCL进入分离器中,减压分散团聚颗粒; Si3N4 above solid and gas phase synthesis means generates HCL into the separator, the agglomerated particles dispersed under reduced pressure;

上述物料通过引风装置引导经冷却管路进入捕集装置捕集收集成品Si3N4。 It said material by introducing air through the cooling circuit into the means for guiding the collection device collecting trap finished Si3N4.

参见图2,等离子发生器包括正阳极体10,其管腔中设置有彼此配合用于产生等离子弧的阳极部件20、阴极部件30,所述的阳极部件20内部有供等离子弧通过的管状空腔21,其一端为锥孔状并与阴极部件30的锥状端部构成间隙配合,另一端与气相合成装置相连,由本装置产生的等离子弧由该管状空腔21引入氮化硅的气相合成装置中,为合成氮化硅提供可靠的热源;靠近阳极部件20、阴极部件30的配合位置处设有能包附在等离子弧周围并以气旋方式输入起弧、转弧气体的气旋装置,在该气旋装置的作用下,起弧、转弧气体进入阳极部件20、阴极部件30配合产生等离子弧的部位时,由于起弧、转弧气体是冷气,因此在起弧、转弧气体的旋气和冷态的双重作用下,能将产生的等离子弧有效地压縮、集中,避免等离子弧分散。 Referring to Figure 2, the plasma generator comprises a positive anode body 10, which is provided with a lumen with an anode means for generating a plasma arc 20 to each other, the cathode member 30, the interior of the anode tubular member 20, the air supply through the plasma arc synthesis gas chamber 21, one end of a tapered hole shape and configuration of the cathode member and the tapered end portion 30 is a clearance fit, the other end is connected to vapor phase synthesis, and is generated by the plasma arc apparatus introduced by the silicon nitride of the tubular cavity 21 apparatus, a reliable source for the synthesis of silicon nitride; 20 proximate the anode member, the cathode member 30 is provided around the fitting position of the plasma arc can be attached to the package in a cyclonic manner and input arc, arc gas cyclone transfer means, in when the effect of the cyclone device, arcing, turn the arc gas into the anode member 20, the cathode member 30 with generating a plasma arc portion due to arcing, transferred arc gas is cold air, so the arc, transferred arc gas spin-gas plasma arc effectively compressed, concentrated, and to avoid the dual role of plasma a cold state, an arc can produce a dispersion. 所述的阳极部件20内部的管状空腔21大致为台阶状的圆柱形空腔,靠近锥孔的部位为小直径细长孔段,这种孔径结构的空腔在引导等离子弧通过时,能有效起到压縮、集中等离子弧的作用;上述的管状空腔21周围的冷却水腔22与阳极体10上设置的冷却水通路11连通,设置冷却水腔22 同样可以起到压縮、集中等离子弧的作用。 The internal anode cavity 21 of the tubular member 20 is substantially cylindrical cavity is stepped, tapered portion near the small diameter hole section of the elongated hole, the cavity of this pore structure in the plasma arc through the guide, can effective compression functions, concentration effect of the plasma arc; around the tubular cavity 21 of the cooling water and the cooling water chamber 22 disposed on the anode body 10 communicates passage 11, a cooling water chamber 22 also serve to compress, concentrated effect of the plasma arc.

参见图2、 5、 6、 7,所述的气旋装置包括一个旋气套管40,其管壁上设有连通套管内外的通孔41,通孔41的外端与起弧、转弧气体的气源管路连通,通孔41的内端沿旋气套管40内壁的切线方向引入, 这样可以确保对所产生的等离子弧的有效压縮。 Referring to FIG. 2, 5, 6, 7, said apparatus comprising a cyclone air rotating sleeve 40 which is provided with a through hole 41, the outer end of the through hole 41 communicates with the inside and outside arc tube wall sleeve, transfer arc gas supply conduit communicates gas, the inner end of the through hole 41 of the casing along a tangential direction of the spin gas introduced into the inner wall 40, which can ensure the effective compression or the like of ions generated arc. 所述的旋气套管40 上的通孔41在同一截面上彼此对称的设置3~5个,图5中给出的是4 The spin-gas sleeve through hole 4041 disposed symmetrically to each other on the same cross section 3 to 5, is given in Figure 5 4

