CN110899706A - Beryllium rod and preparation method thereof - Google Patents

Beryllium rod and preparation method thereof Download PDF

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Publication number
CN110899706A
CN110899706A CN201911034559.5A CN201911034559A CN110899706A CN 110899706 A CN110899706 A CN 110899706A CN 201911034559 A CN201911034559 A CN 201911034559A CN 110899706 A CN110899706 A CN 110899706A
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China
Prior art keywords
beryllium
steel sheath
extrusion
powder
preparation
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CN201911034559.5A
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Chinese (zh)
Inventor
王东新
刘兆刚
王维一
谢垚
李军义
王亮
刘宁
王战宏
赵克俊
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Northwest Rare Metal Materials Research Institute Ningxia Co Ltd
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Northwest Rare Metal Materials Research Institute Ningxia Co Ltd
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Priority to CN201911034559.5A priority Critical patent/CN110899706A/en
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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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B22F2003/208—Warm or hot extruding

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a preparation method of a beryllium rod, which comprises the following steps: preparing beryllium powder with the average particle size of 2-100 mu m into a cylindrical powder blank by adopting a die pressing or cold isostatic pressing method; secondly, consolidating the cylindrical powder blank; step three, after the consolidated cylindrical powder blank is sequentially shaped and loaded into a steel sheath, heating to 300-600 ℃ under a vacuum condition, preserving heat for 1-3 hours, and sealing and welding an air exhaust opening of the steel sheath; preheating an extrusion cylinder of the extruder; heating the sealed and welded steel sheath to 800-1140 ℃, preserving heat for 2-16 hours, putting the steel sheath into a preheated extrusion cylinder, and extruding at an extrusion speed of more than 100mm/s, an extrusion temperature of more than 1100 ℃ and an extrusion ratio of 13-16; and step five, carrying out acid washing on the extruded steel sheath, and removing the steel sheath to obtain the required beryllium rod. The invention also discloses a beryllium bar. The method can prepare the pure beryllium bar with qualified apparent quality, low impurity content, compact structure and excellent performance, and improves the plasticity of the material.

