CN103157795A - Preparation method of large-scale molybdenum plate blank - Google Patents

Preparation method of large-scale molybdenum plate blank Download PDF

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Publication number
CN103157795A
CN103157795A CN2013100998579A CN201310099857A CN103157795A CN 103157795 A CN103157795 A CN 103157795A CN 2013100998579 A CN2013100998579 A CN 2013100998579A CN 201310099857 A CN201310099857 A CN 201310099857A CN 103157795 A CN103157795 A CN 103157795A
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punching block
hours
molybdenum
rubber moulding
latex rubber
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CN2013100998579A
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CN103157795B (en
Inventor
曹维成
黄晓玲
张焜
史振琦
薛夏英
葛宽余
白秋平
何晓红
王岗
吴亚利
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Jinduicheng Molybdenum Co Ltd
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Jinduicheng Molybdenum Co Ltd
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Abstract

The invention discloses a preparation method of a large-scale molybdenum plate blank. The preparation method of the large-scale molybdenum plate blank includes five steps: selecting and disposing, filling powder, pressing, demoulding and firing of molybdenum powder. A molybdenum plate blank with a thickness of 65 to 120 millimeters, a width of 500 to 600 millimeters, a length of 900 to 1500 millimeters and a weight more than 500 kilograms can be successfully produced. The molybdenum plate blank is neat in appearance, small in dimensional deviation, not prone to crazing after rolled and even in grain structure. Due to the fact that ultrasound screening is adopted in production process, powder mounding times are reduced, labor intensity is reduced, and production efficiency is improved. Meanwhile, due to the fact that a traditional rubber mold is replaced by soft latex mold, demoulding is enabled to be easy.

Description

The preparation method of large-scale molybdenum plate base
Technical field
The invention belongs to technical field of material, be specifically related to a kind of preparation method of large-scale molybdenum plate base.
Background technology
At present, the specification of the large-scale molybdenum plate base of prior art preparation is mainly substance 100~200kg, and the raw material of molybdenum plate base is generally the pure molybdenum powder of 3.0~3.8 μ m with average Fisher particle size.Adopt powder metallurgic method to produce, its production stage is: at first design steel mold and rubber mold according to the regular size of product requirement, molybdenum powder is quantitatively packed in mould, about 20% the molybdenum powder of often packing into need be measured the molybdenum powder height, if the dress powder height of molybdenum powder surpasses calculated value, need the artificial pier powder, fill again powder after reducing the molybdenum powder height, until quantitatively molybdenum powder is all packed in mould.Suppress putting into isostatic cool pressing equipment after the mould sealing, the molybdenum pressed compact that suppresses is taken out from mould, drop in intermediate frequency furnace and carry out sintering according to the technique that designs, obtain molybdenum plate base finished product, at last the molybdenum plate base is rolled.
Mainly there are the following problems for the preparation method of existing molybdenum plate base: 1, due to the molybdenum powder poor fluidity, conventional molybdenum powder needs repeatedly pier powder in dress powder process, therefore the dress powder density of bottom molybdenum powder will be higher than the mould upper end, thereby causes molybdenum plate base lower end size greater than the upper end; 2, due to needs artificial pier powder repeatedly, cause work larger, and be difficult to produce the molybdenum plate base of the above specification of 200kg; 3, in dress powder process, gauffer easily appears in the rubber mold bottom, causes the empty hole of molybdenum plate base surface appearance and uneven, becomes waste material, needs operating personnel constantly to lift glued membrane; 4, after the compacting, molybdenum plate base pressed compact is due to contraction, and its height is much smaller than mold height, and traditional rubber mold is relatively hard, needs operating personnel to go deep in mould, demoulding rope being tied up to the pressed compact height to locate below 1/3, then pressed compact is hung out, and demoulding difficulty is larger.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of large-scale molybdenum plate base, solved prior art and can't produce the above large-scale molybdenum plate base of 500kg, the problem that molybdenum plate base size is irregular and demoulding difficulty is large.
