TWI813105B - Pulsed metal powder preparation and condensation method - Google Patents
Pulsed metal powder preparation and condensation method Download PDFInfo
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- TWI813105B TWI813105B TW110148449A TW110148449A TWI813105B TW I813105 B TWI813105 B TW I813105B TW 110148449 A TW110148449 A TW 110148449A TW 110148449 A TW110148449 A TW 110148449A TW I813105 B TWI813105 B TW I813105B
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- 239000000843 powder Substances 0.000 title claims abstract description 111
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 83
- 239000002184 metal Substances 0.000 title claims abstract description 83
- 238000009833 condensation Methods 0.000 title claims abstract description 56
- 230000005494 condensation Effects 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 88
- 239000002923 metal particle Substances 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000007664 blowing Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 25
- 239000011229 interlayer Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000002893 slag Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 239000011135 tin Substances 0.000 description 4
- 230000001788 irregular Effects 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- 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
Abstract
Description
本發明涉及粉末製備技術領域，特別涉及一種脈衝式金屬粉製備冷凝方法。The invention relates to the technical field of powder preparation, and in particular to a pulse type metal powder preparation and condensation method.
目前，在次微米級金屬粉末製備行業，多採用物理氣相法生產金屬鎳粉。金屬在反應器熔池內熔融、氣化後，金屬蒸汽在系統氮氣的作用下進入冷凝管，在冷凝管內通過氮冷卻，形成粉末後進入收集罐。At present, in the sub-micron metal powder preparation industry, the physical vapor 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 condensation tube under the action of system nitrogen. It is cooled by nitrogen in the condensation tube and forms powder before entering the collection tank.
但是目前的物理氣相法生產金屬鎳粉時，金屬蒸汽直接通過冷凝管冷凝，而冷凝管的內容積小，粉末在脈衝冷卻室內的氣固比僅為1：200至1：250，導致存在粉末濃度大、溫度高以及粉末冷卻不充分的問題。而且，由於冷凝管的截面積小，氣體在管內流速高，流態雷諾數Re≧3000，因此系統流態呈過度流和紊流狀。現有的方法獲得的金屬鎳粉因粉末過大還會導致粉末粒子之間及粒子與管壁之間碰撞機率增大，進而在高溫環境下，未冷卻的金屬粒子之間相互熔結，易形成連體，或形成不規則的異形粒子，導致粉末品質下降。However, when the current physical vapor phase method is used to produce metal nickel powder, the metal vapor is condensed directly through the condenser tube, and the internal volume of the condenser tube is small. The gas-to-solid ratio of the powder in the pulse cooling chamber is only 1:200 to 1:250, resulting in Problems such as high powder concentration, high temperature and insufficient powder cooling. Moreover, due to the small cross-sectional area of the condensation tube, the gas flow rate in the tube is high, and the flow Reynolds number is Re≧3000, so the system flow state is excessive flow and turbulent flow. The metal nickel powder obtained by the existing method will also increase the probability of collision between the powder particles and between the particles and the pipe wall because the powder is too large. Furthermore, in a high temperature environment, the uncooled metal particles will sinter with each other and easily form connections. bodies, or form irregular shaped particles, resulting in a decrease in powder quality.
有鑑於此，本發明的目的在於提供一種脈衝式金屬粉製備冷凝方法，以實現提升金屬粉末分佈均勻度與成品率的目的。其具體方案如下：In view of this, the object of the present invention is to provide a pulse-type metal powder preparation and condensation method to achieve the purpose of improving metal powder distribution uniformity and yield. The specific plan is as follows:
一種脈衝式金屬粉製備冷凝方法，所述方法包括如下步驟：A pulse type metal powder preparation and condensation method, the method includes the following steps:
步驟1: 將原料置入反應器內熔融蒸發，使得金屬蒸汽進入冷凝管內結晶、成核，形成粉末胚料；Step 1: Put the raw materials into the reactor to melt and evaporate, so that the metal vapor enters the condenser tube to crystallize and nucleate to form a powder blank;
步驟2: 粉末胚料進入脈衝冷卻室內冷卻，形成單體金屬粒子，且脈衝冷卻時脈充冷卻室內充滿氮氣；Step 2: The powder blank enters the pulse cooling chamber for cooling to form single metal particles, and during pulse cooling, the pulse cooling chamber is filled with nitrogen;
步驟3: 單體金屬粒子在氣流作用下進入收集器內收集；Step 3: The single metal particles enter the collector and are collected under the action of air flow;
步驟4: 收集器內的反吹裝置將金屬粉末反吹入收粉器內收集。Step 4: The backflushing device in the collector blows back the metal powder into the powder collector for collection.