Description

Beryllium rod and preparation method thereof
Technical Field
The invention belongs to the technical field of metal material pressure processing, and relates to a beryllium rod and a preparation method thereof.
Background
The metal beryllium has the advantages of light weight, high rigidity, high elastic modulus, high specific heat capacity, good thermal conductivity, good thermal stability, good dimensional stability and the like, and is widely applied to the fields of nuclear warheads, nuclear reactors, inertial navigation, optical systems, structural materials, thermodynamics, high-energy physics and other typical commercial applications.
At present, it is reported that there are two main methods for preparing pure beryllium rods: (1) the method has the advantages that the method has the defects of low yield, poor performance of beryllium rod preparation and high cost; (2) and preparing a beryllium ingot blank by adopting a cold isostatic pressing and hot isostatic pressing process, and processing by using linear cutting according to the size of the beryllium bar. But the isostatic pressing cost is high, the cutting processing time is long, the produced waste is more, the process period is long, and the production cost is high.
Disclosure of Invention
The invention aims to provide a method for preparing a beryllium rod, which aims to solve the technical problem that metal beryllium is difficult to plastically deform in the prior art.
The second purpose of the invention is to provide a beryllium rod.
In order to achieve one of the purposes, the invention adopts the following technical scheme:
a preparation method of a beryllium rod comprises the following steps:
preparing beryllium powder with the average particle size of 2-100 mu m into a cylindrical powder blank by adopting a die pressing or cold isostatic pressing method;
secondly, consolidating the cylindrical powder blank;
step three, after the consolidated cylindrical powder blank is sequentially shaped and loaded into a steel sheath, heating the cylindrical powder blank to 300-600 ℃ under a vacuum condition, preserving heat for 1-3 hours, and sealing and welding an air exhaust opening of the steel sheath, so that the defects of oxidation, surface air hole generation and the like of the consolidated cylindrical powder blank in the heating and heat preserving process are avoided;
preheating an extrusion cylinder of the extruder; heating the sealed and welded steel sheath to 800-1140 ℃, preserving heat for 2-16 hours, then preheating, and extruding at an extrusion speed of more than 100mm/s, an extrusion temperature of more than 1100 ℃ and an extrusion ratio of 13-16;
and step five, carrying out acid washing on the extruded steel sheath, and removing the steel sheath to obtain the required beryllium rod.
Further, in the step one, the purity of the beryllium powder is more than or equal to 99 percent; the average particle size of the beryllium powder is 10-50 mu m; the beryllium powder is flaky powder or spherical powder.
Further, in the third step, the steel sheath is made of stainless steel or Q235 steel.
Further, in step three, the vacuum value of the vacuum condition is 10-5-10-2Pa。
Further, in the third step, the heat preservation time is 5-10 hours.
Further, in the fourth step, the preheating temperature of the extrusion cylinder is 300-500 ℃.
Further, the extrusion speed is 105-110 mm/s; the extrusion temperature is 1140-1180 ℃;
further, in the fifth step, the acid for acid washing is dilute nitric acid or concentrated nitric acid configured according to a volume ratio of 1: 3-1: 5.
In order to achieve the second purpose, the invention adopts the following technical scheme:
a beryllium bar is prepared by the preparation method.
The invention has the beneficial effects that:
1. the process is simple and feasible, and by implementing the extrusion process, the pure beryllium bar material with qualified apparent quality, low impurity content, compact matrix structure, good mechanical property, few internal defects and high yield is prepared, so that the plasticity of the material is improved, the technical problem of extrusion forming of the brittle metal beryllium material is solved, and the method has important significance for further expanding the application range of the metal beryllium.
2. The beryllium bar is prepared by adopting an extrusion process, so that the production period is short, the efficiency is high, the produced waste is less, and the production cost is low; and the blank is compact, has no casting defects such as holes, shrinkage porosity, large grains and the like, and is easy to plastically deform.
3. Tensile strength sigma of beryllium rod prepared by the inventionb450 to 700MPa, yield strength sigma0.2300 to 480MPa and an elongation delta of 4 to 10 percent.
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention.
Example 1:
step one, determining the using amount of beryllium powder and the sizes of a beryllium ingot and an extrusion die according to the size and the extrusion deformation of a beryllium rod to be prepared, and preparing sheet beryllium powder with the purity of 99.3 percent and the average particle size of 10 mu m into a cylindrical powder blank by adopting a steel die;
step two, adopting a vacuum sintering process to consolidate the cylindrical powder blank;
step three, the consolidated cylindrical powder blank is sequentially shaped and loaded into a steel sheath 10-2Heating to 400 ℃ under Pa vacuum, preserving heat for 3 hours, and sealing and welding an exhaust opening of the steel sheath;
step four, preheating an extrusion cylinder of an extruder to 400 ℃, heating the sealed and welded steel sheath to 1140 ℃, preserving heat for 16 hours, putting the steel sheath into the preheated extrusion cylinder, and extruding at the extrusion speed of 105mm/s and the extrusion temperature of 1120 ℃ and the extrusion ratio of 15;
and step five, adopting dilute nitric acid to carry out acid washing on the extruded steel sheath, and removing the steel sheath, thereby obtaining the required beryllium rod.
The beryllium rod prepared by the embodiment has qualified apparent quality, low impurity content, compact structure, excellent mechanical property and easy plastic deformation, and has short production period, high efficiency, less produced waste, low production cost and tensile strength sigmab600MPa, yield strength sigma0.2430MPa and an elongation delta of 8%.
Example 2:
step one, determining the using amount of beryllium powder and the sizes of a beryllium ingot and an extrusion die according to the size and the extrusion deformation of a beryllium rod to be prepared, and preparing spherical beryllium powder with the purity of 99.2 percent and the average particle size of 50 mu m into a cylindrical powder blank by adopting a rubber soft sheath;
step two, adopting a vacuum sintering process to consolidate the cylindrical powder blank;
step three, sequentially shaping the consolidated cylindrical powder blank, filling the cylindrical powder blank into a Q235 steel sheath, and then placing the shaped cylindrical powder blank into a container 10-3Heating to 300 ℃ under Pa vacuum, keeping the temperature for 1 hour, and sealing and welding an air extraction opening of the steel sheath;
step four, preheating an extrusion cylinder of an extruder to 300 ℃, heating the sealed and welded steel sheath to 800 ℃, preserving heat for 2 hours, putting the steel sheath into the preheated extrusion cylinder, and extruding at an extrusion speed of 110mm/s, an extrusion temperature of 1140 ℃ and an extrusion ratio of 13;
and step five, adopting nitric acid with the volume concentration of 1/3 to perform acid washing on the extruded steel sheath, and removing the steel sheath to obtain the required beryllium rod.
The beryllium rod prepared by the embodiment has qualified apparent quality, low impurity content, compact structure, excellent mechanical property and easy plastic deformation, and has short production period, high efficiency, less produced waste, low production cost and tensile strength sigmab550MPa, yield strength sigma0.2410MPa and an elongation delta of 7%.
Example 3:
step one, determining the using amount of beryllium powder and the sizes of a beryllium ingot and an extrusion die according to the size and the extrusion deformation of a beryllium rod to be prepared, and preparing spherical beryllium powder with the purity of 99.1 percent and the average particle size of 50 mu m into a cylindrical powder blank by adopting a rubber soft sheath;
step two, adopting a vacuum sintering process to consolidate the cylindrical powder blank;
step three, sequentially shaping the consolidated cylindrical powder blank, filling the cylindrical powder blank into a Q235 steel sheath, and then placing the shaped cylindrical powder blank into a container 10-4Heating to 600 ℃ under Pa vacuum, keeping the temperature for 2 hours, and sealing and welding an exhaust opening of the steel sheath;
step four, preheating an extrusion cylinder of an extruder to 500 ℃, heating the sealed and welded steel sheath to 1000 ℃, preserving heat for 10 hours, putting the steel sheath into the preheated extrusion cylinder, and extruding at the extrusion speed of 108mm/s, the extrusion temperature of 1160 ℃ and the extrusion ratio of 16;
and step five, adopting nitric acid with the volume concentration of 1/5 to perform acid washing on the extruded steel sheath, and removing the steel sheath to obtain the required beryllium rod.
The beryllium rod prepared by the embodiment has qualified apparent quality, low impurity content, compact structure, excellent mechanical property and easy plastic deformation, and has short production period, high efficiency, less produced waste, low production cost and tensile strength sigmab540MPa, yield strength sigma0.2400MPa and an elongation delta of 6%.
Example 4:
step one, determining the using amount of beryllium powder and the sizes of a beryllium ingot and an extrusion die according to the size and the extrusion deformation of a beryllium rod to be prepared, and preparing sheet beryllium powder with the purity of 99.5 percent and the average particle size of 100 mu m into a cylindrical powder blank by adopting a rubber soft sheath;
step two, adopting a vacuum sintering process to consolidate the cylindrical powder blank;
step three, the consolidated cylindrical powder blank is sequentially shaped and filled into a stainless steel sheath and then is placed in a container 10-4Heating to 500 ℃ under Pa vacuum, keeping the temperature for 2.5 hours, and sealing and welding an exhaust opening of the steel sheath;
step four, preheating an extrusion cylinder of an extruder to 350 ℃, heating the sealed and welded steel sheath to 1100 ℃, preserving heat for 12 hours, putting the steel sheath into the preheated extrusion cylinder, and extruding at the extrusion speed of 107mm/s, the extrusion temperature of 1180 ℃ and the extrusion ratio of 14;
and step five, adopting nitric acid with the volume concentration of 1/4 to perform acid washing on the extruded steel sheath, and removing the steel sheath to obtain the required beryllium rod.
The beryllium rod prepared by the embodiment has qualified apparent quality, low impurity content, compact structure, excellent mechanical property and easy plastic deformation, and has short production period, high efficiency, less produced waste, low production cost and tensile strength sigmab470MPa, yield strength sigma0.2360MPa and an elongation delta of 4%.
It will be evident to those skilled in the art that the embodiments of the present invention are not limited to the details of the foregoing illustrative embodiments, and that the embodiments of the present invention are capable of being embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the embodiments being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Furthermore, it is obvious that the word "comprising" does not exclude other elements or steps, and the singular does not exclude the plural. Several units, modules or means recited in the system, apparatus or terminal claims may also be implemented by one and the same unit, module or means in software or hardware. The terms first, second, etc. are used to denote names, but not any particular order.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the embodiments of the present invention and not for limiting, and although the embodiments of the present invention are described in detail with reference to the above preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the embodiments of the present invention without departing from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (9)

