WO2022142527A1 - 一种脉冲式金属粉制备冷凝方法 - Google Patents

一种脉冲式金属粉制备冷凝方法 Download PDF

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WO2022142527A1
WO2022142527A1 PCT/CN2021/120665 CN2021120665W WO2022142527A1 WO 2022142527 A1 WO2022142527 A1 WO 2022142527A1 CN 2021120665 W CN2021120665 W CN 2021120665W WO 2022142527 A1 WO2022142527 A1 WO 2022142527A1
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metal powder
cooling chamber
preparing
pulsed
powder
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PCT/CN2021/120665
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English (en)
French (fr)
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柴立新
汪艳春
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江苏博迁新材料股份有限公司
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Priority to JP2023528288A priority Critical patent/JP2023550716A/ja
Publication of WO2022142527A1 publication Critical patent/WO2022142527A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material

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  • the present application relates to the technical field of powder preparation, in particular to a method for preparing and condensing pulsed metal powder.
  • the physical gas phase method is mostly used to produce metal nickel powder. After the metal is melted and gasified in the molten pool of the reactor, the metal vapor enters the condenser under the action of nitrogen in the system, and is cooled by nitrogen in the condenser to form powder and then enter the collection tank.
  • the metal vapor is directly condensed through the condenser tube, and the inner volume of the condenser tube is small, and the gas-solid ratio of the powder in the pulse cooling chamber is only 1: (200-250), resulting in the existence of The problems of high powder concentration, high temperature and insufficient powder cooling.
  • the gas flow velocity in the tube is high, and the flow state Reynolds number Re ⁇ 3000, so the system flow state is excessive flow and turbulent flow.
  • the metal nickel powder obtained by the existing method is too large, the probability of collision between the powder particles and between the particles and the tube wall will increase, and then in a high temperature environment, the uncooled metal particles are sintered with each other. , it is easy to form a conjoined body, or form irregular shaped particles, resulting in a decrease in the quality of the powder.
  • the purpose of the present application is to provide a method for preparing and condensing pulsed metal powder, so as to achieve the purpose of improving the distribution uniformity and yield of metal powder. Its specific plan is as follows:
  • a pulsed metal powder preparation and condensation method comprises the following steps:
  • Step 1 put the raw material into the reactor to melt and evaporate, so that the metal vapor enters the condensation tube to crystallize and nucleate to form a powder blank;
  • Step 2 The powder blanks enter the pulse cooling chamber for cooling to form single metal particles, and the pulse cooling chamber is filled with nitrogen during the pulse cooling;
  • Step 3 The single metal particles are collected in the collector under the action of air flow
  • Step 4 The backflushing device in the collector blows the metal powder back into the powder collector for collection.
  • the pulse cooling chamber includes a dish-shaped head, a cylinder, an observation hole and a gas distributor; the gas distributor is an annular gas distributor.
  • the annular gas distributor is provided with a plurality of gas nozzles distributed in equal arcs, and the open ends of the gas nozzles face the center of the condensation pipe.
  • the cross-sectional area ratio of the condensation tube to the pulse cooling chamber is 1:(8-15); the volume ratio of the condensation tube to the pulse cooling chamber is 1:(10-15).
  • the metal powder is spherical, and the particle size is less than 100 nm.
  • the pulse cooling chamber is under negative pressure; the pressure in the reactor is 70-90 kPa.
  • a zirconia lining layer is provided in the condensation tube.
  • the gas-solid ratio of the metal powder in the pulse cooling chamber is 1:(1500-2000).
  • the condensation tube and/or the pulse cooling chamber are provided with an interlayer, and the interlayer has cooling water therein.
  • step 3 the single metal particles enter the collector from the pulse cooling chamber through the inclined pipe.
  • the present application provides a method for preparing and condensing pulsed metal powder, and the method for preparing and condensing pulsed metal powder has the following beneficial effects:
  • the metal vapor forms less slag on the chamber wall, less waste powder, and achieves the purpose of increasing the powder yield by 15%.
  • FIG. 1 is a schematic structural diagram of an embodiment of a pulsed metal powder preparation condensing device of the present disclosure.
  • a pulsed metal powder preparation condensation device includes a reactor 1 , a condensation tube 2 , a pulsed cooling chamber 3 , a collector 4 and a powder collector 5 .
