CN103157795B - Preparation method of large-scale molybdenum plate blank - Google Patents
Preparation method of large-scale molybdenum plate blank Download PDFInfo
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- CN103157795B CN103157795B CN201310099857.9A CN201310099857A CN103157795B CN 103157795 B CN103157795 B CN 103157795B CN 201310099857 A CN201310099857 A CN 201310099857A CN 103157795 B CN103157795 B CN 103157795B
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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
Technical field
The invention belongs to technical field of material, be specifically related to a kind of preparation method of large-scale molybdenum plate blank.
Background technology
At present, the specification of large-scale molybdenum plate blank prepared by prior art is mainly substance 100 ~ 200kg, and the raw material of molybdenum plate blank is generally the pure molybdenum powder of 3.0 ~ 3.8 μm by average Fisher particle size.Powder metallurgic method is adopted to produce, its production stage is: first design steel mold and rubber mold according to the regular size of product requirement, molybdenum powder is quantitatively loaded in mould, the molybdenum powder often loading about 20% need measure molybdenum powder height, if the dress powder height of molybdenum powder exceedes calculated value, then need artificial pier powder, after reducing molybdenum powder height, carry out dress powder again, until quantitatively molybdenum powder all loads in mould.Put into isostatic cool pressing equipment after being sealed by mould to suppress, the molybdenum pressed compact suppressed is taken out from mould, drop in intermediate frequency furnace and sinter according to the technique designed, obtain molybdenum plate blank finished product, finally molybdenum plate blank is rolled.
Mainly there are the following problems for the preparation method of existing molybdenum plate blank: 1, due to molybdenum powder poor fluidity, conventional molybdenum powder needs repeatedly pier powder in dress powder process, therefore the dress powder density of bottom molybdenum powder is higher than mould upper end, thus causes molybdenum plate blank lower end size to be greater than upper end; 2, due to needs repeatedly artificial pier powder, cause work comparatively large, and be difficult to the molybdenum plate blank producing more than 200kg specification; 3, fill in powder process and easily occur gauffer bottom rubber mold, cause molybdenum plate blank surface to occur becoming empty hole and uneven waste material, need operating personnel constantly to lift glued membrane; 4, after compacting, molybdenum plate blank pressed compact is owing to shrinking, and its height is much smaller than mold height, and conventional rubber mould is relatively hard, needs operating personnel to go deep in mould, demoulding rope being tied up to pressed compact height less than 1/3 to locate, then is hung out by pressed compact, 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 blank, solve prior art and cannot produce the large-scale molybdenum plate blank of more than 500kg, molybdenum plate blank size is irregular and demoulding difficulty is large problem.
The technical solution adopted in the present invention is: the preparation method of large-scale molybdenum plate blank, comprises the steps:
The first step, choosing and process of molybdenum powder
Choose that particle mean size is 3.5 μm ~ 4.5 μm, pine is than being 1.1 ~ 1.3g/cm
3molybdenum powder, carry out the ultrasonic screening of 325 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, dress powder
Punching block is vertically placed on ground, opening upwards; With hoisting ring, latex rubber moulding is sling to punching block, more slowly decline latex rubber moulding until the distance from bottom 10 ~ 20mm of the bottom of latex rubber moulding and punching block time, stop declining, latex rubber moulding be fixedly connected with punching block; Now again the molybdenum powder that the first step is handled well is put into latex rubber moulding, according to the capacity of latex rubber moulding, first load the molybdenum powder of 80% ~ 90%, then vibrate punching block, make that molybdenum powder is evenly distributed in latex rubber moulding, consolidation, then continue to load molybdenum powder until latex rubber moulding is filled;
3rd step, die mould
Punching block second step being installed molybdenum powder puts into cold isostatic press, liquid in cold isostatic press enters punching block inside by inlet opening and applies pressure to latex rubber moulding, the rate of rise of cold isostatic press is set to 10 ~ 15Mpa/min, open cold isostatic pressing machine, until when the pressure of cold isostatic press is 185 ~ 200Mpa, suppresses 7 ~ 9 minutes, then with 8 ~ 10 minutes, release is carried out to cold isostatic press, complete die mould, obtained molybdenum plate pressed compact;
4th step, the demoulding
Take out the punching block after die mould, removed the backplate on punching block, latex rubber moulding is exposed, then by turning under latex rubber moulding, molybdenum plate pressed compact is exposed, lifting rope be bundled in the exposed portion of molybdenum plate pressed compact thus hang out molybdenum plate pressed compact;
5th step, sintering
The molybdenum plate pressed compact 4th step taken out drops in intermediate frequency furnace, adopts the method progressively heated to heat molybdenum plate pressed compact, obtained molybdenum plate blank.