可選的，所述脈衝冷卻室包括碟形封頭、圓柱體、觀察孔和氣體分佈器；所述氣體分佈器為環形氣體分佈器。Optionally, 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.
可選的，所述環形氣體分佈器設置有多個等弧度分佈的氣體噴嘴，所述氣體噴嘴的開口端朝向所述冷凝管中心。Optionally, the annular gas distributor is provided with a plurality of gas nozzles distributed in equal arcs, with the open ends of the gas nozzles facing the center of the condensation tube.
可選的，所述冷凝管與脈衝冷卻室的截面積比為1：8至1：15；所述冷凝管與所述脈衝冷卻室的容積比為1：10至1：15。Optionally, the cross-sectional area ratio of the condenser tube to the pulse cooling chamber is 1:8 to 1:15; the volume ratio of the condenser tube to the pulse cooling chamber is 1:10 to 1:15.
可選的，所述金屬粉末呈球形，且粒徑小於100nm。Optionally, the metal powder is spherical and has a particle size less than 100 nm.
可選的，所述脈衝冷卻室內呈負壓；所述反應器內的壓強為70-90kPa。Optionally, the pulse cooling chamber has a negative pressure; the pressure in the reactor is 70-90kPa.
可選的，所述冷凝管內設置有氧化鋯內襯層。Optionally, a zirconium oxide lining layer is provided inside the condensation tube.
可選的，所述金屬粉末在所述脈衝冷卻室內的氣固比為1：1500至1：2000。Optionally, the gas-to-solid ratio of the metal powder in the pulse cooling chamber is 1:1500 to 1:2000.
可選的，所述冷凝管和/或所述脈衝冷卻室設置有夾層，所述夾層內具有冷卻水。Optionally, the condensation tube and/or the pulse cooling chamber are provided with an interlayer, and the interlayer contains cooling water.
可選的，在步驟3中，單體金屬粒子通過斜管從脈衝冷卻室進入收集器內。Optionally, in step 3, the single metal particles enter the collector from the pulse cooling chamber through the inclined tube.
通過以上方案可知，本申請提供了一種脈衝式金屬粉製備冷凝方法，該脈衝式金屬粉製備冷凝方法具有以下有益效果：It can be seen from the above scheme that this application provides a pulse type metal powder preparation and condensation method. The pulse type metal powder preparation and condensation method has the following beneficial effects:
1：通過截面積大的脈衝冷卻室的設置，使得氣體在管內流速降低，流態雷諾數Re≤3000，冷凝系統流態呈過度流和層流狀。1: Through the setting of a pulse cooling chamber 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.
2：通過體積大的脈衝冷卻室的設置，有效擴大了金屬粉末的冷卻空間，降低了金屬粉末在脈衝冷卻室中的密度，進而有效降低粉末粒子之間及粒子與管壁之間碰撞機率，達到避免金屬粒子連體及避免產生不規則異形粒子的目的。2: By setting up a large pulse cooling chamber, the cooling space of the metal powder is effectively expanded, the density of the metal powder in the pulse cooling chamber is reduced, and the probability of collision between the powder particles and between the particles and the tube wall is effectively reduced. To achieve the purpose of avoiding the concatenation of metal particles and the generation of irregular shaped particles.
3：通過溫度場分佈均勻的脈衝冷卻室的設置，獲得粒子分佈均勻的金屬粉末，實現超大與超細粒子少、粉末粒度分佈窄的效果。3: By setting up a pulse cooling chamber with uniform temperature field distribution, metal powder with uniform particle distribution can be obtained, achieving the effect of fewer oversized and ultrafine particles and a narrow powder size distribution.
4：通過減小脈衝冷卻室的中心部位與室壁的溫差，使得金屬蒸汽在室壁上形成的熔渣少，廢粉少，達到提升15%的粉末成品率的目的。4: By reducing the temperature difference between the center of the pulse cooling chamber and the chamber wall, the metal vapor forms less slag and waste powder on the chamber wall, achieving the goal of increasing the powder yield by 15%.