The technical solution adopted in the present invention is: the preparation method of large-scale molybdenum plate base comprises the steps:
The first step, the choosing and processing of molybdenum powder
Choose particle mean size and be 3.5 μ m~4.5 μ m, pine than being 1.1~1.3g/cm 3Molybdenum powder, carry out the 325 ultrasonic screenings of order, remove the granule molybdenum powder aggregate in molybdenum powder, after screening, the volume of oversize accounts for 6~10% of molybdenum powder cumulative volume before screening;
Second step, the dress powder
Punching block vertically is placed on ground, opening upwards; With hoisting ring, the latex rubber moulding is sling to punching block, then slow decreasing latex rubber moulding is fixedly connected with the latex rubber moulding until during the distance from bottom 10~20mm of the bottom of latex rubber moulding and punching block, stop descending with punching block; The molybdenum powder that handle the first step well this moment is again put into the latex rubber moulding, according to the capacity of latex rubber moulding, then 80%~90% the molybdenum powder of first packing into vibrates punching block, make that molybdenum powder is evenly distributed, consolidation in the latex rubber moulding, then continue to pack into molybdenum powder until the latex rubber moulding be filled;
The 3rd step, die mould
The punching block that second step is installed molybdenum powder is put into cold isostatic press, liquid in cold isostatic press enters punching block inside and the latex rubber moulding is exerted pressure by inlet opening, the rate of rise of cold isostatic press is set to 10~15Mpa/min, the open cold isostatic pressing machine, until the pressure of cold isostatic press when being 185~200Mpa, being suppressed 7~9 minutes, then with 8~10 minutes, cold isostatic press is carried out release, complete die mould, make the molybdenum plate pressed compact;
The 4th step, the demoulding
The punching block after die mould is completed in taking-up, removes the backplate on punching block, makes the latex rubber moulding expose, then will turn under the latex rubber moulding so that the molybdenum plate pressed compact exposes, thereby the exposed portions serve that lifting rope is bundled in the molybdenum plate pressed compact is hung out the molybdenum plate pressed compact;
The 5th step, sintering
The molybdenum plate pressed compact that the 4th step was taken out drops in intermediate frequency furnace, adopts the method for progressively heating that the molybdenum plate pressed compact is heated, and makes the molybdenum plate base.
Characteristics of the present invention also are,
In second step, punching block is the terrace with edge of inner hollow, and the water table opening of punching block is: long 820~840mm, wide 110~175mm; Base square is: long 816~836mm, wide 110~175mm; Be highly: 1400~2200mm, the outer wall of punching block is provided with several inlet openings, and 1/3 At The Height of punching block is provided with backplate along a week of punching block.
In second step, the latex rubber moulding is the terrace with edge of inner hollow, and the water table opening of latex rubber moulding is: long 810~830mm, wide 100~165mm; Base square is: long 806~826mm, wide 100~165mm; Be highly: 1600~2500mm, and the upper base of latex rubber moulding, base square are not more than respectively upper base, the base square of punching block.
The progressively method of heating in the 5th step is: first heat and made furnace temperature rise to 1000 ℃ from room temperature in 6 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1200 ℃ from 1000 ℃ in 3 hours, then be incubated 5 hours; Heat and made furnace temperature rise to 1400 ℃ from 1200 ℃ in 3 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1640 ℃ from 1400 ℃ in 4.5 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1840 ℃ from 1640 ℃ in 4 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1920 ℃ from 1840 ℃ in 3.5 hours, then be incubated 6 hours.
The invention has the beneficial effects as follows: use preparation method of the present invention, can successfully produce thickness 65~120mm, width 500~600mm, length 900~1500mm, the molybdenum plate base finished product of the above specification of substance 500kg, and molybdenum plate base outward appearance is regular, and dimensional discrepancy is little, and rolling rear without cracking, grain structure is even, in production process, adopt ultrasonic screening, reduced pier powder number of times, reduced labour intensity, improve production efficiency, adopted simultaneously soft latex rubber moulding to replace traditional rubber rubber moulding, made the demoulding be more prone to.
Description of drawings
Fig. 1 is the structural representation of punching block in the preparation method of the large-scale molybdenum plate base of the present invention;
Fig. 2 is the structural representation of latex rubber moulding in the preparation method of the large-scale molybdenum plate base of the present invention.
In figure, 1. punching block, 2. inlet opening, 3. backplate, 4. latex rubber moulding.
The specific embodiment
The present invention is described in detail below in conjunction with the specific embodiment.