Feature of the present invention is also,
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 that the outer wall of punching block is provided with several inlet openings, 1/3 At The Height of punching block is provided with backplate in one week along punching block.
In second step, 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 upper base, the base square of punching block respectively.
The method progressively heated in 5th step is: first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 DEG C from 1840 DEG C, 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 blank finished product of the above specification of substance 500kg, and molybdenum plate blank outward appearance is regular, and dimensional discrepancy is little, and without cracking after rolling, grain structure is even, in production process, adopt ultrasonic screening, decrease pier powder number of times, reduce labour intensity, improve production efficiency, adopt soft latex rubber moulding to replace traditional rubber rubber moulding simultaneously, the demoulding is more prone to.
Accompanying drawing explanation
Fig. 1 is the structural representation of punching block in the preparation method of large-scale molybdenum plate blank of the present invention;
Fig. 2 is the structural representation of latex rubber moulding in the preparation method of large-scale molybdenum plate blank of the present invention.
In figure, 1. punching block, 2. inlet opening, 3. backplate, 4. latex rubber moulding.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
Have employed punching block 1 and latex rubber moulding 4 two kinds of structures in preparation method of the present invention.
The structure of punching block 1 disclosed by the invention is: punching block 1 is the terrace with edge of inner hollow, and 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 that the outer wall of punching block 1 is provided with several inlet openings 2,1/3 At The Height of punching block 1 is provided with backplate 3 in one week along punching block 1.
The structure of latex rubber moulding 4 disclosed by the invention is: latex rubber moulding 4 is the terrace with edge of inner hollow, and 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 upper base, the base square of punching block 1 respectively
Be described with instantiation below:
Embodiment 1
The first step, choosing and process of molybdenum powder
Choose that particle mean size is 4.5 μm, pine is than being 1.3g/cm
3molybdenum powder, carry out the ultrasonic screening of 325 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, dress powder
Punching block 1 is vertically placed on ground, and the upper base of punching block 1 is long is 820mm, and wide is 110mm, and going to the bottom long is 816mm, and wide is 110mm, and the height of punching block 1 is 2200mm; Sling with hoisting ring to punching block 1 by latex rubber moulding 4, wherein the upper base of latex rubber moulding 4 is long is 810mm, and wide is 100mm, and going to the bottom long is 806mm, and wide is 100mm, and the height of latex rubber moulding 4 is 2500mm; Again slowly decline latex rubber moulding 4 until the distance from bottom 15mm of the bottom of latex rubber moulding 4 and punching block 1 time, stop declining, latex rubber moulding 4 be fixedly connected with punching block 1; Now again the molybdenum powder that the first step is handled well is put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, first load the molybdenum powder of 85%, then vibrate punching block 1, make that molybdenum powder is evenly distributed in latex rubber moulding 4, consolidation, then continue to load molybdenum powder until latex rubber moulding 4 is filled;
3rd step, die mould
The punching block 1 installing molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside by inlet opening 2 and applies pressure to latex rubber moulding 4, the rate of rise of cold isostatic press is set to 12Mpa/min, open cold isostatic pressing machine, until when the pressure of cold isostatic press is 185Mpa, suppresses 9 minutes, then with 10 minutes, release is carried out to cold isostatic press, complete die mould, obtained molybdenum plate pressed compact;
4th step, the demoulding
Take out the punching block after die mould 1, removed the backplate 3 on punching block 1, latex rubber moulding 4 is exposed, then latex rubber moulding is turned over for 4 times molybdenum plate pressed compact is exposed, lifting rope be bundled in the exposed portion of molybdenum plate pressed compact thus hang out molybdenum plate pressed compact;
5th step, sintering
The molybdenum plate pressed compact 4th step taken out drops in intermediate frequency furnace, and first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1900 DEG C from 1840 DEG C, then be incubated 6 hours, then take out, obtained length is 1500mm, and width is 530mm, and thickness is the molybdenum plate blank of 70mm.
The design of prismatic table shape mould is to offset because molybdenum powder deadweight is excessive, depositing the base substrate lower thick upper thin caused downwards, to ensure that final molybdenum plate blank is for the uniform cuboid of appearance and size in preparation process.
