CN108687158B - preparation method of isotropic molybdenum plate - Google Patents
preparation method of isotropic molybdenum plate Download PDFInfo
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- CN108687158B CN108687158B CN201810447470.0A CN201810447470A CN108687158B CN 108687158 B CN108687158 B CN 108687158B CN 201810447470 A CN201810447470 A CN 201810447470A CN 108687158 B CN108687158 B CN 108687158B
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- molybdenum
- isotropic
- molybdenum plate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/02—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
Abstract
The invention discloses a preparation method of an isotropic molybdenum plate. The method comprises the following steps: (1) the method comprises the following steps of (1) processing a molybdenum blank with the molybdenum content of more than 99% as a raw material at least twice through a high-speed forging process, wherein the impact energy instantaneously borne by a molybdenum plate at each time is 3-7 MJ, and the pass deformation is 30-50%; (2) rolling the product obtained in the step (1) at least once to enable the total deformation amount to reach 10-30%; (3) and heating the rolled product to 800-1200 ℃, and keeping the temperature for 60-120 min at the heating rate of 100-500 ℃/min. The molybdenum plate prepared by the method is almost flawless in the interior and is isotropic.
Description
Technical Field
The invention belongs to the technical field of metal template preparation, and particularly relates to a preparation method of an isotropic molybdenum plate.
Background
molybdenum parts used in the field of precision electronic components and other precision devices are often extremely complex in structure and have high requirements on the dimensional precision of the parts, for example: a slow wave structural member of the high-power traveling wave tube, a grid of the high-power transmitting tube, a liner of the armor piercing bomb and the like. To meet the performance and precision machining requirements of such products, it is a necessary condition that the molybdenum plate has isotropy or small anisotropy. The molybdenum plate manufactured by the prior art has obvious anisotropy, internal defects and poor machining performance due to the plate texture, so that the manufacturing requirements of the precision molybdenum part cannot be met.
Disclosure of Invention
aiming at the defects in the prior art, the invention provides the preparation method of the isotropic molybdenum plate, which can effectively solve the problems of anisotropy and insufficient machining performance of the molybdenum plate prepared by the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
A method of making an isotropic molybdenum plate comprising the steps of:
(1) The method comprises the following steps of (1) processing a molybdenum blank with the molybdenum content of more than 99% as a raw material at least twice through a high-speed forging process, wherein the impact energy instantaneously borne by a molybdenum plate at each time is 3-7 MJ, and the pass deformation is 30-50%;
(2) Rolling the product obtained in the step (1) at least once to enable the total deformation amount to reach 10-30%;
(3) And heating the rolled product to 800-1200 ℃, and keeping the temperature for 60-120 min at the heating rate of 100-500 ℃/min.
Further, the specific process of the high-speed forging process in the step (1) is as follows: the forging speed is 100-120 m/s; the impact energy instantaneously born by the molybdenum billet each time is 4.6MJ, and the pass deformation is 35%.
Further, the rolling in the step (2) is warm rolling or cold rolling.
Further, the temperature in the warm rolling process is 750-1000 ℃.
Further, in the step (3), the temperature is 900 ℃, the heating rate is 240 ℃/min, and the temperature is kept for 80 min.
the invention has the beneficial effects that:
1. The high-purity molybdenum blank with the molybdenum content of more than 99.98 percent is used as a raw material for preparing the molybdenum plate, so that the adverse effect of impurity elements on the performance of the molybdenum plate is reduced.
2. The high-speed and high-energy forging process breaks the internal crystal grains into fine isometric crystal grains, a plurality of micro defects existing in the molybdenum billet are pressed and disappear, and due to the extremely high deformation speed, newly generated micro cracks are pressed and disappear again before expanding, so that the molybdenum plate with few internal defects is obtained.
3. the thickness size precision of the molybdenum plate is improved by the total deformation of the proper molybdenum plate after warm rolling or cold rolling so as to meet the requirement of subsequent precision machining; finally, the molybdenum plate is ensured to have isotropic characteristics through homogenization heat treatment.
Detailed Description
The following description of the embodiments of the present invention is provided to facilitate the understanding of the present invention by those skilled in the art, but it should be understood that the present invention is not limited to the scope of the embodiments, and it will be apparent to those skilled in the art that various changes may be made without departing from the spirit and scope of the invention as defined and defined in the appended claims, and all matters produced by the invention using the inventive concept are protected.
Example 1
A method of making an isotropic molybdenum plate comprising the steps of:
(1) Using a molybdenum blank with the molybdenum content of 99.995 percent as a raw material, and utilizing a press machine to perform high-speed forging process processing twice according to the product requirements, wherein the forging speed of each time is 120m/s, the impact energy instantaneously born by the molybdenum blank is 4.6MJ, and the pass deformation is 35 percent;
(2) rolling the product obtained in the step (1) twice by cold rolling to ensure that the total deformation of the product reaches 30 percent and the deformation of each rolling is the same;
(3) and (3) heating the cold-rolled product to 900 ℃ at the speed of 240 ℃/min, and preserving the heat for 80min to prepare the isotropic molybdenum plate.
