CN104475746B - Prepare the rotating centrifugal atomization process and device of beryllium and beryllium alloy bead - Google Patents

Prepare the rotating centrifugal atomization process and device of beryllium and beryllium alloy bead Download PDF

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CN104475746B
CN104475746B CN201410686750.9A CN201410686750A CN104475746B CN 104475746 B CN104475746 B CN 104475746B CN 201410686750 A CN201410686750 A CN 201410686750A CN 104475746 B CN104475746 B CN 104475746B
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beryllium
melting furnace
centrifugal
bead
shaft support
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CN104475746A (en
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张建利
罗天勇
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Abstract

A kind of rotating centrifugal atomization process and device for being used to prepare beryllium and beryllium alloy microballoon, beryllium and beryllium alloy bead prepared by the technique can be used for 3D printing increasing material manufacturing beryllium metal parts and nuclear energy special dimension.The technique is initially formed the liquid beryllium metal of melting; secondly liquid beryllium metal is drained on the trapezoidal inclined plane of the axle support of rotation at a high speed; liquid beryllium metal is got rid of into beryllium drop of uniform size by the centrifugal force produced using high speed rotation; then beryllium drop forms spherical in the presence of surface tension, further under inert gas shielding cooled and solidified into the beryllium bead with high sphericity, sphere diameter size uniform.The technique is compared to melting gas atomization, and the beryllium bead sphericity of preparation is high, sphere diameter uniform, controllable;Compared to the rotating electrode atomized technique of plasma asistance, due to without preparing beryllium electrode using heat and other static pressuring processes, reducing technological process link, reducing the production cost of beryllium bead.