4 two kinds of structures of punching block 1 and latex rubber moulding have been adopted in preparation method of the present invention.
The structure of punching block 1 disclosed by the invention is: punching block 1 for the terrace with edge of inner hollow, the water table opening of punching block 1 is: long 820~840mm, wide 110~175mm; Base square is: long 816~836mm, wide 110~175mm; Be highly: 1400~2200mm, the outer wall of punching block 1 are provided with several inlet openings 2, and 1/3 At The Height of punching block 1 is provided with backplate 3 along a week of punching block 1.
The structure of latex rubber moulding 4 disclosed by the invention is: latex rubber moulding 4 for the terrace with edge of inner hollow, the water table opening of latex rubber moulding 4 is: long 810~830mm, wide 100~165mm; Base square is: long 806~826mm, wide 100~165mm; Be highly: 1600~2500mm, and the upper base of latex rubber moulding 4, base square are not more than respectively upper base, the base square of punching block 1
Below describe with instantiation:
Embodiment 1
The first step, the choosing and processing of molybdenum powder
Choosing particle mean size is that 4.5 μ m, pine are than being 1.3g/cm 3Molybdenum powder, carry out the 325 ultrasonic screenings of order, remove the granule molybdenum powder aggregate in molybdenum powder, after screening, the volume of oversize accounts for 6% of molybdenum powder cumulative volume before screening;
Second step, the dress powder
Punching block 1 vertically is placed on ground, and the upper base of punching block 1 is long is 820mm, and wide is 110mm, the long 816mm that is that goes to the bottom, and wide is 110mm, the height of punching block 1 is 2200mm; With hoisting ring, latex rubber moulding 4 is sling to punching block 1, wherein the upper base of latex rubber moulding 4 is long is 810mm, and wide is 100mm, the long 806mm that is that goes to the bottom, and wide is 100mm, the height of latex rubber moulding 4 is 2500mm; Slow decreasing latex rubber moulding 4 until during the distance from bottom 15mm of the bottom of latex rubber moulding 4 and punching block 1, stop descending, is fixedly connected with latex rubber moulding 4 with punching block 1 again; The molybdenum powder that handle the first step well this moment is again put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, then 85% the molybdenum powder of first packing into vibrates punching block 1, make that molybdenum powder is evenly distributed, consolidation in latex rubber moulding 4, then continue to pack into molybdenum powder until latex rubber moulding 4 be filled;
The 3rd step, die mould
The punching block 1 that installs molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside and latex rubber moulding 4 is exerted pressure by inlet opening 2, the rate of rise of cold isostatic press is set to 12Mpa/min, the open cold isostatic pressing machine, until the pressure of cold isostatic press when being 185Mpa, being suppressed 9 minutes, then with 10 minutes, cold isostatic press is carried out release, complete die mould, make the molybdenum plate pressed compact;
The 4th step, the demoulding
The punching block 1 after die mould is completed in taking-up, removes the backplate 3 on punching block 1, makes latex rubber moulding 4 expose, then the latex rubber moulding is turned over for 4 times so that the molybdenum plate pressed compact exposes, thereby the exposed portions serve that lifting rope is bundled in the molybdenum plate pressed compact is hung out the molybdenum plate pressed compact;
The 5th step, sintering
The molybdenum plate pressed compact that the 4th step was taken out drops in intermediate frequency furnace, first heats to make furnace temperature rise to 1000 ℃ from room temperature in 6 hours, then is incubated 4 hours; Heat and made furnace temperature rise to 1200 ℃ from 1000 ℃ in 3 hours, then be incubated 5 hours; Heat and made furnace temperature rise to 1400 ℃ from 1200 ℃ in 3 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1640 ℃ from 1400 ℃ in 4.5 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1840 ℃ from 1640 ℃ in 4 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1900 ℃ from 1840 ℃ in 3.5 hours, then be incubated 6 hours, then take out, making length is 1500mm, and width is 530mm, and thickness is the molybdenum plate base of 70mm.
The design of terrace with edge shape mould is in order to offset because molybdenum powder deadweight is excessive, and is thin thick under the base substrate that causes to deposit in preparation process, to guarantee that final molybdenum plate base is as the uniform cuboid of appearance and size.