个通孔,它们从同一截面的沿圆周彼此均匀对称布置的四个方向进入, 图6中的通孔41供输入起弧气体;在另一截面上,沿圆周彼此均匀对称的设置3〜5个,图7中的通孔41为四个,它们供输入转弧气体。 Through-holes are symmetrically arranged in four directions from circumferentially uniformly from one another into the same section, the through holes 641 for inputting FIG arcing gas; on another cross section, circumferentially disposed symmetrical to each other ~ 5 a through hole 741 in FIG four, they turn for inputting the arc gas. 如图6、 7中的结构所示,两个截面上的通孔41的气流进入后形成的的旋转方向相同,这样可以增强气旋效果,使等离子弧四周受到的压縮均匀一致,使其保持集中、快速的特性。 6, the structure of FIG. 7, FIG same rotational direction after the formation of the gas flow through hole 41 into the two sections, which can enhance the effect of the cyclone, so that the plasma arc is uniformly compressed by four weeks, remains centralized, fast characteristics.

参见图2、 3、 4,所述的管状空腔21中的小直径细长孔段的孔长与孔径比通常为2〜5,比值为3〜4较为理想。 Referring to FIG. 2, 3, 4, the small-diameter hole length of the elongated aperture with the bore section in said tubular cavity 21 is generally 2 ~ 5 ratio, a ratio of 3 to 4 is preferable. 所述的阳极体10上设有两个冷却水的输入口12和两个输出口13,这种多路冷却水通路的结构可以保证冷却的均匀性,从而确保等离子弧四周受到的压縮均匀一致,使其保持集中、快速的特性。 With the anode body 10 on the two cooling water inlet port 12 and two output ports 13, which multiplex structure the cooling water passage may ensure the uniformity of the cooling, thereby ensuring that the plasma arc being uniformly compressed four weeks consistent, to keep it focused and fast characteristics. 输入口12对应于阳极部件20、阴极部件30的锥面、锥孔之间配合间隙所在的位置,两输入口12彼此平行且反向的沿阳极体10内腔的切线方向引入,这种位置的设置是为了使等离子弧从刚产生开始既受到来自周围的均匀有效的压縮。 The input port 12 corresponds to a position where the gap between the fitting 20, the tapered surface, the tapered hole part of the anode of the cathode member 30, 10 introduced into the lumen of a tangential direction of the input port 12 of the two parallel and opposite each other along the anode body, such position is provided to the plasma arc is generated from beginning either immediately subjected to a uniform and effective compression from the surroundings.

由图4可见,两个水流输出口13分别位于与上述的输入口12垂直的直径两端,同时参见图1、 2、 3,所述的阳极体IO上连有套在阳极部件20外部的套管50,套管50与阳极部件20的外壁之间的空腔51分别与上述的管状空腔21和冷却水通路11相连构成冷却水的通路。 Seen from Figure 4, two water output port 13 at each end and the diameter perpendicular to the above input port 12, see also 1, 2, FIG 3, the anode body is connected with a sleeve on IO external anode member 20 sleeve 50, the sleeve cavity 51 between the outer wall 50 of the anode member 20 are identical to said tubular cavity 21 and 11 is connected to a cooling water passage constituting the cooling water passage. 套管50是一个工艺结构部件,通过加设套管50—方面便于构成 The sleeve member 50 is a process structure, configuration facilitates sleeve 50 terms provided by the addition of

冷却水的通路,同时又使得各部件的结构不致于太过复杂。 A cooling water passage, while making the structure of each member as not too complex.