  • the reactor 1 is used for melting and evaporating raw materials to obtain metal vapor.
  • the condenser tube 2 is connected to the reactor 1 and the pulse cooling chamber 3, so that the metal vapor crystallizes and nucleates when passing through the condenser tube 2.
  • the powder blanks that crystallize and nucleate The spacing between particles instantly expands, greatly reducing the collision probability of each powder blank particle, thereby effectively reducing the generation of conjoined particles and slag.
  • the collector 4 is used to collect the metal powder obtained by cooling through the pulse cooling chamber 3 , and the metal powder enters the powder collector 5 under the backflushing action of the backflushing tank in the collector 4 for collection.
  • a zirconia lining layer is arranged in the condenser tube 2, and an interlayer is arranged in the condenser tube 2 and/or the pulse cooling chamber 3. There is cooling water in the interlayer.
  • the pulse cooling chamber 3 includes a dish-shaped head, a cylinder, a viewing hole and a gas distributor 6 .
  • the dish-shaped head is used for sealing connection with the condensing pipe 2 .
  • Cylinders are used for cooling and obtaining metal powders.
  • the observation hole is used to observe the formation of metal powder in the cylinder.
  • the gas distributor 6 is an annular gas distributor, and a plurality of gas nozzles with equal arc distribution are arranged on the gas distributor 6 .
  • the open end of the gas nozzle faces the center of the condenser tube 2 to effectively slow down the gas flow rate and blow out the powder blanks.
  • the cross-sectional area ratio of the condenser tube 2 and the pulse cooling chamber 3 is 1:(8-15), and the volume ratio of the condenser tube 2 and the pulse cooling chamber 3 is 1:(10-15), so as to greatly reduce the The collision probability of each powder blank particle can effectively reduce the generation of conjoined particles and slag.
  • the present disclosure provides a pulsed metal powder preparation and condensation method.
  • a preparation condensation device consisting of a reactor 1, a condenser tube 2, a pulsed cooling chamber 3, a collector 4 and a powder collector 5, the pulsed cooling method is used to obtain metal powder.
  • the method of pulse cooling includes the following steps:
  • Step 1 The raw materials are put into the reactor 1 to melt and evaporate, so that the metal vapor enters the condenser tube 2 for crystallization and nucleation to form powder blanks.
  • Step 2 The powder blank enters the pulse cooling chamber 3 for cooling to form single metal particles, and the pulse cooling chamber 3 is filled with nitrogen during pulse cooling.
  • Step 3 the single metal particles enter the collector 4 through the inclined pipe under the action of the air flow of the pulsed metal powder preparation condensing device for collection.
  • Step 4 The backflushing device in the collector 4 backflushes the metal powder into the powder collector 5 for collection.
  • the raw material is one or more metals selected from iron, nickel, copper, tin, silver, etc.
  • the obtained metal powder is one or more of iron, nickel, copper, tin, silver, etc. Metal alloy powder.
  • the metal powder is spherical, and the particle size is less than 100nm.
  • the pulse cooling chamber 3 is under negative pressure, the pressure in the reactor 1 is 70-90kPa, and the gas-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:(1500-2000), with To achieve the effect of effectively improving the distribution uniformity and yield of metal powder.
  • the pulsed metal powder preparation condensation device includes a reactor 1 , a condensation tube 2 , a pulsed cooling chamber 3 , a collector 4 and a powder collector 5 .
  • the reactor 1 is used for melting and evaporating raw materials to obtain metal vapor.
  • the condenser tube 2 is connected to the reactor 1 and the pulse cooling chamber 3, so that the metal vapor crystallizes and nucleates when passing through the condenser tube 2.
  • the powder blanks that crystallize and nucleate The spacing between particles instantly expands, greatly reducing the collision probability of each powder blank particle, thereby effectively reducing the generation of conjoined particles and slag.
  • the collector 4 is used to collect the metal powder obtained by cooling through the pulse cooling chamber 3 , and the metal powder enters the powder collector 5 under the backflushing action of the backflushing tank in the collector 4 for collection.
  • a zirconia lining layer is arranged in the condenser tube 2, and an interlayer is arranged in the condenser tube 2. There is cooling water in the interlayer.
  • the pulse cooling chamber 3 includes a dish-shaped head, a cylinder, a viewing hole and a gas distributor 6 .
  • the dish-shaped head is used for sealing connection with the condensing pipe 2 .