1. A preparation method of a beryllium rod is characterized by comprising the following steps:
preparing beryllium powder with the average particle size of 2-100 mu m into a cylindrical powder blank by adopting a die pressing or cold isostatic pressing method;
secondly, consolidating the cylindrical powder blank;
step three, after the consolidated cylindrical powder blank is sequentially shaped and loaded into a steel sheath, heating to 300-600 ℃ under a vacuum condition, preserving heat for 1-3 hours, and sealing and welding an air exhaust opening of the steel sheath;
preheating an extrusion cylinder of the extruder; heating the sealed and welded steel sheath to 800-1140 ℃, preserving heat for 2-16 hours, putting the steel sheath into a preheated extrusion cylinder, and extruding at an extrusion speed of more than 100mm/s, an extrusion temperature of more than 1100 ℃ and an extrusion ratio of 13-16;
and step five, carrying out acid washing on the extruded steel sheath, and removing the steel sheath to obtain the required beryllium rod.
2. The preparation method according to claim 1, wherein in the first step, the beryllium powder has a purity of not less than 99%; the average particle size of the beryllium powder is 10-50 mu m; the beryllium powder is flaky powder or spherical powder.
3. The preparation method according to claim 1 or 2, wherein in the third step, the steel sheath is made of stainless steel or Q235 steel.
4. The method according to claim 1 or 2, wherein the vacuum value of the vacuum condition in step three is 10-5-10-2Pa。
5. The method according to claim 1 or 2, wherein the heat-retaining time is 5 to 10 hours in the third step.
6. The method according to claim 1 or 2, wherein the preheating temperature of the extrusion cylinder in the fourth step is 300 to 500 ℃.
7. The method according to claim 1 or 2, wherein in the fifth step, the extrusion speed is 105 to 110 mm/s; the extrusion temperature is 1140-1180 ℃.
8. The preparation method according to claim 1 or 2, wherein in the fifth step, the acid for acid washing is dilute nitric acid or concentrated nitric acid configured according to a volume ratio of 1: 3-1: 5.
9. A beryllium rod prepared by the preparation method of any one of claims 1 to 8.
CN201911034559.5A 2019-10-29 2019-10-29 Beryllium rod and preparation method thereof Pending CN110899706A (en)