如图2所示,所述的阳极体10上设有调节阳极、阴极部件20、 30的锥面、锥孔之间配合间隙的调整机构,通过该调整机构对阳极、 阴极部件20、 30的锥面、锥孔之间配合间隙实施调节,可以改变工作气体的流量,这对改变等离子弧弧压有显著效果,从而可以满足不同工艺要求的产品对电压和电流的要求。 As illustrated, the anode 2 is provided on the body 10 with the adjustment mechanism adjusting the gap between the anode and the cathode member 20, the tapered surface 30, tapered bore, through which the adjusting mechanism for the anode, the cathode member 20, 30 tapered surface, with the gap between the cone regulation embodiment, the flow rate of the working gas can be changed, this change has a significant effect on the plasma arc arc voltage to meet different process requirements of the product of the voltage and current requirements. 所述的配合间隙的调整机构包括一个局部管体位于阳极体10内部并与其相对固定的套管60,套管60的里端抵靠在旋气套管40上,阴极部件30与内部设有冷却水路的调节杆70相连,调节杆70在套管60和旋气套管40内腔中可沿轴向移动,阴极部件30的柱形外表面与旋气套管40之间有供起弧、转弧气体进入阳极部件20、阴极部件30锥面之间的通路间隙。 The fit clearance adjustment mechanism includes a local anode body located inside tubular body 10 and sleeve 60 fixed relative thereto, in the end of the sleeve 60 against the sleeve 40 screwed gas, the cathode member 30 is provided with an internal the cooling water passage 70 is connected to the adjusting lever, the adjusting lever 70 in the lumen of the sleeve 40 axially movable, cylindrical outer surface of the cathode member 30 and screwed in the sleeve 60 and the rotary air inlet sleeve 40 with a supply of arcing between , arc transfer member 20 into the anode gas passage 30, the gap between the tapered surface of the cathode member.

以下结合图2对本发明中的等离子发生器的工作原理作简要说明。 2 in conjunction with the following operating principle of the present invention is the plasma generator will be briefly described.

给本发明接通合适的高频起弧电源,经气旋装置输入符合工艺条件的高压氮、氢、氩气,电气系统在适当电压和电流情况下高频起弧, 所产生的等离子弧在旋气压縮、机械压縮以及冷却压縮的多元复合压縮环境下获得集中、快速的等离子弧,并通过弧径通路到达气相合成装置为其提供合成环境。 The present invention is suitable for turning on the high-frequency arc power, high pressure nitrogen gas cyclone via the input line with the process conditions, hydrogen, argon, where appropriate electrical system voltage and high frequency current arc, plasma arc generated during the spin gas compression, mechanical compression and cooling the compressed ambient polyhydric compound obtained compression concentrated, rapid plasma arc, and to provide synthetic environments diameter passage through an arc device to the vapor phase synthesis.

以下结合图1对间隙的调整机构的工作原理简要说明。 The following works in conjunction with FIG gap adjusting mechanism 1 is briefly described.

套管60和旋气套管40通过压帽80与阳极体10固定,转动套管60上设有转柄90,由于转柄90只能相对于套管60转动,与转柄90 螺纹配合的调节杆70则沿其轴向移动,同时由于调节杆70的里端与阴极部件30相连,所以转动转柄90时,阴极部件30的尾段圆柱状的部位在旋气套管40内沿轴向移动,从而实现了阳极部件20、阴极部件30的锥面、锥孔之间配合间隙的调整。 Rotating the sleeve 60 and the sleeve 40 by the gas pressure cap 80 and the anode body 10 is fixed, rotating the sleeve 90 with the crown 60, the crown 90 because only the sleeve 60 is rotated relative to the crown 90 and threadedly engaged adjusting rod 70 to move axially, while the inner end is connected to the cathode Since the adjustment member 30 of the lever 70, so that rotation of the crown 90, the shaft 40 along the end section of the cylindrical portion of the cathode sleeve member 30 is screwed in the gas mobile, enabling adjustment of the gap between the fitting 20, the tapered surface, the tapered hole 30 of the anode members cathode member.