  • Cylinders are used for cooling and obtaining metal powders.
  • the observation hole is used to observe the formation of metal powder in the cylinder.
  • the gas distributor 6 is an annular gas distributor, and a plurality of gas nozzles with equal arc distribution are arranged on the gas distributor 6 .
  • the open end of the gas nozzle faces the center of the condenser tube 2 to effectively slow down the gas flow rate and blow out the powder blanks.
  • the cross-sectional area ratio of the condenser tube 2 and the pulse cooling chamber 3 is 1:8, and the volume ratio of the condenser tube 2 and the pulse cooling chamber 3 is 1:10, so as to greatly reduce the collision of each powder blank particle probability, thereby effectively reducing the generation of conjoined particles and slag.
  • the pulsed metal powder preparation and condensation method provided in this example uses a preparation condensation device composed of a reactor 1, a condenser tube 2, a pulsed cooling chamber 3, a collector 4 and a powder collector 5 to obtain metal by a pulsed cooling method. powder.
  • the method of pulse cooling includes the following steps:
  • Step 1 The raw materials are put into the reactor 1 to melt and evaporate, so that the metal vapor enters the condenser tube 2 for crystallization and nucleation to form powder blanks.
  • Step 2 The powder blank enters the pulse cooling chamber 3 for cooling to form single metal particles, and the pulse cooling chamber 3 is filled with nitrogen during pulse cooling.
  • Step 3 the single metal particles enter the collector 4 through the inclined pipe under the action of the air flow of the pulsed metal powder preparation condensing device for collection.
  • Step 4 The backflushing device in the collector 4 backflushes the metal powder into the powder collector 5 for collection.
  • the raw material is one or more metals selected from iron, nickel, copper, tin, silver, etc.
  • the obtained metal powder is one or more of iron, nickel, copper, tin, silver, etc. Metal alloy powder.
  • the metal powder is spherical, and the particle size is less than 100nm.
  • the pulse cooling chamber 3 is under negative pressure, the pressure in the reactor 1 is 70kPa, and the gas-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:1500, so as to effectively improve the metal powder. The effect of distribution uniformity and yield.
  • the difference between the second embodiment and the first embodiment is that the cross-sectional area ratio of the condenser tube 2 to the pulse cooling chamber 3 in the second embodiment is 1:12, and the volume ratio of the condenser tube 2 to the pulse cooling chamber 3 is 1:13.
  • the difference between the third embodiment and the first embodiment is that the cross-sectional area ratio of the condenser tube 2 to the pulse cooling chamber 3 in the third embodiment is 1:15, and the volume ratio of the condenser tube 2 to the pulse cooling chamber 3 is 1:15.
  • Example 4 The difference between Example 4 and Example 1 is that the pressure in the reactor 1 in Example 4 is 80 kPa, and the gas-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:1800.
  • Example 5 The difference between Example 5 and Example 1 is that the pressure in the reactor 1 in Example 5 is 90 kPa, and the gas-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:2000.
  • the difference between the sixth embodiment and the first embodiment is that the condensation pipe 2 and the pulse cooling chamber 3 in the sixth embodiment are both provided with an interlayer, and the interlayer has cooling water.
  • the pulse cooling chamber 3 by setting the pulse cooling chamber 3 with a large cross-sectional area, the flow rate of the gas in the tube is reduced, the flow state Reynolds number Re ⁇ 3000, and the flow state of the condensation system is excessive flow and laminar flow.
  • the pulse cooling chamber 3 By setting the pulse cooling chamber 3 with a large volume, the cooling space of the metal powder is effectively enlarged, the density of the metal powder in the pulse cooling chamber 3 is reduced, and the gap between the powder particles and between the particles and the tube wall is effectively reduced. Collision probability, to achieve the purpose of avoiding the conjoined metal particles and the generation of irregular shaped particles.
  • the pulse cooling chamber 3 With uniform temperature field distribution, metal powder with uniform particle distribution can be obtained, and the effect of less super-large and ultra-fine particles and narrow particle size distribution of the powder can be achieved.
  • the metal vapor forms less slag and less waste powder on the chamber wall, and achieves the purpose of improving the powder yield by 15%. Therefore, there is less slagging on the inner wall of the condenser pipe 2, the condenser pipe 2 is not easily blocked, and the production cycle is shortened by 20%.