Description

Prepare the rotating centrifugal atomization process and device of beryllium and beryllium alloy bead
Technical field
The invention belongs to field of powder metallurgy, 3D printing increases material manufacturing technology field and nuclear energy technology field, specifically relate to And a kind of rotation prepared for the 3D printing increasing material manufacturing shaping of beryllium and the beryllium bead with high sphericity of nuclear energy technology Centrifugal atomizing technique.
Background technology
Beryllium is indispensable valuable materials in atomic energy, rocket, guided missile, aviation, space travel and metallurgical industry.X Ray has very strong transmission ability to beryllium, therefore beryllium is to manufacture the material that X-ray tube wicket is not replaced.Beryllium by neutron, Particle, deuteron and gamma-rays hit or can produce neutron when irradiating, therefore beryllium is a kind of neutron source material again.Beryllium is due to atomic number Number is low, by the scattering process with neutron can slowing down and reflected neutron well, so beryllium is in some core nuclear reactors It is a kind of excellent moderator and reflector material.Other beryllium is all lighter than conventional aluminium and titanium, and specific strength is four times of steel, heat absorption Ability is strong, and thermal conductivity is high, stable mechanical performance, while can be used for manufacturing the structural material of rocket and satellite.
But the processing and manufacturing of beryllium part is extremely difficult, it is impossible to by the way of traditional forging machine adds, mainly adopt at present Beryllium part is processed with heat and other static pressuring processes, but heat and other static pressuring processes are high to equipment requirement, very flexible, high processing costs.With The rise of 3D printing increases material manufacturing technology, laser solid forming technology is expected to the processing applied to beryllium part, but the technology is needed The beryllium bead of sphericity height, good fluidity, sphere diameter below 200 microns is wanted as raw material.Meanwhile, with international magnetic confinement fusion The development of technology, the solid-state multiplication agent tritium proliferation experiment that China develops autonomous Design of being participated in the experiment on International Thermal-Nuclear Experimental Reactor Cladding modular.And this module is also required to the beryllium bead of sphericity height, good fluidity, sphere diameter in 1mm or so uniform, controllables.
Preparing the technique of beryllium bead at present mainly has two kinds, and a kind of is the method for aerosolization, that is, utilizes high pressure inert air-flow The molten metal stream of beryllium is dispelled, vaporific subsphaeroidal beryllium drop is formed in the presence of surface tension, is cooled into gas The characteristics of beryllium bead, this method is that cost is low, but sphericity is poor, and sphere diameter is uneven.
Another method is plasma asistance electric rotating machine centrifugal atomization, i.e., beryllium is first processed into beryllium electrode bar, with tungsten By high-voltage power formation plasma between electrode, the top of beryllium electrode is melted, while rotation beryllium electrode at a high speed, will be melted Liquid beryllium throw away, form vaporific spherical droplets, cooling in an inert atmosphere obtains that sphericity is high, the uniform beryllium of sphere diameter is small Ball.Although it is uniform that this method prepares beryllium bead sphericity height, sphere diameter, need first to prepare beryllium electrode using heat and other static pressuring processes Rod, i.e., the large ball diameter beryllium pearl first obtained magnesiothermic reduction smashes to form irregular beryllium powder with high pressure draught impact, then by beryllium Powder is encapsulated in involucrum using vacuum electron beam welding, then prepares beryllium rod using HTHP using hot isostatic press, whole Individual technique is related to multiple technical requirements and equipment cost very high link, therefore to prepare cost higher for beryllium bead, not Applied using the scale market of beryllium.
For this problem, we combine plasma asistance rotation electrode centrifugal atomizing technique and melting gas atomization The characteristics of a kind of new technology of rotating centrifugal atomization is have developed to prepare sphericity height, sphere diameter uniform, controllable, 3D can be met Print the beryllium bead of increasing material manufacturing and fusion nuclear energy application demand and relative inexpensiveness.
The content of the invention
The invention belongs to field of powder metallurgy, 3D printing increases material manufacturing technology field and nuclear energy technology field, specifically relate to And a kind of 3D printing increasing material manufacturing shaping prepared for beryllium and nuclear energy field specific use have high sphericity, the sphere diameter equal The rotating centrifugal atomization process of even controllable and relative inexpensiveness beryllium bead.
To achieve the above objectives, the present invention proposes a kind of method that rotating centrifugal atomization prepares beryllium and beryllium alloy bead, This method is realized in accordance with the following steps:It is initially formed the liquid beryllium metal of melting;Then liquid beryllium metal is drained into and revolved at a high speed On the trapezoidal inclined plane of the axle support turned, rotate the centrifugal force produced using high speed and liquid beryllium metal is got rid of into beryllium liquid of uniform size Drop, beryllium drop forms spherical in the presence of surface tension;The last cooled and solidified under inert gas shielding is into high spherical Degree, the beryllium bead of sphere diameter size uniform.