参见图2、 8,本发明公开的制备纳米氮化硅粉体的气相合成装置包括一个由石墨管件120制得的内壁呈现为文氏结构腔体的反应室121,其外部设有由夹层套管130构成的冷却腔131,可以实现强制制冷,夹层套管130上设有便于同等离子体发生器相连的连接部件110, 位于连接部件110 —端的反应室121腔室的上端与等离子体发生器的等离子弧输出通路连通,反应室121上还设有原料输入管路150,所述的反应室121的上端设有载气输入通路100,该通路100与反应室121的上部设置的载气分配装置相通,该载气分配装置与反应室121 之间设有沿反应室121的内壁自上而下进入反应室121内部的载气通路141。 Referring to FIG. 2, 8, Nano Silicon Nitride Powder vapor synthesis apparatus disclosed in the present invention comprises a reaction chamber presenting a venturi structure 121 is cavity 120 by an inner wall made of a graphite tube, which is provided with an external sleeve of a sandwich pipe 130 constituting the cooling chamber 131, and forced cooling may be achieved, sleeve 130 is provided on the interlayer facilitate plasma generator is connected to the same connecting member 110, the connecting member 110 is located - the end of the reaction chamber 121 and the upper chamber of the plasma generator the plasma arc output communication passage, a carrier gas is also a material dispensing feed line 150, the upper end of the reaction chamber 121 is provided with a carrier gas feed passage 100, the passage 100 and the upper portion of the reaction chamber 121 of the reaction chamber 121 on means in communication with the carrier gas passage 141 from top to bottom along the inner walls of the reaction chamber 121 to enter the interior of the reaction chamber 121 between the dispensing means and carrier gas the reaction chamber 121. 反应室121采用文氏结构,其喉管部位可以加大离子流速度, 可达超音速,扩展管部位加速冷却,这样可以有效防止晶粒长大。 The reaction chamber 121 using a venturi structure, which can increase the throat portion of the plasma stream velocity up to supersonic expansion pipe portion accelerated cooling, can effectively prevent the grain growth.

所述的载气分配装置包括一个与载气输入通路100相通的位于等离子入口周围的环状载气腔142,环状载气腔142与载气通路141连通。 Said dispensing means comprising a carrier gas around the input path 100 communicating the annular inlet located in the plasma chamber 142 the carrier gas with a carrier gas, the carrier gas annular chamber 142 communicates with a carrier gas passage 141.

所述的载气通路141是由环状的圆盘140与反应室121的腔壁之间以均匀的环形间隙方式配合形成的。 The carrier gas passage 141 between the chamber wall by an annular disc 140 and the reaction chamber 121 in a uniform manner with an annular gap is formed. 通过载气分配装置140可以实现顶吹功能,即具有一定压力和流量的N2气流连续沿反应室121的腔 Function 140 may be implemented by top blowing a carrier gas dispensing device, i.e. a certain pressure and flow rate of the reaction chamber along the continuous N2 gas flow chamber 121

壁向下吹扫,使反应生成的粉体及时沿管路流向捕集装置。 Wall sweep down, the powder resulting reaction promptly flows along conduit trapping device.

如图9所示,所述的原料输入管路150设置若干个,并且均匀对 9, the feed conduit 150 is provided a plurality of input and uniformity of