  • references in this application to "first”, “second”, “third”, “fourth”, etc. are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It is to be understood that the data so used are interchangeable under appropriate circumstances so that the embodiments described herein can be practiced in sequences other than those illustrated or described herein. Furthermore, the terms “comprising” and “having”, and any variations thereof, are intended to cover non-exclusive inclusion, for example, a process, method or apparatus comprising a series of steps or elements is not necessarily limited to those steps or elements expressly listed , but may include other steps or elements not expressly listed or inherent to these processes, methods or apparatus.

Abstract

一种脉冲式金属粉制备冷凝方法，所述方法包括如下步骤：步骤1、将原料置入反应器（1）内熔融蒸发，使得金属蒸汽进入冷凝管（2）内结晶、成核，形成粉体胚料；步骤2、粉体胚料进入脉冲冷却室（3）内冷却，形成单体金属粒子，且脉冲冷却时脉冲冷却室（3）内充满氮气；步骤3、单体金属粒子在气流作用下进入收集器（4）内收集；步骤4、收集器（4）内的反吹装置将金属粉体反吹入收粉器（5）内收集。该冷凝方法具有显著提升金属粉体分布均匀度与成品率的效果。

Description

一种脉冲式金属粉制备冷凝方法 技术领域
本申请涉及粉体制备技术领域，特别涉及一种脉冲式金属粉制备冷凝方法。
背景技术
目前，在亚微米级金属粉体制备行业，多采用物理气相法生产金属镍粉。金属在反应器熔池内熔融、气化后，金属蒸汽在***氮气的作用下进入冷凝管，在冷凝管内通过氮冷却，形成粉体后进入收集罐。
但是目前的物理气相法生产金属镍粉时，金属蒸汽直接通过冷凝管冷凝，而冷凝管的内容积小，粉体在脉冲冷却室内的气固比仅为1：(200-250)，导致存在粉体浓度大、温度高以及粉体冷却不充分的问题。而且，由于冷凝管的截面积小，气体在管内流速高，流态雷诺数Re≧3000，因此***流态呈过度流和紊流状。现有的方法获得的金属镍粉因粉体过大还会导致粉体粒子之间及粒子与管壁之间碰撞机率增大，进而在高温环境下，未冷却的金属粒子之间相互熔结，易形成连体，或形成不规则的异形粒子，导致粉体品质下降。
发明内容
有鉴于此，本申请的目的在于提供一种脉冲式金属粉制备冷凝方法，以实现提升金属粉体分布均匀度与成品率的目的。其具体方案如下：
一种脉冲式金属粉制备冷凝方法，所述方法包括如下步骤：
步骤1、将原料置入反应器内熔融蒸发，使得金属蒸汽进入冷凝管内结晶、成核，形成粉体胚料；
步骤2、粉体胚料进入脉冲冷却室内冷却，形成单体金属粒子，且脉冲冷却时脉充冷却室内充满氮气；
步骤3、单体金属粒子在气流作用下进入收集器内收集；
步骤4、收集器内的反吹装置将金属粉体反吹入收粉器内收集。
可选的，所述脉冲冷却室包括碟形封头、圆柱体、观察孔和气体分布器；所述气体分布器为环形气体分布器。
可选的，所述环形气体分布器设置有多个等弧度分布的气体喷嘴，所述气体喷嘴的开口端朝向所述冷凝管的中心。