5：具有冷凝管的內壁結渣現象少、冷凝管不易堵塞以及生產週期縮短20%的效果。5: It has the effect of less slagging on the inner wall of the condenser tube, less blockage of the condenser tube and shortening the production cycle by 20%.
下面將結合本發明實施例中的附圖，對本發明實施例中的技術方案進行清楚、完整地描述。顯然，所描述的實施例僅僅是本發明一部分實施例，而不是全部的實施例。基於本發明中的實施例，本發明所屬技術領域中具有通常知識者所作之均等變化與修飾，皆應仍屬本發明之專利涵蓋範圍內。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, equal changes and modifications made by those with ordinary skill in the technical field to which the present invention belongs should still fall within the scope of the patent of the present invention.
以下針對本發明實施例的脈衝式金屬粉製備冷凝裝置進行具體說明：The following is a detailed description of the pulse-type metal powder preparation and condensation device according to the embodiment of the present invention:
如圖1所示，一種脈衝式金屬粉製備冷凝裝置，包括反應器1、冷凝管2、脈衝冷卻室3、收集器4以及收粉器5。其中，反應器1用於將原料熔融與蒸發，以獲得金屬蒸汽。冷凝管2連接反應器1與脈衝冷卻室3，以使得金屬蒸汽通過冷凝管2時結晶、成核，在進入脈衝冷卻室3內後，通過減緩氣體流速，致使結晶成核的粉末胚料粒子之間的間距瞬間擴大，大幅度減小各個粉末胚料粒子的碰撞機率，從而有效減少連體粒子與熔渣的產生。收集器4用於收集經由脈衝冷卻室3冷卻獲得的金屬粉末，金屬粉末在收集器4內的反吹罐反吹作用下進入收粉器5內收集。為了實現冷卻效果，冷凝管2內設置有氧化鋯內襯層，且冷凝管2和/或脈衝冷卻室3設置有夾層。夾層內具有冷卻水。As shown in Figure 1, a pulse type metal powder preparation condensation device includes a reactor 1, a condensation tube 2, a pulse cooling chamber 3, a collector 4 and a powder collector 5. Among them, reactor 1 is used to melt and evaporate raw materials to obtain metal vapor. The condensation tube 2 connects the reactor 1 and the pulse cooling chamber 3, so that the metal vapor crystallizes and nucleates when passing through the condensation tube 2. After entering the pulse cooling chamber 3, the gas flow rate is slowed down, causing the crystallization and nucleation of the powder blank particles. The distance between them is instantly expanded, 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 in the pulse cooling chamber 3. The metal powder enters the powder collector 5 for collection under the backflush action of the backflush tank in the collector 4. In order to achieve the cooling effect, the condensation tube 2 is provided with a zirconia lining layer, and the condensation tube 2 and/or the pulse cooling chamber 3 are provided with an interlayer. There is cooling water in the mezzanine.
需要提及的是，脈衝冷卻室3包括碟形封頭、圓柱體、觀察孔和氣體分佈器6。碟形封頭用於與冷凝管2密封連接。圓柱體用於金屬粉末的冷卻與獲得。觀察孔用於觀察圓柱體內金屬粉末的生成情況。氣體分佈器6為環形氣體分佈器，氣體分佈器6上設置有多個等弧度分佈的氣體噴嘴。氣體噴嘴的開口端朝向冷凝管2的中心，以有效減緩氣體流速並吹散粉末胚料。It should be mentioned that the pulse cooling chamber 3 includes a dish-shaped head, a cylinder, an observation hole and a gas distributor 6. The disc-shaped head is used for sealing connection with the condenser pipe 2. The cylinder is used for cooling and obtaining metal powder. The observation hole is used to observe the generation of metal powder in the cylinder. The gas distributor 6 is an annular gas distributor, and the gas distributor 6 is provided with a plurality of gas nozzles distributed in equal arcs. 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 away the powder blank.
與此同時，冷凝管2與脈衝冷卻室3的截面積比為1：8至1：15，冷凝管2與脈衝冷卻室3的容積比為1：10至1：15，以大幅度減小各個粉末胚料粒子的碰撞機率，從而有效減少連體粒子與熔渣的產生。At the same time, the cross-sectional area ratio of the condensing tube 2 and the pulse cooling chamber 3 is 1:8 to 1:15, and the volume ratio of the condensing tube 2 and the pulse cooling chamber 3 is 1:10 to 1:15, so as to greatly reduce The collision probability of each powder blank particle effectively reduces the generation of connected particles and slag.