称布置在垂直于轴向的等高截面上,伸至反应室121内的原料输入管路150端部位于靠近等离子弧进入反应室入口122的下方,原料输入管路150的均匀布置使反应时气相离子浓度均匀,气相化学合成过程均匀且稳定。 When disposed in said cross-section perpendicular to the axial direction of the contour, the end portion 150 extends to the raw material input conduit 121 is located in the reaction chamber near the plasma arc into the reaction chamber below the inlet 122, the raw material input conduit 150 is arranged so that a uniform reaction homogeneous gas-phase ion concentration, gas-phase chemical synthesis uniform and stable. 原料输入管路150有四个,端部的出口151与水平面之间以夹角a输至反应室入口122的下方,其中0《a《60。 Feedstock input conduit 150 has four, between the outlet end portion 151 and the horizontal plane at an angle to output a reaction chamber below the inlet 122, where 0 "a" 60. ,如图l、 2、 3所示,将端部的出口设计成多种结构,可以是水平的、向下倾斜的,倾斜的具体角度可以有多个,以适应不同材料各自的反应过程, 例如生产氮化硅纳米粉体时,氨气是水平输入的,SiCL4是倾斜输入的,即氨气离子自上而下与SiCL4离子合成生成Si3 N4。 FIG. L, 2, 3, the outlet end portion designed into a variety of structures, can be horizontal, downwardly inclined angle may have a plurality of specific, to accommodate the respective different reaction materials, for example, the production of silicon nitride nano powders, ammonia level is input, the lean input is SiCl4, i.e. from top to bottom with SiCl4 plasma ammonia synthesis ion generating Si3 N4. 根据生产产品的实际所需原料气,选择相应的进料管路,并且根据生产不同产品反应的具体工艺参数在确定反应温度时,利用等离子弧温度的梯度特定规律,以生产不同类型的产品。 The actual production of the desired product gas feed, select the feed line, depending on the specific process parameters and different products of the reaction when the reaction temperature is determined, with a particular rule with a gradient temperature plasma arc, to produce different types of products.

本发明中采用在同一等高截面上均匀布置原料输入管路150的方案,可以显著减化部件的加工难度,并且有效改善了装置的装配工艺禾口布局。 The present invention uses a uniform feedstock input disposed on the same cross-sectional contour line of the program 150, may be significantly reduced processing difficulty of the member, the assembly process and effectively improves the layout of the installation opening Wo.

如图10所示,气相合成装置下端有一个由小变大的锥状过渡管161与分离器160相连,本方案中,Si3N4从气相合成装置经过小管径的喉管后进入分离器160,由于分离器160中的容积突然变大,Si3N4 的环境压力也就突然减少,因此出现爆炸现象,从而将有效分散团聚颗粒;参见图1,分离器160上连有水平状布置的冷却管路173,在冷却管路173上方还设有一个与冷却管路173平行的冷却管路171, 一端与捕集装置180相连的冷却管路171与冷却管路173之间设有将两者连通的竖向冷却管路172,冷却管路172的下端设有可拆卸的端盖174,这种管路的布置方式,有利于设备安装、维修及清洁工作。 10, has a lower vapor synthesis apparatus from small to large tapered transition tube 161 is connected to the separator 160, in the present embodiment, Si3N4 gas-phase synthesis from the apparatus after the small diameter pipe enters the separator 160, Since the volume of the separator 160 is suddenly increased, the ambient pressure will suddenly decrease Si3N4, resulting in explosions so as to effectively disperse the agglomerated particles; see FIG. 1, a cooling pipe is connected horizontally disposed passage 173 of the separator 160 , 173 above the cooling circuit and the cooling circuit is also provided with a cooling line 173 parallel 171, 171 is provided between the cooling line and the cooling line 173 is connected to one end of the trapping device 180 is in communication both vertical the cooling circuit 172, cooling line 172 of the lower end cap 174 is detachably provided, this conduit arrangement is conducive to installation, maintenance and cleaning work.

在图1中,捕集装置180之后还设置了淋洗回收装置190,使本系统对对尾气加以处理,从而满足环保要求。 In FIG. 1, after the collection device 180 is also provided rinsed recovery 190, enable the system to be processed tail gas to meet the environmental requirements.