可选的，所述冷凝管与脉冲冷却室的截面积比为1：(8-15)；所述冷凝管与所述脉冲冷却室的容积比为1：(10-15)。
可选的，所述金属粉体呈球形，且粒径小于100nm。
可选的，所述脉冲冷却室内呈负压；所述反应器内的压强为70-90kPa。
可选的，所述冷凝管内设置有氧化锆内衬层。
可选的，所述金属粉体在所述脉冲冷却室内的气固比为1：(1500-2000)。
可选的，所述冷凝管和/或所述脉冲冷却室设置有夹层，所述夹层内具有冷却水。
可选的，在步骤3中，单体金属粒子通过斜管从脉冲冷却室进入收集器内。
通过以上方案可知，本申请提供了一种脉冲式金属粉制备冷凝方法，该脉冲式金属粉制备冷凝方法具有以下有益效果：
1、通过截面积大的脉冲冷却室的设置，使得气体在管内流速降低，流态雷诺数Re≤3000，冷凝***流态呈过度流和层流状。
2、通过体积大的脉冲冷却室的设置，有效扩大了金属粉体的冷却空间，降低了金属粉体在脉冲冷却室中的密度，进而有效降低粉体粒子之间及粒子与管壁之间碰撞机率，达到避免金属粒子连体及避免产生不规则异形粒子的目的。
3、通过温度场分布均匀的脉冲冷却室的设置，获得粒子分布均匀的金属粉体，实现超大与超细粒子少、粉体粒度分布窄的效果。
4、通过减小脉冲冷却室的中心部位与室壁的温差，使得金属蒸汽在室壁上形成的熔渣少，废粉少，达到提升15％的粉体成品率的目的。
5、具有冷凝管的内壁结渣现象少、冷凝管不易堵塞以及生产周期缩短20％的效果。
附图说明
为了更清楚地说明本申请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，下面描述中的附图仅仅是本申请的实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据提供的附图获得其他的附图。
图1为本公开的脉冲式金属粉制备冷凝装置的实施例的结构示意图。
附图标记说明：1、反应器；2、冷凝管；3、脉冲冷却室；4、收集器；5、收粉器；6、气体分布器。
具体实施方式
下面将结合本申请实施例中的附图，对本申请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申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，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，都属于本申请保护的范围。
以下针对本发明实施例的脉冲式金属粉制备冷凝装置进行具体说明：
如图1所示，一种脉冲式金属粉制备冷凝装置，包括反应器1、冷凝管2、脉冲冷却室3、收集器4以及收粉器5。其中，反应器1用于将原料熔融与蒸发，以获得金属蒸汽。冷凝管2连接反应器1与脉冲冷却室3，以使得金属蒸汽通过冷凝管2时结晶、成核，在进入脉冲冷却室3内后，通过减缓气体流速，致使结晶成核的粉体胚料粒子之间的间距瞬间扩大，大幅度减小各个粉体胚料粒子的碰撞几率，从而有效减少连体粒子与熔渣的产生。收集器4用于收集经由脉冲冷却室3冷却获得的金属粉体，金属粉体在收集器4内的反吹罐反吹作用下进入收粉器5内收集。为了实现冷却效果，冷凝管2内设置有氧化锆内衬层，且冷凝管2和/或脉冲冷却室3设置有夹层。夹层内具有冷却水。
需要提及的是，脉冲冷却室3包括碟形封头、圆柱体、观察孔和气体分布器6。碟形封头用于与冷凝管2密封连接。圆柱体用于金属粉体的冷却与获得。观察孔用于观察圆柱体内金属粉体的生成情况。气体分布器6为环形气体分布器，气体分布器6上设置有多个等弧度分布的气体喷嘴。气体喷嘴的开口端朝向冷凝管2的中心，以有效减缓气体流速并吹散粉体 胚料。
与此同时，冷凝管2与脉冲冷却室3的截面积比为1：(8-15)，冷凝管2与脉冲冷却室3的容积比为1：(10-15)，以大幅度减小各个粉体胚料粒子的碰撞几率，从而有效减少连体粒子与熔渣的产生。
本公开提供了一种脉冲式金属粉制备冷凝方法，通过采用由反应器1、冷凝管2、脉冲冷却室3、收集器4以及收粉器5组成的制备冷凝装置，以脉冲冷却的方法获得金属粉体。
其中：
脉冲冷却的方法包括如下步骤：