Beryllium the small ball's diameter is controlled by the rotating speed of axle support, and the rotating speed of axle support is controlled at 8000-10000 revs/min;It is described lazy Property protective gas be no more than 10Mpa from helium of the purity more than 99% and helium pressure.
The beryllium alloy, including Be12M and Be17M5, the M be Ti, W, V, Ta, Zr metals, M element is in beryllium alloy Atomic percent is in 5%-30%;Got the raw materials ready according to the mass ratio of the beryllium of beryllium alloy and M element, liquid beryllium is obtained in melting stove heat Alloy.
The device of above-mentioned technique is realized, the device is by magnesiothermic reduction stove or beryllium and beryllium alloy melting furnace, inert gas shielding Closed container chamber and the liquid metal flowed out from melting furnace by rotary centrifugal force is got rid of into beryllium drop of uniform size Centrifugal shaft support is constituted, and the melting furnace is located at the top of the closed container chamber, and the centrifugal shaft support passes through the melting furnace, The centrifugal shaft support upper end is connected with motor driven systems, and the centrifugal shaft support lower end is formed with trapezoidal inclined plane and positioned at described closed In container chamber, the melting furnace lower end, which is provided with, to be located at the closed container by the drainage mouth and drainage mouth of Valve controlling In chamber;The air inlet and inertia that inertia protection gas is formed with the closed container chamber protect the gas outlet of gas.
The furnace chamber of the melting furnace is cylinder shape.
The centrifugal shaft support is connected by a rotating centrifugal axle through the melting furnace inner cylinder ring with motor bearings;From There is heat-barrier coating between heart axle and melting furnace;Centrifugal shaft support is made up of resistant to elevated temperatures tantalum alloy;Centrifugal shaft support is circular cone stage body Configuration, the trapezoidal inclined plane of the frustum of a cone is less than or equal to 45 degree with the angle of table top normal.
Beneficial effects of the present invention are:(1) compared to melting gas atomization, the beryllium bead sphericity of preparation is high, and sphere diameter is equal It is even controllable;(2) the rotating electrode atomized technique of plasma asistance is compared, due to beryllium electrode need not be prepared using heat and other static pressuring processes, Reduce the production cost of beryllium bead.
Brief description of the drawings
Fig. 1 is rotating centrifugal atomization process installation drawing.Figure number explanation:1 rotating centrifugal axle support;2 magnesiothermic reduction stoves or beryllium and Beryllium alloy melting furnace;3 carry the drainage mouth of Valve controlling;The sealing container chamber of 4 inert gas shieldings;5 inertia protection gas Air inlet;6 inertia protect the gas outlet of gas;The electric system of 7 driving rotating centrifugal axle supports.
Embodiment
Present invention process comprises the following steps:
(1) this method is initially formed the liquid beryllium metal of melting, and secondly liquid beryllium metal is drained into the axle of rotation at a high speed On the trapezoidal inclined plane of support, rotate the centrifugal force produced using high speed and liquid beryllium metal is got rid of into beryllium drop of uniform size, then Beryllium drop forms spherical in the presence of surface tension, is further frozen under the cooling of protective gas with high spherical Degree, the beryllium bead of sphere diameter size uniform.
(2) this method needs to be achieved by a set of rotating centrifugal atomising device, and the device is by rotating centrifugal axle Support, the closed container chamber of inert gas shielding, beryllium metal melting furnaces, motor driven systems, beryllium guard system etc. are constituted.
The wherein furnace chamber of smelting furnace is cylinder shape, and lower end is provided with can be by the drainage mouth of Valve controlling;
Rotating centrifugal axle support is connected by a rotating centrifugal axle through vacuum melting furnace inner cylinder ring with motor bearings;
There is heat-barrier coating between rotating centrifugal axle and melting furnace;
Rotating centrifugal axle support is made up of resistant to elevated temperatures tantalum alloy;
Rotating centrifugal axle support is circular cone stage body configuration, and the trapezoidal inclined plane of the frustum of a cone is less than or equal to 45 with the angle of table top normal Degree;
(3) this method can directly obtain the liquid metal of beryllium by magnesium reduction process, and original magnesium reduction process is mutually fitted It is beryllium fluoride (BeF that the melting furnace answered, which transform raw material in cylinder shape, preparation process as,2) and magnesium metal, utilize BeF2+Mg→Be+ MgF2Reaction is directly to the liquid metal beryllium of melting;
(4) this method also can obtain liquid beryllium metal by heating existing beryllium pearl or other beryllium raw material to fusing point Stream.