Molybdenum plate blank obtained by the present embodiment, through detecting, outward appearance is regular, and length is 1500(+5/-5) mm, width is 530(+5/-5) mm, thickness is 70(+2/-2) mm; The density of molybdenum plate blank reaches 9.7g/cm
3, substance is 540kg, and molybdenum plate blank interior tissue is even, and metallographic detection molybdenum plate blank section grain size is 4 grades of number of die is 2000/mm
2; Inner flawless, zero defect is detected through ultrasonic examination, best in quality.
Embodiment 2
The first step, choosing and process of molybdenum powder
Choose that particle mean size is 4.2 μm, pine is than being 1.28g/cm
3molybdenum powder, carry out the ultrasonic screening of 325 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, dress powder
Punching block 1 is vertically placed on ground, and the upper base of punching block 1 is long is 840mm, and wide is 175mm, and going to the bottom long is 836mm, and wide is 175mm, and the height of punching block 1 is 1400mm; Sling with hoisting ring to punching block 1 by 1 latex rubber moulding 4, wherein the upper base of latex rubber moulding 4 is long is 830mm, and wide is 165mm, and going to the bottom long is 826mm, and wide is 165mm, and the height of latex rubber moulding 4 is 1600mm; Again slowly decline latex rubber moulding 4 until the distance from bottom 12mm of the bottom of latex rubber moulding 4 and punching block 1 time, stop declining, latex rubber moulding 4 be fixedly connected with punching block 1; Now again the molybdenum powder that the first step is handled well is put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, first load the molybdenum powder of 90%, then vibrate punching block 1, make that molybdenum powder is evenly distributed in latex rubber moulding 4, consolidation, then continue to load molybdenum powder until latex rubber moulding 4 is filled;
3rd step, die mould
The punching block 1 installing molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside by inlet opening 2 and applies pressure to latex rubber moulding 4, the rate of rise of cold isostatic press is set to 15Mpa/min, open cold isostatic pressing machine, until when the pressure of cold isostatic press is 190Mpa, suppresses 9 minutes, then with 8 minutes, release is carried out to cold isostatic press, complete die mould, obtained molybdenum plate pressed compact;
4th step, the demoulding
Take out the punching block after die mould 1, removed the backplate 3 on punching block 1, latex rubber moulding 4 is exposed, then latex rubber moulding is turned over for 4 times molybdenum plate pressed compact is exposed, lifting rope be bundled in the exposed portion of molybdenum plate pressed compact thus hang out molybdenum plate pressed compact;
5th step, sintering
The molybdenum plate pressed compact 4th step taken out drops in intermediate frequency furnace, and first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1900 DEG C from 1840 DEG C, then be incubated 6 hours, then take out, obtained length is 950mm, and width is 555mm, and thickness is the molybdenum plate blank of 115mm.
The design of prismatic table shape mould is to offset because molybdenum powder deadweight is excessive, depositing the base substrate lower thick upper thin caused downwards, to ensure that final molybdenum plate blank is for the uniform cuboid of appearance and size in preparation process.
Molybdenum plate blank obtained by the present embodiment, through detecting, outward appearance is regular, and length is 950(+5/-5) mm, width is 555(+5/-5) mm, thickness is 115(+2/-2) mm; The density of molybdenum plate blank reaches 9.82g/cm
3, substance is 595kg, and molybdenum plate blank interior tissue is even, and metallographic detection molybdenum plate blank section grain size is 4 grades of number of die is 2000/mm
2; Inner flawless, zero defect is detected through ultrasonic examination, best in quality.
