CN110919003A - Preparation method of vacuum hot-pressed beryllium material with diameter larger than 300mm and beryllium material - Google Patents
Preparation method of vacuum hot-pressed beryllium material with diameter larger than 300mm and beryllium material Download PDFInfo
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- CN110919003A CN110919003A CN201910850543.5A CN201910850543A CN110919003A CN 110919003 A CN110919003 A CN 110919003A CN 201910850543 A CN201910850543 A CN 201910850543A CN 110919003 A CN110919003 A CN 110919003A
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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
- B22F3/14—Both compacting and sintering simultaneously
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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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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Abstract
The invention discloses a preparation method of vacuum hot-pressed beryllium materials with the diameter larger than 300mm, which comprises the following steps: firstly, preparing beryllium powder with the weight content of beryllium more than 99% and the average particle size of 10-14 mu m; secondly, placing the beryllium powder into a graphite die with the inner diameter larger than 300mm, baking, and then placing into a vacuum hot pressing furnace for pressure sintering; and step three, cooling the beryllium powder after pressure sintering to room temperature, and then demolding to obtain the vacuum hot-pressed beryllium material with the diameter larger than 300 mm. The invention also discloses a vacuum hot-pressing beryllium material with the diameter larger than 300 mm. The invention has the characteristics of high pressing force, large diameter of pressed products, high pressing efficiency, low pressing cost and the like.
Description
Technical Field
The invention belongs to the technical field of rare metal powder metallurgy, and relates to a preparation method of vacuum hot-pressed beryllium material with the diameter larger than 300mm and the beryllium material.
Background
Beryllium as a rare light metal has the characteristics of excellent thermal property, high rigidity and specific strength, good dimensional stability, low atomic and neutron absorption cross section and the like, and is widely applied to the aspects of reactors, nuclear weapons, aerospace industry and instruments and meters.
Due to the specific performance and sensitive application field of the beryllium material, the beryllium material is classified as strategic metal in all countries in the world, so that the processing technology and application research of the beryllium material are completely blocked, the beryllium material is not traded, and the beryllium material is not reported. In 1974, the vacuum hot pressing method is adopted in China to prepare beryllium products, and due to the limitation of the performance of die materials, the pressing force is low, and the performances are as follows: the density reaches 1.84g/cm3, the ultimate tensile strength is about 300MPa, and the elongation is about 1%. At present, the vacuum hot-pressing beryllium material with the diameter of less than 200mm can be stably produced, the blow-in cost is high, and the pressing efficiency is low.
Disclosure of Invention
One of the purposes of the invention is to provide a preparation method of vacuum hot-pressed beryllium materials with the diameter larger than 300mm, so as to solve the technical problems of low pressing force, low pressing efficiency and high cost in the pressing process of small-size hot-pressed beryllium materials.
The second purpose of the invention is to provide a vacuum hot-pressed beryllium material with the diameter larger than 300 mm.
In order to achieve one of the purposes, the invention adopts the following technical scheme:
a preparation method of vacuum hot-pressed beryllium materials with the diameter larger than 300mm comprises the following steps:
firstly, preparing beryllium powder with the weight content of beryllium more than 99% and the average particle size of 10-14 mu m;
secondly, placing the beryllium powder into a graphite die with the inner diameter larger than 300mm, baking, and then placing into a vacuum hot pressing furnace for pressure sintering;
and step three, cooling the beryllium powder after pressure sintering to room temperature, and then demolding to obtain the vacuum hot-pressed beryllium material with the diameter larger than 300 mm.
According to the invention, a graphite die with the inner diameter larger than 300mm is adopted, beryllium powder is loaded into a die cavity, graphite punches are plugged into two ends of the graphite die, and the graphite die is pressed, sintered and molded in a vacuum state, so that the generation of beryllium oxide can be effectively reduced in the vacuum state, the powder is softened and flowed under high temperature and high pressure, and pores are filled, thus the density of the material is improved, and the mechanical property and ductility of the beryllium material with the size can be ensured.
Further, the total weight content of impurities in the beryllium powder is less than 1%.
Further, in the second step, the baking temperature is 180-220 ℃; the baking time is more than 8 hours.
Further, the baking time is 10-15 hours.
Further, in the second step, the process conditions of the pressure sintering are as follows:
vacuum degree of not less than 8X 10-2The temperature rise speed is less than 150 ℃/h, the heat preservation temperature is 1100-1150 ℃, and the pressure maintaining pressure is 15-25 MPa/cm2And keeping the temperature and the pressure for 2-8 hours, and cutting off the power and cooling along with the furnace after the heat preservation and the pressure are finished.