本發明提供了一種脈衝式金屬粉製備冷凝方法，通過採用由反應器1、冷凝管2、脈衝冷卻室3、收集器4以及收粉器5組成的製備冷凝裝置，以脈衝冷卻的方法獲得金屬粉末。其中：脈衝冷卻的方法包括如下步驟：The invention provides a pulse type metal powder preparation and condensation method. By using a preparation and condensation device composed of a reactor 1, a condensation tube 2, a pulse cooling chamber 3, a collector 4 and a powder collector 5, the metal is obtained by pulse cooling. powder. Among them: the pulse cooling method includes the following steps:
步驟1： 將原料置入反應器1內熔融蒸發，使得金屬蒸汽進入冷凝管2內結晶、成核，形成粉末胚料。Step 1: Put the raw materials into the reactor 1 to melt and evaporate, so that the metal vapor enters the condenser tube 2 to crystallize and nucleate to form a powder blank.
步驟2：粉末胚料進入脈衝冷卻室3內冷卻，形成單體金屬粒子，且脈衝冷卻時脈衝冷卻室3內充滿氮氣。Step 2: The powder blank enters the pulse cooling chamber 3 for cooling to form single metal particles, and during pulse cooling, the pulse cooling chamber 3 is filled with nitrogen.
步驟3: ：單體金屬粒子在脈衝式金屬粉製備冷凝裝置的氣流作用下通過斜管進入收集器4內收集。Step 3:: The single metal particles enter the collector 4 through the inclined tube and are collected under the action of the air flow of the pulse metal powder preparation condensation device.
步驟4：收集器4內的反吹裝置將金屬粉末反吹入收粉器5內收集。Step 4: The backflushing device in the collector 4 backflushes the metal powder into the powder collector 5 for collection.
需要提及的是，原料為鐵、鎳、銅、錫、銀等中的一種或多種金屬，獲得的金屬粉末為鐵、鎳、銅、錫、銀等中的一種或多種金屬形成的合金粉末。金屬粉末呈球形，且粒徑小於100nm。在脈衝冷卻的過程中，脈衝冷卻室3內呈負壓，反應器1內的壓強為70-90kPa，金屬粉末在脈衝冷卻室3內的氣固比為1：1500至1：2000，以實現有效提升金屬粉末分佈均勻度與成品率的效果。It should be mentioned that the raw material is one or more metals among iron, nickel, copper, tin, silver, etc., and the metal powder obtained is an alloy powder formed from one or more metals among iron, nickel, copper, tin, silver, etc. . The metal powder is spherical and the particle size is less than 100nm. During the pulse cooling process, there is a negative pressure in the pulse cooling chamber 3, the pressure in the reactor 1 is 70-90kPa, and the gas-to-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:1500 to 1:2000 to achieve Effectively improve the uniformity of metal powder distribution and yield.
實施例一Embodiment 1
如圖1所示，脈衝式金屬粉製備冷凝裝置包括反應器1、冷凝管2、脈衝冷卻室3、收集器4以及收粉器5。其中，反應器1用於將原料熔融與蒸發，以獲得金屬蒸汽。冷凝管2連接反應器1與脈衝冷卻室3，以使得金屬蒸汽通過冷凝管2時結晶、成核，在進入脈衝冷卻室3內後，通過減緩氣體流速，致使結晶成核的粉末胚料粒子之間的間距瞬間擴大，大幅度減小各個粉末胚料粒子的碰撞機率，從而有效減少連體粒子與熔渣的產生。收集器4用於收集經由脈衝冷卻室3冷卻獲得的金屬粉末，金屬粉末在收集器4內的反吹罐反吹作用下進入收粉器5內收集。為了實現冷卻效果，冷凝管2內設置有氧化鋯內襯層，且冷凝管2設置有夾層。夾層內具有冷卻水。As shown in Figure 1, the pulse metal powder preparation condensation device includes a reactor 1, a condensation tube 2, a pulse cooling chamber 3, a collector 4 and a powder collector 5. Among them, reactor 1 is used to melt and evaporate raw materials to obtain metal vapor. The condensation tube 2 connects the reactor 1 and the pulse cooling chamber 3, so that the metal vapor crystallizes and nucleates when passing through the condensation tube 2. After entering the pulse cooling chamber 3, the gas flow rate is slowed down, causing the crystallization and nucleation of the powder blank particles. The distance between them is instantly expanded, 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 in the pulse cooling chamber 3. The metal powder enters the powder collector 5 for collection under the backflush action of the backflush tank in the collector 4. In order to achieve the cooling effect, the condensation tube 2 is provided with a zirconia lining layer, and the condensation tube 2 is provided with an interlayer. There is cooling water in the mezzanine.