The prepared molybdenum plate base of the present embodiment, through detecting, outward appearance is regular, length is 1500(+5/-5) mm, and width is 530(+5/-5) mm, thickness is 70(+2/-2) mm; The density of molybdenum plate base reaches 9.7g/cm 3, substance is 540kg, and molybdenum plate base interior tissue is even, and it is that 4 grades of number of die are 2000/mm that metallographic detects molybdenum plate base section grain size 2Detect inner flawless, zero defect through ultrasonic examination, best in quality.
Embodiment 2
The first step, the choosing and processing of molybdenum powder
Choosing particle mean size is that 4.2 μ m, pine are than being 1.28g/cm 3Molybdenum powder, carry out the 325 ultrasonic screenings of order, remove the granule molybdenum powder aggregate in molybdenum powder, after screening, the volume of oversize accounts for 8% of molybdenum powder cumulative volume before screening;
Second step, the dress powder
Punching block 1 vertically is placed on ground, and the upper base of punching block 1 is long is 840mm, and wide is 175mm, the long 836mm that is that goes to the bottom, and wide is 175mm, the height of punching block 1 is 1400mm; With hoisting ring, 1 latex rubber moulding 4 is sling to punching block 1, wherein the upper base of latex rubber moulding 4 is long is 830mm, and wide is 165mm, the long 826mm that is that goes to the bottom, and wide is 165mm, the height of latex rubber moulding 4 is 1600mm; Slow decreasing latex rubber moulding 4 until during the distance from bottom 12mm of the bottom of latex rubber moulding 4 and punching block 1, stop descending, is fixedly connected with latex rubber moulding 4 with punching block 1 again; The molybdenum powder that handle the first step well this moment is again put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, then 90% the molybdenum powder of first packing into vibrates punching block 1, make that molybdenum powder is evenly distributed, consolidation in latex rubber moulding 4, then continue to pack into molybdenum powder until latex rubber moulding 4 be filled;
The 3rd step, die mould
The punching block 1 that installs molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside and latex rubber moulding 4 is exerted pressure by inlet opening 2, the rate of rise of cold isostatic press is set to 15Mpa/min, the open cold isostatic pressing machine, until the pressure of cold isostatic press when being 190Mpa, being suppressed 9 minutes, then with 8 minutes, cold isostatic press is carried out release, complete die mould, make the molybdenum plate pressed compact;
The 4th step, the demoulding
The punching block 1 after die mould is completed in taking-up, removes the backplate 3 on punching block 1, makes latex rubber moulding 4 expose, then the latex rubber moulding is turned over for 4 times so that the molybdenum plate pressed compact exposes, thereby the exposed portions serve that lifting rope is bundled in the molybdenum plate pressed compact is hung out the molybdenum plate pressed compact;
The 5th step, sintering
The molybdenum plate pressed compact that the 4th step was taken out drops in intermediate frequency furnace, first heats to make furnace temperature rise to 1000 ℃ from room temperature in 6 hours, then is incubated 4 hours; Heat and made furnace temperature rise to 1200 ℃ from 1000 ℃ in 3 hours, then be incubated 5 hours; Heat and made furnace temperature rise to 1400 ℃ from 1200 ℃ in 3 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1640 ℃ from 1400 ℃ in 4.5 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1840 ℃ from 1640 ℃ in 4 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1900 ℃ from 1840 ℃ in 3.5 hours, then be incubated 6 hours, then take out, making length is 950mm, and width is 555mm, and thickness is the molybdenum plate base of 115mm.
The design of terrace with edge shape mould is in order to offset because molybdenum powder deadweight is excessive, and is thin thick under the base substrate that causes to deposit in preparation process, to guarantee that final molybdenum plate base is as the uniform cuboid of appearance and size.
The prepared molybdenum plate base of the present embodiment, through detecting, outward appearance is regular, length is 950(+5/-5) mm, and width is 555(+5/-5) mm, thickness is 115(+2/-2) mm; The density of molybdenum plate base reaches 9.82g/cm 3, substance is 595kg, and molybdenum plate base interior tissue is even, and it is that 4 grades of number of die are 2000/mm that metallographic detects molybdenum plate base section grain size 2Detect inner flawless, zero defect through ultrasonic examination, best in quality.