步骤1、将原料置入反应器1内熔融蒸发，使得金属蒸汽进入冷凝管2内结晶、成核，形成粉体胚料。
步骤2、粉体胚料进入脉冲冷却室3内冷却，形成单体金属粒子，且脉冲冷却时脉冲冷却室3内充满氮气。
步骤3、单体金属粒子在脉冲式金属粉制备冷凝装置的气流作用下通过斜管进入收集器4内收集。
步骤4、收集器4内的反吹装置将金属粉体反吹入收粉器5内收集。
需要提及的是，原料为铁、镍、铜、锡、银等中的一种或多种金属，获得的金属粉体为铁、镍、铜、锡、银等中的一种或多种金属形成的合金粉体。金属粉体呈球形，且粒径小于100nm。在脉冲冷却的过程中，脉冲冷却室3内呈负压，反应器1内的压强为70-90kPa，金属粉体在脉冲冷却室3内的气固比为1：(1500-2000)，以实现有效提升金属粉体分布均匀度与成品率的效果。
实施例一
如图1所示，脉冲式金属粉制备冷凝装置包括反应器1、冷凝管2、脉冲冷却室3、收集器4以及收粉器5。其中，反应器1用于将原料熔融与蒸发，以获得金属蒸汽。冷凝管2连接反应器1与脉冲冷却室3，以使得金属蒸汽通过冷凝管2时结晶、成核，在进入脉冲冷却室3内后，通过减缓气体流速，致使结晶成核的粉体胚料粒子之间的间距瞬间扩大，大幅度减小各个粉体胚料粒子的碰撞几率，从而有效减少连体粒子与熔渣的产生。 收集器4用于收集经由脉冲冷却室3冷却获得的金属粉体，金属粉体在收集器4内的反吹罐反吹作用下进入收粉器5内收集。为了实现冷却效果，冷凝管2内设置有氧化锆内衬层，且冷凝管2设置有夹层。夹层内具有冷却水。
需要提及的是，脉冲冷却室3包括碟形封头、圆柱体、观察孔和气体分布器6。碟形封头用于与冷凝管2密封连接。圆柱体用于金属粉体的冷却与获得。观察孔用于观察圆柱体内金属粉体的生成情况。气体分布器6为环形气体分布器，气体分布器6上设置有多个等弧度分布的气体喷嘴。气体喷嘴的开口端朝向冷凝管2的中心，以有效减缓气体流速并吹散粉体胚料。
与此同时，冷凝管2与脉冲冷却室3的截面积比为1：8，冷凝管2与脉冲冷却室3的容积比为1：10，以大幅度减小各个粉体胚料粒子的碰撞几率，从而有效减少连体粒子与熔渣的产生。
该实施例提供的脉冲式金属粉制备冷凝方法，通过采用由反应器1、冷凝管2、脉冲冷却室3、收集器4以及收粉器5组成的制备冷凝装置，以脉冲冷却的方法获得金属粉体。
其中：
脉冲冷却的方法包括如下步骤：
步骤1、将原料置入反应器1内熔融蒸发，使得金属蒸汽进入冷凝管2内结晶、成核，形成粉体胚料。
步骤2、粉体胚料进入脉冲冷却室3内冷却，形成单体金属粒子，且脉冲冷却时脉冲冷却室3内充满氮气。
步骤3、单体金属粒子在脉冲式金属粉制备冷凝装置的气流作用下通过斜管进入收集器4内收集。
步骤4、收集器4内的反吹装置将金属粉体反吹入收粉器5内收集。
需要提及的是，原料为铁、镍、铜、锡、银等中的一种或多种金属，获得的金属粉体为铁、镍、铜、锡、银等中的一种或多种金属形成的合金粉体。金属粉体呈球形，且粒径小于100nm。在脉冲冷却的过程中，脉冲冷却室3内呈负压，反应器1内的压强为70kPa，金属粉体在脉冲冷却室3 内的气固比为1：1500，以实现有效提升金属粉体分布均匀度与成品率的效果。
实施例二
实施例二与实施例一的区别在于，实施例二中的冷凝管2与脉冲冷却室3的截面积比为1：12，冷凝管2与脉冲冷却室3的容积比为1：13。
实施例三
实施例三与实施例一的区别在于，实施例三中的冷凝管2与脉冲冷却室3的截面积比为1：15，冷凝管2与脉冲冷却室3的容积比为1：15。
实施例四
实施例四与实施例一的区别在于，实施例四中的反应器1内压强为80kPa，金属粉体在脉冲冷却室3内的气固比为1：1800。
实施例五
实施例五与实施例一的区别在于，实施例五中的反应器1内压强为90kPa，金属粉体在脉冲冷却室3内的气固比为1：2000。
实施例六
实施例六与实施例一的区别在于，实施例六中的冷凝管2和脉冲冷却室3均设置有夹层，夹层内具有冷却水。