需要提及的是，脈衝冷卻室3包括碟形封頭、圓柱體、觀察孔和氣體分佈器6。碟形封頭用於與冷凝管2密封連接。圓柱體用於金屬粉末的冷卻與獲得。觀察孔用於觀察圓柱體內金屬粉末的生成情況。氣體分佈器6為環形氣體分佈器，氣體分佈器6上設置有多個等弧度分佈的氣體噴嘴。氣體噴嘴的開口端朝向冷凝管2的中心，以有效減緩氣體流速並吹散粉末胚料。It should be mentioned that the pulse cooling chamber 3 includes a dish-shaped head, a cylinder, an observation hole and a gas distributor 6. The disc-shaped head is used for sealing connection with the condenser pipe 2. The cylinder is used for cooling and obtaining metal powder. The observation hole is used to observe the generation of metal powder in the cylinder. The gas distributor 6 is an annular gas distributor, and the gas distributor 6 is provided with a plurality of gas nozzles distributed in equal arcs. 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 away the powder blank.
與此同時，冷凝管2與脈衝冷卻室3的截面積比為1：8，冷凝管2與脈衝冷卻室3的容積比為1：10，以大幅度減小各個粉末胚料粒子的碰撞機率，從而有效減少連體粒子與熔渣的產生。At the same time, 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 probability of each powder blank particle. , thereby effectively reducing the generation of conjoined particles and slag.
該實施例提供的脈衝式金屬粉製備冷凝方法，通過採用由反應器1、冷凝管2、脈衝冷卻室3、收集器4以及收粉器5組成的製備冷凝裝置，以脈衝冷卻的方法獲得金屬粉末。The pulse metal powder preparation and condensation method provided in this embodiment uses a preparation and condensation device composed of a reactor 1, a condenser tube 2, a pulse cooling chamber 3, a collector 4 and a powder collector 5 to obtain metal by pulse cooling. powder.
其中，脈衝冷卻的方法包括如下步驟：Among them, the pulse cooling method includes the following steps:
步驟1: 將原料置入反應器1內熔融蒸發，使得金屬蒸汽進入冷凝管2內結晶、成核，形成粉末胚料。Step 1: Put the raw materials into the reactor 1 to melt and evaporate, so that the metal vapor enters the condenser tube 2 to crystallize and nucleate to form a powder blank.
步驟2: 粉末胚料進入脈衝冷卻室3內冷卻，形成單體金屬粒子，且脈衝冷卻時脈衝冷卻室3內充滿氮氣。Step 2: The powder blank enters the pulse cooling chamber 3 and is cooled to form single metal particles. During pulse cooling, the pulse cooling chamber 3 is filled with nitrogen.
步驟3: 單體金屬粒子在脈衝式金屬粉製備冷凝裝置的氣流作用下通過斜管進入收集器4內收集。Step 3: The single metal particles enter the collector 4 through the inclined tube under the action of the air flow of the pulsed metal powder preparation condensation device and are collected.
步驟4: 收集器4內的反吹裝置將金屬粉末反吹入收粉器5內收集。Step 4: The backflushing device in the collector 4 backflushes the metal powder into the powder collector 5 for collection.