Embodiment 3
The first step, the choosing and processing of molybdenum powder
Choosing particle mean size is that 4.0 μ m, pine are than being 1.2g/cm 3Molybdenum powder, carry out the 325 ultrasonic screenings of order, remove the granule molybdenum powder aggregate in molybdenum powder, after screening, the volume of oversize accounts for 7% of molybdenum powder cumulative volume before screening;
Second step, the dress powder
Punching block 1 vertically is placed on ground, and the upper base of punching block 1 is long is 820mm, and wide is 110mm, the long 816mm that is that goes to the bottom, and wide is 110mm, the height of punching block 1 is 2200mm; With hoisting ring, latex rubber moulding 4 is sling to punching block 1, wherein the upper base of latex rubber moulding 4 is long is 810mm, and wide is 100mm, the long 806mm that is that goes to the bottom, and wide is 100mm, the height of latex rubber moulding 4 is 2500mm; Slow decreasing latex rubber moulding 4 until during the distance from bottom 15mm of the bottom of latex rubber moulding 4 and punching block 1, stop descending, is fixedly connected with latex rubber moulding 4 with punching block 1 again; The molybdenum powder that handle the first step well this moment is again put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, then 85% the molybdenum powder of first packing into vibrates punching block 1, make that molybdenum powder is evenly distributed, consolidation in latex rubber moulding 4, then continue to pack into molybdenum powder until latex rubber moulding 4 be filled;
The 3rd step, die mould
The punching block 1 that installs molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside and latex rubber moulding 4 is exerted pressure by inlet opening 2, the rate of rise of cold isostatic press is set to 10Mpa/min, the open cold isostatic pressing machine, until the pressure of cold isostatic press when being 190Mpa, being suppressed 7 minutes, then with 9 minutes, cold isostatic press is carried out release, complete die mould, make the molybdenum plate pressed compact;
The 4th step, the demoulding
The punching block 1 after die mould is completed in taking-up, removes the backplate 3 on punching block 1, makes latex rubber moulding 4 expose, then the latex rubber moulding is turned over for 4 times so that the molybdenum plate pressed compact exposes, thereby the exposed portions serve that lifting rope is bundled in the molybdenum plate pressed compact is hung out the molybdenum plate pressed compact;
The 5th step, sintering
The molybdenum plate pressed compact that the 4th step was taken out drops in intermediate frequency furnace, first heats to make furnace temperature rise to 1000 ℃ from room temperature in 6 hours, then is incubated 4 hours; Heat and made furnace temperature rise to 1200 ℃ from 1000 ℃ in 3 hours, then be incubated 5 hours; Heat and made furnace temperature rise to 1400 ℃ from 1200 ℃ in 3 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1640 ℃ from 1400 ℃ in 4.5 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1840 ℃ from 1640 ℃ in 4 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1900 ℃ from 1840 ℃ in 3.5 hours, then be incubated 6 hours, then take out, making length is 1505mm, and width is 520mm, and thickness is the molybdenum plate base of 68mm.
The design of terrace with edge shape mould is in order to offset because molybdenum powder deadweight is excessive, and is thin thick under the base substrate that causes to deposit in preparation process, to guarantee that final molybdenum plate base is as the uniform cuboid of appearance and size.
The prepared molybdenum plate base of the present embodiment, through detecting, outward appearance is regular, length is 1505(+5/-5) mm, and width is 520(+5/-5) mm, thickness is 68(+2/-2) mm; The density of molybdenum plate base reaches 9.87g/cm 3, substance is 525kg, and molybdenum plate base interior tissue is even, and it is that 3 grades of number of die are 1500/mm that metallographic detects molybdenum plate base section grain size 2Detect inner flawless, zero defect through ultrasonic examination, best in quality.