Further, the temperature rise speed is 100-140 ℃/h, the heat preservation temperature is 1120-1140 ℃, and the pressure maintaining pressure is 18-22 MPa/cm2And the heat preservation and pressure maintaining time is 4-6 hours.
In order to achieve the second purpose, the invention adopts the following technical scheme:
a vacuum hot-pressed beryllium material with the diameter larger than 300mm is prepared by the preparation method.
The beneficial effects of the invention are described as follows:
the vacuum hot-pressed beryllium material prepared by the method has the advantages that on the premise that the diameter is larger than 300mm, the ultimate tensile strength is larger than about 300MPa, the elongation is larger than 2%, the pressing efficiency is high, and the pressing cost is low.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Example 1:
step one, beryllium powder with the weight content of 99.4 percent and the average grain diameter of 14 mu m is prepared, and the total weight content of impurities is 0.5 percent.
Secondly, placing the beryllium powder into a die, baking, and then placing into a vacuum hot pressing furnace for pressure sintering;
the baking temperature is 180 ℃; baking for 10 hours.
The process conditions of pressure sintering are as follows: vacuum 1X 10-2Heating at 145 deg.C/h, 1140 deg.C, and holding pressure of 25MPa/cm2And keeping the temperature and the pressure for 2 hours.
And step three, cooling the beryllium powder after pressure sintering to room temperature, and then demolding to obtain the vacuum hot-pressed beryllium material with the diameter of 310 mm.
The performance parameters of the vacuum hot-pressed beryllium material with the diameter of 310mm prepared in the embodiment are shown in the following table:
example 2:
step one, beryllium powder with 99.8 percent of beryllium weight and 10 mu m of average grain diameter is prepared, and the total weight content of impurities is 0.1 percent.
Secondly, placing the beryllium powder into a graphite die with the inner diameter larger than 300mm, baking, and then placing into a vacuum hot pressing furnace for pressure sintering;
the baking temperature is 200 ℃; the baking time was 15 hours.
The process conditions of the pressure sintering are as follows: vacuum 2X 10-2Heating at 100 deg.C/h, holding at 1150 deg.C, and maintaining at 18MPa/cm2And keeping the temperature and the pressure for 8 hours.
And step three, cooling the beryllium powder after pressure sintering to room temperature, and then demolding to obtain the vacuum hot-pressed beryllium material with the diameter of 350 mm.
The performance parameters of the vacuum hot-pressed beryllium material with the diameter of 350mm prepared in the embodiment are shown in the following table:
example 3:
step one, beryllium powder with the weight content of 99.5% and the average grain diameter of 11 μm is prepared.
Secondly, placing the beryllium powder into a graphite die with the inner diameter larger than 300mm, baking, and then placing into a vacuum hot pressing furnace for pressure sintering;
the baking temperature is 220 ℃; the baking time was 13 hours.
The process conditions of the pressure sintering are as follows: vacuum 3X 10-2Heating at 140 deg.C/h, 1100 deg.C, and 22MPa/cm2And keeping the temperature and the pressure for 6 hours.
And step three, cooling the beryllium powder after pressure sintering to room temperature, and then demolding to obtain the vacuum hot-pressed beryllium material with the diameter of 330 mm.
The performance parameters of the vacuum hot-pressed beryllium material with the diameter of 330mm prepared in the embodiment are shown in the following table:
example 4:
step one, beryllium powder with the weight content of 99.7% and the average grain diameter of 12 mu m is prepared.
Secondly, placing the beryllium powder into a graphite die with the inner diameter larger than 300mm, baking, and then placing into a vacuum hot pressing furnace for pressure sintering;
the baking temperature is 210 ℃; the baking time was 14 hours.
The process conditions of the pressure sintering are as follows: vacuum 3X 10-2Heating at 120 deg.C/h, holding at 1120 deg.C, and holding pressure at 15MPa/cm2And keeping the temperature and the pressure for 4 hours.
And step three, cooling the beryllium powder after pressure sintering to room temperature, and then demolding to obtain the vacuum hot-pressed beryllium material with the diameter of 340 mm.
