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A kind of rapid preparation process of fine-grained molybdenum plate

A preparation process, a technology of molybdenum plate, applied in the field of rapid preparation process of fine-grained molybdenum plate, can solve the problems of high cost, long sintering time, long time consumption, etc., to reduce loss and energy consumption, easy to microstructure, easy to uniform and small Effect

Active Publication Date: 2020-05-12
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of preparing molybdenum slabs by smelting method is that the production scale is large and the slab size is large, but the product grains are coarse and the microstructure is uneven; after decades of development, the powder metallurgy method can also produce large-size slabs, but resistance Conventional sintering and densification in the furnace, the densification process is slow, the required sintering temperature is too high, and the sintering time is too long. At the same time, the prepared plate also has coarse grains and poor microstructure uniformity.
[0003] Chinese patent CN 102699327A discloses a production process of molybdenum crucible. The preparation method mentioned needs to be heated in a hydrogen intermediate frequency sintering furnace at 1900°C for 30 hours, which leads to high energy consumption, high cost and large material grains.
[0004] Chinese patent CN 105220095B discloses a method for preparing a large single-weight molybdenum sheet. The method includes: using a molybdenum slab as a raw material, a hot rolling mill is used to open the molybdenum slab. The deformation of the billet is 20% to 30%; after the billet is annealed, heat preservation is carried out after annealing; after annealing, eight times of rolling are carried out to form a molybdenum slab. The preparation process is complicated and time-consuming, which increases the production cost.

Method used

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  • A kind of rapid preparation process of fine-grained molybdenum plate
  • A kind of rapid preparation process of fine-grained molybdenum plate
  • A kind of rapid preparation process of fine-grained molybdenum plate

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Embodiment 1

[0026] A rapid preparation process of a fine-grained molybdenum plate in this embodiment comprises the following steps:

[0027] Step 1, granulation: adding molybdenum powder with an average particle size of 20-50nm into 1 wt% stearic acid organic solvent, mixing evenly, spray drying and granulation;

[0028] Step 2, pressing: under the uniaxial pressure of 200MPa, the sprayed molybdenum particles are calmly pressed into a rectangular compact, and the pressure is maintained for 120s;

[0029] Step 3. Microwave sintering: In a microwave sintering furnace, heat up to 1600°C at a heating rate of 40°C / min under vacuum conditions, keep the temperature for 30 minutes, and cool the furnace to room temperature to obtain a sintered molybdenum slab with a density greater than 95%.

[0030] Step 4, cross-rolling: under a hydrogen atmosphere, heat the sintered molybdenum slab to 1350°C and keep it warm for 40 minutes, carry out two passes of cross-rolling, the deformation rate of each cro...

Embodiment 2

[0034] A rapid preparation process of a fine-grained molybdenum plate in this embodiment comprises the following steps:

[0035] Step 1, granulation: adding molybdenum powder with an average particle size of 20-50nm into 2wt% stearic acid organic solvent, mixing evenly, spray drying and granulation;

[0036] Step 2, pressing: under the uniaxial pressure of 200MPa, the sprayed molybdenum particles are calmly pressed into a rectangular compact, and the pressure is maintained for 120s;

[0037] Step 3. Microwave sintering: In a microwave sintering furnace, the temperature is raised to 1550°C at a heating rate of 70°C / min under vacuum conditions, kept for 15 minutes, and the furnace is cooled to room temperature to obtain a sintered molybdenum slab with a density greater than 95%.

[0038] Step 4, cross-rolling: under a hydrogen atmosphere, heat the sintered molybdenum slab to 1280°C and keep it warm for 30 minutes, carry out two passes of cross-rolling, the deformation rate of ea...

Embodiment 3

[0041] A rapid preparation process of a fine-grained molybdenum plate in this embodiment comprises the following steps:

[0042] Step 1, granulation: adding molybdenum powder with an average particle size of 20-50nm into 0.5wt% stearic acid organic solvent, mixing evenly, spray drying and granulation;

[0043] Step 2, pressing: under the uniaxial pressure of 250MPa, the sprayed molybdenum particles are calmly pressed into a rectangular compact, and the pressure is maintained for 120s;

[0044] Step 3. Microwave sintering: In a microwave sintering furnace, heat up to 1600°C at a heating rate of 50°C / min under vacuum conditions, keep the temperature for 20 minutes, and cool the furnace to room temperature to obtain a sintered molybdenum slab with a density greater than 95%.

[0045] Step 4, cross-rolling: under a hydrogen atmosphere, heat the sintered molybdenum slab to 1300°C and keep it warm for 40 minutes, perform two passes of cross-rolling, the deformation rate of each cros...

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Abstract

The invention discloses a rapid preparation process of a fine-grain molybdenum plate, and belongs to the technical field of powder metallurgy. The process comprises the following steps of (1) granulation; (2) suppression; and (3) microwave sintering, specifically, in a microwave sintering furnace, a green blank is rapidly heated to 1500-1600 DEG C and insulated for 10-40 minutes under a vacuum condition to obtain a sintered molybdenum plate blank with density greater than 95%; and (4) cross rolling, specifically, under the reducing atmosphere, the sintered molybdenum plate blank obtained by the step (3) is heated rapidly to 1200-1400 DEG C and insulated for 20-40 minutes for cogging and cross rolling, then, two to four passes of heating rolling are carried out, the heating temperature of each pass is reduced by 40-60 DEG C and the deformation of each pass of heating rolling is 20-25%, and after annealing, the molybdenum plate with fine and uniform grains is obtained. The rapid preparation process of the fine-grain molybdenum plate adopts the nano-powder combined with microwave sintering technology to densify molybdenum powders, so that the grains of the sintered blank are fine, theaverage grain size is 0.5-2 [mu]m, and microstructure is uniform; and the grain size is about 2-4 [mu]m after cross rolling, the microstructure of the plate is uniform and the grains of the plate arefine, and the strength of the plate is further improved.

Description

technical field [0001] The invention belongs to the technical field of powder metallurgy, and in particular relates to a rapid preparation process of fine-grained molybdenum plates. Background technique [0002] Molybdenum has the advantages of high melting point, good thermal and electrical conductivity, high hardness and high temperature strength, and is widely used in magnetron sputtering targets and some high temperature applications. With the development of modern technology and market, higher requirements are put forward for the purity, structure uniformity, grain size and processing performance of molybdenum plate. At present, for the production of molybdenum plates, there are methods such as smelting method and powder metallurgy method. The advantage of preparing molybdenum slabs by smelting method is that the production scale is large and the slab size is large, but the product grains are coarse and the microstructure is uneven; after decades of development, the po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F1/00B22F3/02B22F3/105B22F3/18B22F3/24B21B9/00B21B1/38
CPCY02P10/25
Inventor 段柏华张钊王德志杨栋林
Owner CENT SOUTH UNIV
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