Claims (7)

1、一种制备纳米氮化硅粉体的系统,其特征在于: 包括等离子发生器,由工作气体Ar、N2、H2经起弧、转弧形成等离子弧,并保持等离子弧区域周围的还原性气氛; 上述等离子发生器产生的等离子弧输至气相合成装置,反应气体SiCL4和NH3经管路输入气相合成装置中,并保持物料平衡和反应温度环境; 上述气相合成装置产生的固态Si3N4和HCL进入分离器中,减压分散团聚颗粒; 上述物料通过引风装置引导经冷却管路进入捕集装置捕集收集成品Si3N4; 上述等离子发生器包括阳极体(10),其管腔中设置有彼此配合用于产生等离子弧的阳极部件(20)、阴极部件(30),所述的阳极部件(20)内部有供等离子弧通过的管状空腔(21),其一端为锥孔状并与阴极部件(30)的锥状端部构成间隙配合,另一端与气相合成装置相连;靠近阳极部件(20)、阴极部件(30)的配合位置处设有能 1, a nano-system for preparing silicon nitride powder, characterized by: a plasma generator, a working gas Ar, N2, H2 by arcing, plasma arc into the arc transfer, hold, etc. and a reducing region surrounding the plasma arc atmosphere; the plasma generator of the plasma arc input to the gas-phase synthesis means, the reaction gas SiCL4 and NH3 via line input gas synthesis unit, and maintain mass balance, and the reaction temperature environment; solid Si3N4 said vapor-phase synthesis means generates and HCL enters the separator vessel, the agglomerated particles dispersed under reduced pressure; the above-described materials by introducing air into the cooling circuit through the guide means trap collecting trap apparatus of Si3N4 finished; the plasma generator comprising an anode body (10), which is provided with a lumen fitted with each other the anode member (20), the cathode member (30) of the plasma arc generating et al., (20) inside the anode member of the tubular cavity for the plasma arc through (21), one end of a tapered hole shape and the cathode member ( 30) constitutes a tapered end portion with a gap, and the other end connected to vapor phase synthesis means; fitting at a position close to the anode member (20), the cathode member (30) is provided with energy 附在等离子弧周围并以气旋方式输入起弧、转弧气体的气旋装置;在上述的阳极部件(20)的管状空腔(21)周围设有冷却水腔(22); 上述气相合成装置包括一个由石墨管件(120)制成的内壁呈文氏结构腔体的反应室(121),其外部设有由夹层套管(130)构成的冷却腔(131),夹层套管(130)上设有便于同等离子体发生器相连的连接部件(110),位于连接部件(110)一端的反应室(121)腔室的上端与等离子体发生器的等离子弧输出通路连通,反应室(121)上还设有原料输入管路(150),所述的反应室(121)的上端设有载气输入通路(100),该通路(100)与反应室(121)的上部设置的载气分配装置相通,该载气分配装置与反应室(121)之间设有沿反应室(121)的内壁自上而下进入反应室(121)内部的载气通路(141); 所述的阳极部件(20)内部的管状空腔(21)大致为台阶状的圆柱形空腔,靠近锥孔的部位为小直径 Attached around the plasma arc and the arc in a cyclonic manner the input, transfer means arc gas cyclone; (21) around a cooling water chamber (22) in the cavity of the tubular member above the anode (20); and said apparatus comprises a vapor-phase synthesis a reaction chamber (121) an inner wall structure of the cavity's submission of a graphite tube member (120) is made, which is provided outside the cooling chamber (131) by a sandwich sleeve (130) configured, the sleeve is provided on the interlayer (130) there facilitate connection member connected with the plasma generator (110), located in the connecting member (110) at one end of the reaction chamber (121) and the upper end of the plasma generator of the plasma chamber equal arc output passage communicating the reaction chamber (121) There is also a raw material input conduit (150), an upper end of said reaction chamber (121) is provided with a carrier gas feed passage (100), the dispensing device on top of the carrier gas passage (100) with the reaction chamber (121) provided communication, along with the reaction chamber (121) from top to bottom into the inner wall of the reaction chamber (121) inside