综上，本申请通过截面积大的脉冲冷却室3的设置，使得气体在管内流速降低，流态雷诺数Re≤3000，冷凝***流态呈过度流和层流状。通过体积大的脉冲冷却室3的设置，有效扩大了金属粉体的冷却空间，降低了金属粉体在脉冲冷却室3中的密度，进而有效降低粉体粒子之间及粒子与管壁之间碰撞机率，达到避免金属粒子连体与避免产生不规则异形粒子的目的。通过温度场分布均匀的脉冲冷却室3的设置，获得粒子分布均匀的金属粉体，实现超大与超细粒子少、粉体粒度分布窄的效果。通过减小脉冲冷却室3中心部位与室壁的温差，使得金属蒸汽在室壁上形成的熔渣少，废粉少，达到提升15％的粉体成品率的目的。因此，具有冷凝管2的内壁结渣现象少、冷凝管2不易堵塞以及生产周期缩短20％的效果。
本申请涉及的“第一”、“第二”、“第三”、“第四”等(如果存在)是用于区别类似的对象，而不必用于描述特定的顺序或先后次序。应该理 解这样使用的数据在适当情况下可以互换，以便这里描述的实施例能够以除了在这里图示或描述的内容以外的顺序实施。此外，术语“包括”和“具有”以及他们的任何变形，意图在于覆盖不排他的包含，例如，包含了一系列步骤或单元的过程、方法或设备不必限于清楚地列出的那些步骤或单元，而是可包括没有清楚地列出的或对于这些过程、方法或设备固有的其它步骤或单元。
需要说明的是，在本申请中涉及“第一”、“第二”等的描述仅用于描述目的，而不能理解为指示或暗示其相对重要性或者隐含指明所指示的技术特征的数量。由此，限定有“第一”、“第二”的特征可以明示或者隐含地包括至少一个该特征。另外，各个实施例之间的技术方案可以相互结合，但是必须是以本领域普通技术人员能够实现为基础，当技术方案的结合出现相互矛盾或无法实现时应当认为这种技术方案的结合不存在，也不在本申请要求的保护范围之内。
本文中应用了具体个例对本申请的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本申请的方法及其核心思想；同时，对于本领域的一般技术人员，依据本申请的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本申请的限制。

Claims (10)

  1. 一种脉冲式金属粉制备冷凝方法，其特征在于，所述方法包括如下步骤：
    步骤1、将原料置入反应器内熔融蒸发，使得金属蒸汽进入冷凝管内结晶、成核，形成粉体胚料；
    步骤2、粉体胚料进入脉冲冷却室内冷却，形成单体金属粒子，且脉冲冷却时脉冲冷却室内充满氮气；
    步骤3、单体金属粒子在气流作用下进入收集器内收集；
    步骤4、收集器内的反吹装置将金属粉体反吹入收粉器内收集。
  2. 根据权利要求1所述的脉冲式金属粉制备冷凝方法，其特征在于：所述脉冲冷却室包括碟形封头、圆柱体、观察孔和气体分布器，所述气体分布器为环形气体分布器。
  3. 根据权利要求1或2所述的脉冲式金属粉制备冷凝方法，其特征在于：所述环形气体分布器设置有多个等弧度分布的气体喷嘴，所述气体喷嘴的开口端朝向所述冷凝管的中心。
  4. 根据权利要求1至3中任一项所述的脉冲式金属粉制备冷凝方法，其特征在于：所述冷凝管与脉冲冷却室的截面积比为1：(8-15)，所述冷凝管与所述脉冲冷却室的容积比为1：(10-15)。
  5. 根据权利要求1至4中任一项所述的脉冲式金属粉制备冷凝方法，其特征在于：所述金属粉体呈球形，且粒径小于100nm。
  6. 根据权利要求1至5中任一项所述的脉冲式金属粉制备冷凝方法，其特征在于：所述脉冲冷却室内呈负压，所述反应器内压强为70-90kPa。
  7. 根据权利要求1至6中任一项所述的脉冲式金属粉制备冷凝方法，其特征在于：所述冷凝管内设置有氧化锆内衬层。
  8. 根据权利要求1至7中任一项所述的脉冲式金属粉制备冷凝方法，其特征在于：所述金属粉体在所述脉冲冷却室内的气固比为1：(1500-2000)。
  9. 根据权利要求1至8中任一项所述的脉冲式金属粉制备冷凝方法，其特征在于：所述冷凝管和/或所述脉冲冷却室设置有夹层，所述夹层内具有冷却水。
  10. 根据权利要求1至9中任一项所述的脉冲式金属粉制备冷凝方法，其特征在于：在步骤3中，单体金属粒子通过斜管从脉冲冷却室进入收集器内。
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