The performance parameters of the vacuum hot-pressed beryllium material with the diameter of 340mm prepared in the embodiment are shown in the following table:
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 (7)
1. A preparation method of vacuum hot-pressed beryllium materials with the diameter larger than 300mm is characterized by comprising the following steps:
firstly, preparing beryllium powder with the weight content of beryllium more than 99% and the average particle size of 10-14 mu m;
secondly, placing the beryllium powder into a graphite die with the inner diameter larger than 300mm, baking, and then placing into a vacuum hot pressing furnace for pressure sintering;
and step three, cooling the beryllium powder after pressure sintering to room temperature, and then demolding to obtain the vacuum hot-pressed beryllium material with the diameter larger than 300 mm.
2. The method of claim 1, wherein the beryllium powder has a total impurity content of less than 1% by weight.
3. The preparation method according to claim 1 or 2, wherein in the second step, the baking temperature is 180-220 ℃; the baking time is more than 8 hours.
4. The method according to claim 3, wherein the baking time is 10 to 15 hours.
5. The preparation method according to claim 1 or 2, wherein in the second step, the process conditions of the pressure sintering are as follows:
vacuum degree of not less than 8X 10-2The temperature rise speed is less than 150 ℃/h, the heat preservation temperature is 1100-1150 ℃, and the pressure maintaining pressure is 15-25 MPa/cm2And keeping the temperature and the pressure for 2-8 hours, and cutting off the power and cooling along with the furnace after the heat preservation and the pressure are finished.
6. The method according to claim 5, wherein the temperature rise rate is 100 to 140 ℃/h, the holding temperature is 1120 to 1140 ℃, and the holding pressure is 18 to 22MPa/cm2And the heat preservation and pressure maintaining time is 4-6 hours.
7. A vacuum hot-pressed beryllium material with the diameter larger than 300mm, which is prepared by the preparation method of any one of claims 1-6.
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| CN201910850543.5A CN110919003A (en) | 2019-09-10 | 2019-09-10 | Preparation method of vacuum hot-pressed beryllium material with diameter larger than 300mm and beryllium material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111804909A (en) * | 2020-06-18 | 2020-10-23 | 西北稀有金属材料研究院宁夏有限公司 | Powder filling method of beryllium material forming blank for CETR reactor |
| CN113275566A (en) * | 2021-04-09 | 2021-08-20 | 西北稀有金属材料研究院宁夏有限公司 | Preparation method of vacuum hot-pressed beryllium material with diameter of 500-700 mm and beryllium material |
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| GB1088049A (en) * | 1963-10-07 | 1967-10-18 | Atomic Energy Authority Uk | Improvements in or relating to the sintering of beryllium |
| JP2016018875A (en) * | 2014-07-08 | 2016-02-01 | トヨタ自動車株式会社 | Method for manufacturing sintered compact |
| CN105345006A (en) * | 2015-06-11 | 2016-02-24 | 西北稀有金属材料研究院 | Direct-heating type hot-pressing equipment suitable for producing large-size beryllium materials |
| CN107513634A (en) * | 2017-08-21 | 2017-12-26 | 湖南金马铝业有限责任公司 | A kind of densification process for preparing high body and dividing SiCp/Al composites |
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2019
- 2019-09-10 CN CN201910850543.5A patent/CN110919003A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1088049A (en) * | 1963-10-07 | 1967-10-18 | Atomic Energy Authority Uk | Improvements in or relating to the sintering of beryllium |
| JP2016018875A (en) * | 2014-07-08 | 2016-02-01 | トヨタ自動車株式会社 | Method for manufacturing sintered compact |
| CN105345006A (en) * | 2015-06-11 | 2016-02-24 | 西北稀有金属材料研究院 | Direct-heating type hot-pressing equipment suitable for producing large-size beryllium materials |
| CN107513634A (en) * | 2017-08-21 | 2017-12-26 | 湖南金马铝业有限责任公司 | A kind of densification process for preparing high body and dividing SiCp/Al composites |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111804909A (en) * | 2020-06-18 | 2020-10-23 | 西北稀有金属材料研究院宁夏有限公司 | Powder filling method of beryllium material forming blank for CETR reactor |
| CN111804909B (en) * | 2020-06-18 | 2022-07-08 | 西北稀有金属材料研究院宁夏有限公司 | Powder filling method of beryllium material forming blank for CETR reactor |
| CN113275566A (en) * | 2021-04-09 | 2021-08-20 | 西北稀有金属材料研究院宁夏有限公司 | Preparation method of vacuum hot-pressed beryllium material with diameter of 500-700 mm and beryllium material |
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