Example 2
A method of making an isotropic molybdenum plate comprising the steps of:
(1) Taking a molybdenum blank with the molybdenum content of 99.992% as a raw material, and carrying out three times of high-speed forging processing by using a press according to the product requirement, wherein the forging speed of each time is 100m/s, the impact energy instantaneously born by the molybdenum blank each time is 3MJ, and the pass deformation is 30%;
(2) rolling the product obtained in the step (1) once at 750 ℃ to ensure that the total deformation of the product reaches 20 percent, and the deformation of each rolling is the same;
(3) And (3) heating the product after warm rolling to 1000 ℃ at the speed of 200 ℃/min, and preserving the heat for 60min to prepare the isotropic molybdenum plate.
Example 3
A method of making an isotropic molybdenum plate comprising the steps of:
(1) taking a molybdenum blank with the molybdenum content of more than 99.994 percent as a raw material, and performing four times of high-speed forging process processing by using a press according to the product requirement, wherein the forging speed of each time is 110m/s, the impact energy instantaneously born by the molybdenum blank each time is 7MJ, and the pass deformation is 50 percent;
(2) Rolling the product obtained in the step (1) for three times at 1000 ℃ to ensure that the total deformation of the product reaches 28 percent, and the deformation of each rolling is the same;
(3) And heating the product after warm rolling to 1200 ℃ at the speed of 300 ℃/min, and preserving the heat for 120min to prepare the isotropic molybdenum plate.
Comparative example 1
compared with the example 1, the high-speed forging process is absent in the step (1), and the rest of the process is the same as the example 1.
Comparative example 2
compared with the example 1, the temperature raising and maintaining process is lacked in the step (3), and the rest processes are the same as the example 1.
Comparative example 3
Compared with the embodiment 1, the high-speed forging process is absent in the step (1), the heating and heat preservation treatment process is absent in the step (3), and the rest processes are the same as the embodiment 1.
detection of
The performance parameters of the molybdenum plates prepared in examples 1 to 3 and comparative examples 1 to 3 were measured under the same conditions, and the results are shown in table 1.
TABLE 1 comparison of molybdenum plate Performance parameters
Gap Rate (%) | content of impurities (%) | Isotropy | |
Example 1 | 0.50 | 0.005 | Is that |
Example 2 | 0.66 | 0.008 | is that |
Example 3 | 0.55 | 0.006 | is that |
Comparative example 1 | 5.6 | 0.0018 | Is that |
Comparative example 2 | 1.32 | 0.001 | Whether or not |
Comparative example 3 | 7.8 | 0.0019 | whether or not |
As can be seen from the data in Table 1, the molybdenum plates prepared in examples 1 to 3 have higher quality than the molybdenum plates prepared in comparative examples, particularly the molybdenum plate prepared in example 1 has the best effect, and the quality detection data of the molybdenum plates prepared in comparative examples 1 to 3 show that the high-speed forging process and the temperature-raising and heat-preserving treatment have great influence on the performance of the molybdenum plates, so that the molybdenum plates with almost no defect inside and isotropy can be prepared only by matching the steps and the process parameters mentioned in the method.
Claims (1)
1. A method for preparing an isotropic molybdenum plate, comprising the steps of:
(1) Taking a molybdenum blank with the molybdenum content of more than 99.994 percent as a raw material, and performing four times of high-speed forging process processing by using a press according to the product requirement, wherein the forging speed of each time is 110m/s, the impact energy instantaneously born by the molybdenum blank each time is 7MJ, and the pass deformation is 50 percent;
(2) rolling the product obtained in the step (1) for three times at 1000 ℃ to ensure that the total deformation of the product reaches 28 percent, and the deformation of each rolling is the same;
(3) And heating the product after warm rolling to 1200 ℃ at the speed of 300 ℃/min, and preserving the heat for 120min to prepare the isotropic molybdenum plate.
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CN101956159A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum titanium sputtering target |
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CN104419901A (en) * | 2013-08-27 | 2015-03-18 | 宁波江丰电子材料股份有限公司 | Method for manufacturing tantalum target material |
CN104624642A (en) * | 2015-01-12 | 2015-05-20 | 郑州通达重型机械制造有限公司 | Method for rolling large unit-weight and wide molybdenum plates for sputtering target material |
CN107022739A (en) * | 2017-05-19 | 2017-08-08 | 包头稀土研究院 | The manufacture method of sputter coating molybdenum rotary target material |
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JPS62134131A (en) * | 1985-12-06 | 1987-06-17 | Toshiba Corp | Manufacture of high purity molybdenum or tungsten |
US20060042728A1 (en) * | 2004-08-31 | 2006-03-02 | Brad Lemon | Molybdenum sputtering targets |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101956159A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum titanium sputtering target |
CN102011076A (en) * | 2010-11-15 | 2011-04-13 | 宁夏东方钽业股份有限公司 | Processing technique of niobium alloy plate |
CN102560383A (en) * | 2012-01-12 | 2012-07-11 | 宝鸡市科迪普有色金属加工有限公司 | Molybdenum niobium alloy plate target material processing technology |
CN104419901A (en) * | 2013-08-27 | 2015-03-18 | 宁波江丰电子材料股份有限公司 | Method for manufacturing tantalum target material |
CN104190937A (en) * | 2014-06-19 | 2014-12-10 | 洛阳科威钨钼有限公司 | A preparation method of an ultra large fine-grain molybdenum electrode |
CN104624642A (en) * | 2015-01-12 | 2015-05-20 | 郑州通达重型机械制造有限公司 | Method for rolling large unit-weight and wide molybdenum plates for sputtering target material |
CN107022739A (en) * | 2017-05-19 | 2017-08-08 | 包头稀土研究院 | The manufacture method of sputter coating molybdenum rotary target material |
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