(5) the liquid metal beryllium melted in this method enters inert gas shielding by the drainage mouth of melting furnace lower end Sealing container chamber, falls on the trapezoidal inclined plane of rotating centrifugal axle support;The axle support of rotation is by the liquid on its trapezoidal inclined plane at a high speed Metallic beryllium is thrown away, and liquid metal beryllium forms spherical beryllium drop in the presence of surface tension, and beryllium drop is in inert gas shielding Quick cooled and solidified in dropping process in sealing container chamber, forms beryllium bead, in the bottom collection of vacuum chamber.
(6) inert protective gas selects the high-purity helium with higher heat-conductivity, to improve cooling effect, can increase Helium pressure but no more than 10Mpa.
(7) the main rotating speed by axle support of the sphere diameter of beryllium bead is controlled, and rotating speed is at 2000 revs/min -10000 revs/min Between.
This method can also be used for preparing beryllium alloy, including Be12M and Be17M5(M is Ti, W, V, Ta, the metal, M element such as Zr Atomic percent in beryllium alloy is in 5%-30%);Got the raw materials ready according to the mass ratio of the beryllium of beryllium alloy and M element, in melting furnace Heating obtains liquid beryllium alloy.
Embodiment 1. is prepared for nuclear reactor neutron multiplication and slowing down and reflection using rotating centrifugal atomization process The diameter of effect about 1mm high sphericity beryllium bead, can be according to the following steps:
(1) build a set of rotating centrifugal atomising device, the device by rotating centrifugal axle support, inert gas shielding it is closed Container chamber, beryllium metal melting furnaces, motor driven systems, beryllium guard system etc. are constituted.
The wherein furnace chamber of smelting furnace is cylinder shape, and lower end is provided with can be by the drainage mouth of Valve controlling;
Rotating centrifugal axle support is connected by a rotating centrifugal axle through vacuum melting furnace inner cylinder ring with motor bearings;
There is heat-barrier coating between rotating centrifugal axle and melting furnace;
Rotating centrifugal axle support is made up of resistant to elevated temperatures tantalum alloy;
Rotating centrifugal axle support is circular cone stage body configuration, and the trapezoidal inclined plane of the frustum of a cone is equal to 45 degree with the angle of table top normal, Upper table surface is 60mm, following table diameter 90mm with centrifugation shaft diameter;
(2) existing beryllium pearl is put into beryllium metal melting furnaces, is heated to more than 1300 degree, obtain liquid beryllium metal Stream.
(3) valve of drainage mouth is opened, the liquid metal beryllium of melting enters indifferent gas by the drainage mouth of melting furnace lower end The sealing container chamber of body protection, falls on the trapezoidal inclined plane of rotating centrifugal axle support;The axle support of rotation is by its trapezoidal inclined plane at a high speed On liquid metal beryllium throw away, liquid metal beryllium forms spherical beryllium drop in the presence of surface tension, and beryllium drop is in indifferent gas Quick cooled and solidified in dropping process, forms beryllium bead, in the bottom collection of vacuum chamber in the sealing container chamber of body protection.
(4) inert protective gas selects helium of the purity more than 99%.
(5) the main rotating speed by axle support of the sphere diameter of beryllium bead is controlled, and rotating speed is controlled at 3000 revs/min.
2. the high sphericity that beryllium part is shaped for 3D printing increasing material manufacturing, sphere diameter are prepared using rotating centrifugal atomization process Beryllium bead below 200 microns, can be according to the following steps:
(1) build a set of rotating centrifugal atomising device, the device by rotating centrifugal axle support, inert gas shielding it is closed Container chamber, magnesiothermic reduction stove, motor driven systems, beryllium guard system etc. are constituted.
The wherein furnace chamber of magnesiothermic reduction stove is cylinder shape, and lower end is provided with can be by the drainage mouth of Valve controlling;
Rotating centrifugal axle support is connected by a rotating centrifugal axle through magnesiothermic reduction stove inner cylinder ring with motor bearings;
Rotating centrifugal axle and do not have between thermal reduction furnace and have heat-barrier coating;
Rotating centrifugal axle support is made up of resistant to elevated temperatures tantalum alloy;
Rotating centrifugal axle support is circular cone stage body configuration, and the trapezoidal inclined plane of the frustum of a cone is equal to 45 degree with the angle of table top normal, Upper table surface is 60mm, following table diameter 90mm with centrifugation shaft diameter;
(2) by beryllium fluoride (BeF2) and magnesium metal be dosed into the magnesiothermic reduction stove of transformation, utilize BeF2+Mg→Be+MgF2 Reaction is directly to the liquid metal beryllium of melting.
(3) valve of drainage mouth is opened, the liquid metal beryllium of melting enters inert gas by the drainage mouth of furnace chamber lower end The sealing container chamber of protection, falls on the trapezoidal inclined plane of rotating centrifugal axle support;The axle support of rotation is by its trapezoidal inclined plane at a high speed Liquid metal beryllium throw away, liquid metal beryllium forms spherical beryllium drop in the presence of surface tension, and beryllium drop is in inert gas Quick cooled and solidified in dropping process in the sealing container chamber of protection, forms beryllium bead, in the bottom collection of vacuum chamber.
(4) inert protective gas selects helium of the purity more than 99%.
(5) the main rotating speed by axle support of the sphere diameter of beryllium bead is controlled, and rotating speed is controlled at 8000-10000 revs/min.