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FR2814179A1 (en) * 2000-09-15 2002-03-22 Franco Belge Combustibles Creep-resistant silver-based alloy for production of neutron absorption elements includes indium, cadmium and, optionally, hafnium, and their oxides in the form of particles distributed in the alloy
CN103014395A (en) * 2012-12-09 2013-04-03 温州聚星电接触科技有限公司 Method for preparing efficient aerated mixed powder
CN104493167A (en) * 2014-11-20 2015-04-08 中国航空工业集团公司北京航空材料研究院 Method for forming powder high-temperature alloy annular member
CN104588653A (en) * 2015-01-20 2015-05-06 哈尔滨工业大学 Preparation method of TiAl alloy profile
CN105256171A (en) * 2015-10-30 2016-01-20 中南大学 Copper-nickel-tin alloy bar and manufacturing method thereof
CN107695358A (en) * 2017-09-07 2018-02-16 北京科技大学 A kind of preparation method of welding electrode
CN110355363A (en) * 2019-08-16 2019-10-22 苏州金江铜业有限公司 A kind of preparation method of aluminium oxide chromium-zirconium-copper composite material

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US5482672A (en) * 1995-02-09 1996-01-09 Friedman; Ira Process for extruding tantalum and/or niobium
FR2814179A1 (en) * 2000-09-15 2002-03-22 Franco Belge Combustibles Creep-resistant silver-based alloy for production of neutron absorption elements includes indium, cadmium and, optionally, hafnium, and their oxides in the form of particles distributed in the alloy
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CN104588653A (en) * 2015-01-20 2015-05-06 哈尔滨工业大学 Preparation method of TiAl alloy profile
CN105256171A (en) * 2015-10-30 2016-01-20 中南大学 Copper-nickel-tin alloy bar and manufacturing method thereof
CN107695358A (en) * 2017-09-07 2018-02-16 北京科技大学 A kind of preparation method of welding electrode
CN110355363A (en) * 2019-08-16 2019-10-22 苏州金江铜业有限公司 A kind of preparation method of aluminium oxide chromium-zirconium-copper composite material

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