需要提及的是，原料為鐵、鎳、銅、錫、銀等中的一種或多種金屬，獲得的金屬粉末為鐵、鎳、銅、錫、銀等中的一種或多種金屬形成的合金粉末。金屬粉末呈球形，且粒徑小於100nm。在脈衝冷卻的過程中，脈衝冷卻室3內呈負壓，反應器1內的壓強為70kPa，金屬粉末在脈衝冷卻室3內的氣固比為1：1500，以實現有效提升金屬粉末分佈均勻度與成品率的效果。It should be mentioned that the raw material is one or more metals among iron, nickel, copper, tin, silver, etc., and the metal powder obtained is an alloy powder formed from one or more metals among iron, nickel, copper, tin, silver, etc. . The metal powder is spherical and the particle size is less than 100nm. During the pulse cooling process, there is a negative pressure in the pulse cooling chamber 3, the pressure in the reactor 1 is 70kPa, and the gas-to-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:1500 to effectively improve the uniform distribution of the metal powder. efficiency and yield.
實施例二Embodiment 2
實施例二與實施例一的區別在於，實施例二中的冷凝管2與脈衝冷卻室3的截面積比為1：12，冷凝管2與脈衝冷卻室3的容積比為1：13。The difference between the second embodiment and the first embodiment is that in the second embodiment, the cross-sectional area ratio of the condensation tube 2 and the pulse cooling chamber 3 is 1:12, and the volume ratio of the condensation tube 2 and the pulse cooling chamber 3 is 1:13.
實施例三Embodiment 3
實施例三與實施例一的區別在於，實施例三中的冷凝管2與脈衝冷卻室3的截面積比為1：15，冷凝管2與脈衝冷卻室3的容積比為1：15。The difference between the third embodiment and the first embodiment is that the cross-sectional area ratio of the condensation tube 2 and the pulse cooling chamber 3 in the third embodiment is 1:15, and the volume ratio of the condensation tube 2 and the pulse cooling chamber 3 is 1:15.
實施例四Embodiment 4
實施例四與實施例一的區別在於，實施例四中的反應器1內壓強為80kPa，金屬粉末在脈衝冷卻室3內的氣固比為1：1800。The difference between Embodiment 4 and Embodiment 1 is that the pressure in reactor 1 in Embodiment 4 is 80 kPa, and the gas-to-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:1800.
實施例五Embodiment 5
實施例五與實施例一的區別在於，實施例五中的反應器1內壓強為90kPa，金屬粉末在脈衝冷卻室3內的氣固比為1：2000。The difference between Embodiment 5 and Embodiment 1 is that the pressure in reactor 1 in Embodiment 5 is 90 kPa, and the gas-to-solid ratio of the metal powder in the pulse cooling chamber 3 is 1:2000.
實施例六Embodiment 6
實施例六與實施例一的區別在於，實施例六中的冷凝管2和脈衝冷卻室3均設置有夾層，夾層內具有冷卻水。The difference between Embodiment 6 and Embodiment 1 is that in Embodiment 6, both the condensation tube 2 and the pulse cooling chamber 3 are provided with interlayers, and the interlayers contain cooling water.
綜上，本申請通過截面積大的脈衝冷卻室3的設置，使得氣體在管內流速降低，流態雷諾數Re≤3000，冷凝系統流態呈過度流和層流狀。通過體積大的脈衝冷卻室3的設置，有效擴大了金屬粉末的冷卻空間，降低了金屬粉末在脈衝冷卻室3中的密度，進而有效降低粉末粒子之間及粒子與管壁之間碰撞機率，達到避免金屬粒子連體與避免產生不規則異形粒子的目的。通過溫度場分佈均勻的脈衝冷卻室3的設置，獲得粒子分佈均勻的金屬粉末，實現超大與超細粒子少、粉末粒度分佈窄的效果。通過減小脈衝冷卻室3中心部位與室壁的溫差，使得金屬蒸汽在室壁上形成的熔渣少，廢粉少，達到提升15%的粉末成品率的目的。因此，具有冷凝管2的內壁結渣現象少、冷凝管2不易堵塞以及生產週期縮短20%的效果。To sum up, in this application, by setting up 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. Through the setting of the large pulse cooling chamber 3, the cooling space of the metal powder is effectively expanded, the density of the metal powder in the pulse cooling chamber 3 is reduced, and the probability of collision between the powder particles and between the particles and the tube wall is effectively reduced. This achieves the purpose of avoiding the concatenation of metal particles and the generation of irregular shaped particles. By setting up the pulse cooling chamber 3 with uniform temperature field distribution, metal powder with uniform particle distribution is obtained, achieving the effect of having fewer oversized and ultrafine particles and a narrow powder size distribution. By reducing the temperature difference between the center of the pulse cooling chamber 3 and the chamber wall, the metal vapor forms less slag and waste powder on the chamber wall, thereby achieving the purpose of increasing the powder yield by 15%. Therefore, there is less slagging on the inner wall of the condensation pipe 2, the condensation pipe 2 is less likely to be clogged, and the production cycle is shortened by 20%.