Claims (3)

1. the device of the rotating centrifugal atomization process for preparing beryllium and beryllium alloy microballoon, it is characterized in that the device is by magnesiothermic reduction Stove or beryllium and beryllium alloy melting furnace(2), inert gas shielding closed container chamber(4)And will be from melting furnace(2)Outflow Liquid metal gets rid of into beryllium drop centrifugal shaft support of uniform size by rotary centrifugal force(1)Constitute, the melting furnace(2)Positioned at institute State closed container chamber(4)Top, the centrifugal shaft support(1)Through the melting furnace(2), the centrifugal shaft support(1)Upper end With motor driven systems(7)Connection, the centrifugal shaft support(1)Lower end is formed with trapezoidal inclined plane and positioned at the closed container chamber (4)It is interior, the melting furnace(2)Lower end is provided with can be by the drainage mouth of Valve controlling(3)And drainage mouth(3)Positioned at described closed Container chamber(4)It is interior;The closed container chamber(4)The air inlet that inertia protects gas is formed with interior(5)Gas is protected with inertia Gas outlet(6).
2. device according to claim 1, it is characterized in that the melting furnace(2)Furnace chamber be cylinder shape.
3. device according to claim 1, it is characterized in that the centrifugal shaft support(1)Run through the melting furnace by one (2)The rotating centrifugal axle of inner cylinder ring is connected with motor bearings;Centrifugal shaft support(1)And melting furnace(2)Between have heat-barrier coating;From Heart axle support(1)It is made up of resistant to elevated temperatures tantalum alloy;Centrifugal shaft support(1)For circular cone stage body configuration, the trapezoidal inclined plane and platform of the frustum of a cone The angle of face normal is less than or equal to 45 degree.
CN201410686750.9A 2014-11-25 2014-11-25 Prepare the rotating centrifugal atomization process and device of beryllium and beryllium alloy bead Active CN104475746B (en)

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CN111283209A (en) * 2019-12-24 2020-06-16 南京超旭节能科技有限公司 Processing method for catalyst alloy
CN111531180B (en) * 2020-05-21 2021-06-29 西藏智材新材料有限公司 Metallic beryllium powder for 3D printing and preparation method and application thereof
CN111570813B (en) * 2020-05-29 2021-11-19 西藏智材新材料有限公司 Beryllium-aluminum alloy powder and preparation method and application thereof
CN111778412B (en) * 2020-07-13 2024-07-05 苏州金江电子科技有限公司 Centrifugal remelting in-situ solidification device
CN112345420A (en) * 2020-11-09 2021-02-09 中北大学 Device and method for testing particle size and particle size distribution of liquid drops in rotating packed bed
CN113649574B (en) * 2021-08-15 2022-07-15 中南大学 Method for improving dimensional stability of high-purity beryllium material for precision instruments and meters
CN114769606B (en) * 2022-06-22 2022-10-18 中国科学院近代物理研究所 Method for preparing beryllium-titanium alloy pellets based on plasma rotating electrode

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