of the carrier gas passage (141) between (121) of the carrier gas with the reaction chamber dispensing means; said anode member ( 20) inside the tubular cavity (21) substantially stepped cylindrical cavity, close to the taper hole a small diameter portion 长孔段,上述的管状空腔(21)周围的冷却水腔(22)与阳极体(10)上设置的冷却水通路(11)连通; 所述的气旋装置包括一个旋气套管(40),其管壁上设有连通套管内外的通孔(41),通孔(41)的外端与起弧、转弧气体的气源管路连通,通孔(41)的内端沿旋气套管(40)内壁的切线方向引入; 所述的载气分配装置包括一个与载气输入通路(100)相通的位于等离子入口周围的环状载气腔(142),环状载气腔(142)与载气通路(141)连通,所述的载气通路(141)是由环状的圆盘(140)与反应室(121)的腔壁之间以环形间隙方式配合形成的。 The elongated hole section is provided on the cooling water passage (10) of the tubular cavity (21) surrounding the cooling water chamber (22) and the anode body (11) in communication; said rotating means includes a cyclone air inlet sleeve (40 ), which is provided with a through hole communicating inside and outside the sleeve (41), the through-hole (41) on the outer end of the arc tube wall, the inner end of the rotation arc gas source gas communication conduit, the through-hole (41) along the rotary air sleeve (40) is introduced into the tangential direction of the inner wall; said dispensing means comprises a carrier gas with a carrier gas input channel (100) communicating with the plasma inlet positioned around an annular carrier gas chamber (142), an annular carrier gas chamber (142) communicates with a carrier gas passage (141), the carrier gas passage (141) is an annular disc (140) cooperate to form an annular gap between the chamber wall and the way the reaction chamber (121) of .
2、 根据权利要求1所述的制备纳米氮化硅粉体的系统,其特征在于:所述的阳极体(10)上设有调节阳极部件(20)、阴极部件(30) 的锥面、锥孔之间配合间隙的调整机构。 2, preparation of nano silicon nitride powder system according to claim 1, wherein: said anode body provided with the anode adjusting member (20), the cathode member (30) of the conical surface (10), with the adjusting mechanism of the gap between the tapered hole.
3、 根据权利要求1或2所述的制备纳米氮化硅粉体的系统,其特征在于:所述的管状空腔(21)中的小直径细长孔段的孔长与孔径比为2〜5,所述的阳极体(10)上设有两个冷却水的输入口(12)和两个输出口(13),输入口(12)对应于阳极部件(20)、阴极部件(30) 的锥面、锥孔之间配合间隙所在的位置,两输入口(12)彼此平行且反向的沿阳极体(10)内腔的切线方向引入。 3, nano-silicon nitride powder prepared according to claim 1 or system of claim 2, wherein: the elongated hole length and aperture ratio of the small-diameter bore section of said tubular cavity (21) is 2 ~ 5, the anode body is provided with two cooling water inlet port (12) and two output ports (13) (10), the input port (12) corresponding to the anode member (20), the cathode member (30 ) fitting position where the gap between the tapered surface, the tapered hole, introducing (10) the tangential direction of the two input ports of the lumen (12) parallel to one another and in opposite directions along the anode body.
4、 根据权利要求3所述的制备纳米氮化硅粉体的系统,其特征在于:两个输出口(13)分别位于与上述的输入口(12)垂直的直径两端,所述的阳极体(10)上连有套在阳极部件(20)外部的套管(50), 套管(50)与阳极部件(20)的外壁之间的空腔(51)分别与上述的管状空腔(21)和冷却水通路(11)相连构成冷却水的通路。 4, the silicon nitride powder according to claim preparing nano system according to claim 3, wherein: two output ports (13) at each end of the aforementioned vertical inlet (12) diameter, said anode even with a sleeve cavity between the outer wall of the outer sleeve (50), the sleeve (50) and the anode member (20) in the anode member (20) (51) are identical to said cavity of the tubular body (10) (21) and a cooling water passage (11) is connected to the coolant passage configuration.