本發明涉及的「第一」、 「第二」、「第三」、「第四」等(如果存在)是用於區別類似的對象，而不必用於描述特定的順序或先後次序。應該理解這樣使用的數據在適當情況下可以互換，以便這裡描述的實施例能夠以除了在這裡圖示或描述的內容以外的順序實施。此外，術語「包括」和「具有」以及他們的任何變形，意圖在於覆蓋不排他的包含，例如，包含了一系列步驟或單元的過程、方法或設備不必限於清楚地列出的那些步驟或單元，而是可包括沒有清楚地列出的或對於這些過程、方法或設備固有的其它步驟或單元。"First", "second", "third", "fourth", etc. (if present) mentioned in the present invention 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 "include" and "have" and any variations thereof are intended to cover non-exclusive inclusions, e.g., a process, method or apparatus that includes a series of steps or units need not be limited to those steps or units expressly listed , but may include other steps or elements not expressly listed or inherent to such processes, methods or apparatuses.
需要說明的是，在本申請中涉及「第一」、「第二」等的描述僅用於描述目的，而不能理解為指示或暗示其相對重要性或者隱含指明所指示的技術特徵的數量。由此，限定有「第一」、「第二」的特徵可以明示或者隱含地包括至少一個該特徵。另外，各個實施例之間的技術方案可以相互結合，但是必須是以本發明所屬技術領域中具有通常知識者能夠實現為基礎，當技術方案的結合出現相互矛盾或無法實現時應當認為這種技術方案的結合不存在，也不在本申請要求的保護範圍之內。It should be noted that the descriptions involving "first", "second", etc. in this application are only for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of indicated technical features. . Therefore, features defined as "first" and "second" may explicitly or implicitly include at least one of these features. In addition, the technical solutions in the various embodiments can be combined with each other, but it must be based on the fact that a person with ordinary knowledge in the technical field to which the invention belongs can realize it. When the combination of technical solutions is contradictory or cannot be realized, it should be considered that this technology The combination of solutions does not exist and is not within the protection scope claimed by this application.
本文中應用了具體個例對本申請的原理及實施方式進行了闡述，以上實施例的說明只是用於幫助理解本發明的方法及其核心思想；同時，對於本發明所屬技術領域中具有通常知識者，依據本發明的思想，在具體實施方式及應用範圍上均會有改變之處，綜上所述，本說明書內容不應理解為對本發明的限制。This article uses specific examples to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method and the core idea of the present invention; at the same time, for those with ordinary knowledge in the technical field to which the present invention belongs , according to the idea of the present invention, there will be changes in the specific implementation mode and application scope. In summary, the content of this description should not be understood as a limitation of the present invention.
1:反應器 2:冷凝管 3:脈衝冷卻室 4:收集器 5:收粉器 6:氣體分佈器 1:Reactor 2: Condenser tube 3: Pulse cooling chamber 4: Collector 5: Powder collector 6:Gas distributor
為了更清楚地說明本發明實施例或現有技術中的技術方案，下面將對實施例或現有技術描述中所需要使用的附圖作簡單地介紹；顯而易見地，下面描述中的附圖僅僅是本申請的實施例，對於本領域普通技術人員來講，在不付出創造性勞動的前提下，還可以根據提供的附圖獲得其他的附圖。In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below; obviously, the drawings in the following description are only for the purpose of explaining the embodiments of the present invention or the technical solutions in the prior art. For the embodiments of the application, those of ordinary skill in the art can also obtain other drawings based on the provided drawings without exerting creative efforts.
圖1為本發明的脈衝式金屬粉製備冷凝裝置的實施例的結構示意圖。Figure 1 is a schematic structural diagram of an embodiment of a pulse-type metal powder preparation and condensation device of the present invention.
無。without.
1:反應器 1:Reactor
2:冷凝管 2: Condenser tube
3:脈衝冷卻室 3: Pulse cooling chamber
4:收集器 4: Collector
5:收粉器 5: Powder collector
6:氣體分佈器 6:Gas distributor
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