Embodiment 4
The first step, the choosing and processing of molybdenum powder
Choosing particle mean size is that 3.8 μ m, pine are than being 1.16g/cm 3Molybdenum powder, carry out the 325 ultrasonic screenings of order, remove the granule molybdenum powder aggregate in molybdenum powder, after screening, the volume of oversize accounts for 9% of molybdenum powder cumulative volume before screening;
Second step, the dress powder
Punching block 1 vertically is placed on ground, and the upper base of punching block 1 is long is 830mm, and wide is 165mm, the long 826mm that is that goes to the bottom, and wide is 165mm, the height of punching block is 1700mm; With hoisting ring, latex rubber moulding 4 is sling to punching block 1, wherein the upper base of latex rubber moulding 4 is long is 820mm, and wide is 155mm, the long 816mm that is that goes to the bottom, and wide is 155mm, the height of latex rubber moulding 4 is 1900mm; Slow decreasing latex rubber moulding 4 until during the distance from bottom 10mm of the bottom of latex rubber moulding 4 and punching block 1, stop descending, is fixedly connected with latex rubber moulding 4 with punching block 1 again; The molybdenum powder that handle the first step well this moment is again put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, then 80% the molybdenum powder of first packing into vibrates punching block 1, make that molybdenum powder is evenly distributed, consolidation in latex rubber moulding 4, then continue to pack into molybdenum powder until latex rubber moulding 4 be filled;
The 3rd step, die mould
The punching block 1 that installs molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside and latex rubber moulding 4 is exerted pressure by inlet opening 2, the rate of rise of cold isostatic press is set to 15Mpa/min, the open cold isostatic pressing machine, until the pressure of cold isostatic press when being 195Mpa, being suppressed 8 minutes, then with 10 minutes, cold isostatic press is carried out release, complete die mould, make the molybdenum plate pressed compact;
The 4th step, the demoulding
The punching block 1 after die mould is completed in taking-up, removes the backplate 3 on punching block 1, makes latex rubber moulding 4 expose, then the latex rubber moulding is turned over for 4 times so that the molybdenum plate pressed compact exposes, thereby the exposed portions serve that lifting rope is bundled in the molybdenum plate pressed compact is hung out the molybdenum plate pressed compact;
The 5th step, sintering
The molybdenum plate pressed compact that the 4th step was taken out drops in intermediate frequency furnace, first heats to make furnace temperature rise to 1000 ℃ from room temperature in 6 hours, then is incubated 4 hours; Heat and made furnace temperature rise to 1200 ℃ from 1000 ℃ in 3 hours, then be incubated 5 hours; Heat and made furnace temperature rise to 1400 ℃ from 1200 ℃ in 3 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1640 ℃ from 1400 ℃ in 4.5 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1840 ℃ from 1640 ℃ in 4 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1900 ℃ from 1840 ℃ in 3.5 hours, then be incubated 6 hours, then take out, making length is 960mm, and width is 545mm, and thickness is the molybdenum plate base of 115mm.
The design of terrace with edge shape mould is in order to offset because molybdenum powder deadweight is excessive, and is thin thick under the base substrate that causes to deposit in preparation process, to guarantee that final molybdenum plate base is as the uniform cuboid of appearance and size.
The prepared molybdenum plate base of the present embodiment, through detecting, outward appearance is regular, length is 1060(+5/-5) mm, and width is 545(+5/-5) mm, thickness is 105(+2/-2) mm; The density of molybdenum plate base reaches 9.76g/cm 3, substance is 592kg, and molybdenum plate base interior tissue is even, and it is that 4 grades of number of die are 2000/mm that metallographic detects molybdenum plate base section grain size 2Detect inner flawless, zero defect through ultrasonic examination, best in quality.