5、 根据权利要求2所述的制备纳米氮化硅粉体的系统,其特征在于:所述的配合间隙的调整机构包括一个局部管体位于阳极体(IO) 内部并与其相对固定的套管(60),套管(60)的里端抵靠在旋气套管(40)上,阴极部件(30)与内部设有冷却水路的调节杆(70)相连, 调节杆(70)在套管(60)和旋气套管(40)内腔中可沿轴向移动,阴极部件(30)的柱形外表面与旋气套管(40)之间有供起弧、转弧气体进入阳极部件(20)、阴极部件(30)锥面之间的通路间隙。 5. The silicon nitride powder of claim preparing nano system according to claim 2, characterized in that: the gap adjustment mechanism comprises mating inner tube positioned a partial anode body (IO) and opposite the fixed sleeve (60), the sleeve (60) abuts the inner end of the rotary air sleeve (40), the cathode member (30) is provided with an internal cooling water passage of the adjusting lever (70) is connected to the adjusting lever (70) in the sleeve between the tube (60) and rotary air sleeve (40) axially movable in the lumen, the cathode member (30) and the rotation of the cylindrical outer surface of the gas tube (40) for the arc, the arc gas into the transfer the anode member (20), the cathode member (30) via a gap between the tapered surface.
6、 根据权利要求1所述的制备纳米氮化硅粉体的系统,其特征在于:所述的原料输入管路(150)设置若干个,并且均匀对称布置在垂直于轴向的等高截面上,伸至反应室(121)内的原料输入管路(150) 的端部位于靠近等离子弧进入反应室(121)的入口(122)的下方, 原料输入管路(150)有四个,端部的出口与水平面之间以夹角a输至反应室入口(122)的下方,其中0《a《60。 6, the silicon nitride nano powders prepared according to the system of claim 1, wherein: said starting material feed line (150) is provided a plurality of, and arranged in a symmetrical contour of the cross section perpendicular to the axial below the inlet (122), the starting material feed line extending to the reaction chamber (150) in (121) located adjacent an end portion of a plasma arc into the reaction chamber (121), a raw material input conduit (150) has four, between the outlet end of the horizontal portion at an angle to output a reactor chamber inlet (122) below, wherein 0 "a" 60. .
7、 根据权利要求1所述的制备纳米氮化硅粉体的系统,其特征在于:气相合成装置下端有一个由小变大的锥状过渡管(161)与分离器(160)相连,分离器(160)上连有水平状布置的冷却管路(173), 在冷却管路(173)上方还设有一个与冷却管路(173)平行的冷却管路(171), 一端与捕集装置(180)相连的冷却管路(171)与冷却管路(173)之间设有将两者连通的竖向冷却管路(172),冷却管路(172) 的下端设有可拆卸的端盖(174)。 7, the silicon nitride nano powders prepared according to the system of claim 1, wherein: a lower vapor synthesis apparatus from small to large tapered transition tube (161) and the separator (160) connected to the separation even with a cooling circuit (173) arranged horizontally on the (160), at (173) above is also a cooling line (173) parallel to the cooling line of the cooling circuit (171), one end of the trap means (180) the cooling circuit (171) connected to the cooling circuit communicating with the two vertical cooling lines (172) between (173), the lower end of the cooling circuit (172) is provided with a removable end caps (174).
CN 02138263 2002-09-09 2002-09-09 System for preparing nanometer silicon nitride powder CN100441501C (en)

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CN101550600B (en) 2009-04-22 2011-05-25 中国地质大学(北京) A method to prepare a high-purity high-density monocrystalline silicon nitride nano array
CN104203813B (en) * 2012-03-28 2017-04-26 宇部兴产株式会社 A method for producing silicon nitride powder and silicon nitride powder and silicon nitride sintered body and a circuit board using thereof
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