Embodiment 5
The first step, the choosing and processing of molybdenum powder
Choosing particle mean size is that 3.5 μ m, pine are than being 1.10g/cm 3Molybdenum powder, carry out the 325 ultrasonic screenings of order, remove the granule molybdenum powder aggregate in molybdenum powder, after screening, the volume of oversize accounts for 10% of molybdenum powder cumulative volume before screening;
Second step, the dress powder
Punching block 1 vertically is placed on ground, and the upper base of punching block 1 is long is 840mm, and wide is 175mm, the long 836mm that is that goes to the bottom, and wide is 175mm, the height of punching block 1 is 1400mm; With hoisting ring, latex rubber moulding 4 is sling to punching block 1, wherein the upper base of latex rubber moulding 4 is long is 830mm, and wide is 165mm, the long 826mm that is that goes to the bottom, and wide is 165mm, the height of latex rubber moulding 4 is 1600mm; Slow decreasing latex rubber moulding 4 until during the distance from bottom 15mm of the bottom of latex rubber moulding 4 and punching block 1, stop descending, is fixedly connected with latex rubber moulding 4 with punching block 1 again; The molybdenum powder that handle the first step well this moment is again put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, then 85% the molybdenum powder of first packing into vibrates punching block 1, make that molybdenum powder is evenly distributed, consolidation in latex rubber moulding 4, then continue to pack into molybdenum powder until latex rubber moulding 4 be filled;
The 3rd step, die mould
The punching block 1 that installs molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside and latex rubber moulding 4 is exerted pressure by inlet opening 2, the rate of rise of cold isostatic press is set to 15Mpa/min, the open cold isostatic pressing machine, until the pressure of cold isostatic press when being 200Mpa, being suppressed 7 minutes, then with 8 minutes, cold isostatic press is carried out release, complete die mould, make the molybdenum plate pressed compact;
The 4th step, the demoulding
The punching block 1 after die mould is completed in taking-up, removes the backplate 3 on punching block 1, makes latex rubber moulding 4 expose, then the latex rubber moulding is turned over for 4 times so that the molybdenum plate pressed compact exposes, thereby the exposed portions serve that lifting rope is bundled in the molybdenum plate pressed compact is hung out the molybdenum plate pressed compact;
The 5th step, sintering
The molybdenum plate pressed compact that the 4th step was taken out drops in intermediate frequency furnace, first heats to make furnace temperature rise to 1000 ℃ from room temperature in 6 hours, then is incubated 4 hours; Heat and made furnace temperature rise to 1200 ℃ from 1000 ℃ in 3 hours, then be incubated 5 hours; Heat and made furnace temperature rise to 1400 ℃ from 1200 ℃ in 3 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1640 ℃ from 1400 ℃ in 4.5 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1840 ℃ from 1640 ℃ in 4 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1900 ℃ from 1840 ℃ in 3.5 hours, then be incubated 6 hours, then take out, making length is 980mm, and width is 530mm, and thickness is the molybdenum plate base of 110mm.
The design of terrace with edge shape mould is in order to offset because molybdenum powder deadweight is excessive, and is thin thick under the base substrate that causes to deposit in preparation process, to guarantee that final molybdenum plate base is as the uniform cuboid of appearance and size.
The prepared molybdenum plate base of the present embodiment, through detecting, outward appearance is regular, length is 980(+5/-5) mm, and width is 530(+5/-5) mm, thickness is 110(+2/-2) mm; The density of molybdenum plate base reaches 9.84g/cm 3, substance is 562kg, and molybdenum plate base interior tissue is even, and it is that 4 grades of number of die are 2000/mm that metallographic detects molybdenum plate base section grain size 2Detect inner flawless, zero defect through ultrasonic examination, best in quality.
The above; it is only preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, every any simple modification, change and equivalent structure of above embodiment being done according to the technology of the present invention essence changes, and all still belongs in the protection domain of technical solution of the present invention.

Claims (4)

1. the preparation method of large-scale molybdenum plate base, is characterized in that, comprises the steps:
The first step, the choosing and processing of molybdenum powder
Choose particle mean size and be 3.5 μ m~4.5 μ m, pine than being 1.1~1.3g/cm 3Molybdenum powder, carry out the 325 ultrasonic screenings of order, remove the granule molybdenum powder aggregate in molybdenum powder, after screening, the volume of oversize accounts for 6~10% of molybdenum powder cumulative volume before screening;
Second step, the dress powder
Punching block (1) vertically is placed on ground, opening upwards; With hoisting ring, latex rubber moulding (4) is sling to punching block, slow decreasing latex rubber moulding (4) is until during the distance from bottom 10~20mm of the bottom of latex rubber moulding (4) and punching block (1) again, stop descending, latex rubber moulding (4) is fixedly connected with described punching block (1); The molybdenum powder that handle the first step well this moment is again put into latex rubber moulding (4), capacity according to latex rubber moulding (4), first pack into 80%~90% molybdenum powder, then vibrate described punching block (1), make that molybdenum powder is evenly distributed, consolidation in latex rubber moulding (4), then continue to pack into molybdenum powder until latex rubber moulding (4) be filled;
The 3rd step, die mould
The described punching block (1) that second step is installed molybdenum powder is put into cold isostatic press, liquid in cold isostatic press enters punching block (1) inside and latex rubber moulding (4) is exerted pressure by inlet opening (2), the rate of rise of cold isostatic press is set to 10~15Mpa/min, the open cold isostatic pressing machine, until the pressure of cold isostatic press when being 185~200Mpa, being suppressed 7~9 minutes, then with 8~10 minutes, cold isostatic press is carried out release, complete die mould, make the molybdenum plate pressed compact;
The 4th step, the demoulding
The described punching block (1) after die mould is completed in taking-up, remove the backplate (3) on punching block (1), make latex rubber moulding (4) expose, then will turn over so that the molybdenum plate pressed compact exposes under latex rubber moulding (4), thereby the exposed portions serve that lifting rope is bundled in the molybdenum plate pressed compact is hung out the molybdenum plate pressed compact;
The 5th step, sintering
The molybdenum plate pressed compact that the 4th step was taken out drops in intermediate frequency furnace, adopts the method for progressively heating that the molybdenum plate pressed compact is heated, and makes the molybdenum plate base.
2. the preparation method of large-scale molybdenum plate base as claimed in claim 1, is characterized in that, punching block described in second step (1) is the terrace with edge of inner hollow, and the water table opening of described punching block (1) is: long 820~840mm, wide 110~175mm; Base square is: long 816~836mm, wide 110~175mm; Be highly: 1400~2200mm, the outer wall of described punching block (1) is provided with several inlet openings (2), and 1/3 At The Height of described punching block (1) is provided with backplate (3) week along described punching block (1).
3. the preparation method of large-scale molybdenum plate base as claimed in claim 1 or 2, is characterized in that, the rubber moulding of latex described in second step (4) is the terrace with edge of inner hollow, and the water table opening of described latex rubber moulding (4) is: long 810~830mm, wide 100~165mm; Base square is: long 806~826mm, wide 100~165mm; Be highly: 1600~2500mm, and the upper base of described latex rubber moulding (4), base square are not more than respectively upper base, the base square of described punching block (1).
4. the preparation method of large-scale molybdenum plate base as claimed in claim 1, is characterized in that, the progressively method of heating described in the 5th step is: first heat and made furnace temperature rise to 1000 ℃ from room temperature in 6 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1200 ℃ from 1000 ℃ in 3 hours, then be incubated 5 hours; Heat and made furnace temperature rise to 1400 ℃ from 1200 ℃ in 3 hours, then be incubated 4 hours; Heat and made furnace temperature rise to 1640 ℃ from 1400 ℃ in 4.5 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1840 ℃ from 1640 ℃ in 4 hours, then be incubated 6 hours; Heat and made furnace temperature rise to 1920 ℃ from 1840 ℃ in 3.5 hours, then be incubated 6 hours.
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CN104001913A (en) * 2014-05-29 2014-08-27 金堆城钼业股份有限公司 Press piece type sealing device and method for manufacturing large molybdenum crucible
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CN105195743A (en) * 2014-06-13 2015-12-30 北京矿冶研究总院 Preparation method of large single-weight tungsten plate blank or molybdenum plate blank
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CN101559491A (en) * 2009-05-25 2009-10-21 西安宝德粉末冶金有限责任公司 Integral molding die of large scale sintering porous cone pipe and isotropic molding method therewith
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Publication number Priority date Publication date Assignee Title
CN104001913A (en) * 2014-05-29 2014-08-27 金堆城钼业股份有限公司 Press piece type sealing device and method for manufacturing large molybdenum crucible
CN105195743A (en) * 2014-06-13 2015-12-30 北京矿冶研究总院 Preparation method of large single-weight tungsten plate blank or molybdenum plate blank
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
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CN109894472A (en) * 2019-03-14 2019-06-18 安泰天龙钨钼科技有限公司 A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate
CN115106526A (en) * 2022-06-27 2022-09-27 金堆城钼业股份有限公司 Cold isostatic pressing precision forming device and method for molybdenum material plate blank
CN115106526B (en) * 2022-06-27 2024-06-04 金堆城钼业股份有限公司 Cold isostatic pressing accurate forming device and method for molybdenum material plate blank

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