Embodiment 3
The first step, choosing and process of molybdenum powder
Choose that particle mean size is 4.0 μm, pine is than being 1.2g/cm
3molybdenum powder, carry out the ultrasonic screening of 325 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, dress powder
Punching block 1 is vertically placed on ground, and the upper base of punching block 1 is long is 820mm, and wide is 110mm, and going to the bottom long is 816mm, and wide is 110mm, and the height of punching block 1 is 2200mm; Sling with hoisting ring to punching block 1 by latex rubber moulding 4, wherein the upper base of latex rubber moulding 4 is long is 810mm, and wide is 100mm, and going to the bottom long is 806mm, and wide is 100mm, and the height of latex rubber moulding 4 is 2500mm; Again slowly decline latex rubber moulding 4 until the distance from bottom 15mm of the bottom of latex rubber moulding 4 and punching block 1 time, stop declining, latex rubber moulding 4 be fixedly connected with punching block 1; Now again the molybdenum powder that the first step is handled well is put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, first load the molybdenum powder of 85%, then vibrate punching block 1, make that molybdenum powder is evenly distributed in latex rubber moulding 4, consolidation, then continue to load molybdenum powder until latex rubber moulding 4 is filled;
3rd step, die mould
The punching block 1 installing molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside by inlet opening 2 and applies pressure to latex rubber moulding 4, the rate of rise of cold isostatic press is set to 10Mpa/min, open cold isostatic pressing machine, until when the pressure of cold isostatic press is 190Mpa, suppresses 7 minutes, then with 9 minutes, release is carried out to cold isostatic press, complete die mould, obtained molybdenum plate pressed compact;
4th step, the demoulding
Take out the punching block after die mould 1, removed the backplate 3 on punching block 1, latex rubber moulding 4 is exposed, then latex rubber moulding is turned over for 4 times molybdenum plate pressed compact is exposed, lifting rope be bundled in the exposed portion of molybdenum plate pressed compact thus hang out molybdenum plate pressed compact;
5th step, sintering
The molybdenum plate pressed compact 4th step taken out drops in intermediate frequency furnace, and first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1900 DEG C from 1840 DEG C, then be incubated 6 hours, then take out, obtained length is 1505mm, and width is 520mm, and thickness is the molybdenum plate blank of 68mm.
The design of prismatic table shape mould is to offset because molybdenum powder deadweight is excessive, depositing the base substrate lower thick upper thin caused downwards, to ensure that final molybdenum plate blank is for the uniform cuboid of appearance and size in preparation process.
Molybdenum plate blank obtained by the present embodiment, through detecting, outward appearance is regular, and length is 1505(+5/-5) mm, width is 520(+5/-5) mm, thickness is 68(+2/-2) mm; The density of molybdenum plate blank reaches 9.87g/cm
3, substance is 525kg, and molybdenum plate blank interior tissue is even, and metallographic detection molybdenum plate blank section grain size is 3 grades of number of die is 1500/mm
2; Inner flawless, zero defect is detected through ultrasonic examination, best in quality.
Embodiment 4
The first step, choosing and process of molybdenum powder
Choose that particle mean size is 3.8 μm, pine is than being 1.16g/cm
3molybdenum powder, carry out the ultrasonic screening of 325 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, dress powder
Punching block 1 is vertically placed on ground, and the upper base of punching block 1 is long is 830mm, and wide is 165mm, and going to the bottom long is 826mm, and wide is 165mm, and the height of punching block is 1700mm; Sling with hoisting ring to punching block 1 by latex rubber moulding 4, wherein the upper base of latex rubber moulding 4 is long is 820mm, and wide is 155mm, and going to the bottom long is 816mm, and wide is 155mm, and the height of latex rubber moulding 4 is 1900mm; Again slowly decline latex rubber moulding 4 until the distance from bottom 10mm of the bottom of latex rubber moulding 4 and punching block 1 time, stop declining, latex rubber moulding 4 be fixedly connected with punching block 1; Now again the molybdenum powder that the first step is handled well is put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, first load the molybdenum powder of 80%, then vibrate punching block 1, make that molybdenum powder is evenly distributed in latex rubber moulding 4, consolidation, then continue to load molybdenum powder until latex rubber moulding 4 is filled;
3rd step, die mould
The punching block 1 installing molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside by inlet opening 2 and applies pressure to latex rubber moulding 4, the rate of rise of cold isostatic press is set to 15Mpa/min, open cold isostatic pressing machine, until when the pressure of cold isostatic press is 195Mpa, suppresses 8 minutes, then with 10 minutes, release is carried out to cold isostatic press, complete die mould, obtained molybdenum plate pressed compact;
4th step, the demoulding
Take out the punching block after die mould 1, removed the backplate 3 on punching block 1, latex rubber moulding 4 is exposed, then latex rubber moulding is turned over for 4 times molybdenum plate pressed compact is exposed, lifting rope be bundled in the exposed portion of molybdenum plate pressed compact thus hang out molybdenum plate pressed compact;
5th step, sintering
The molybdenum plate pressed compact 4th step taken out drops in intermediate frequency furnace, and first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1900 DEG C from 1840 DEG C, then be incubated 6 hours, then take out, obtained length is 960mm, and width is 545mm, and thickness is the molybdenum plate blank of 115mm.
The design of prismatic table shape mould is to offset because molybdenum powder deadweight is excessive, depositing the base substrate lower thick upper thin caused downwards, to ensure that final molybdenum plate blank is for the uniform cuboid of appearance and size in preparation process.
Molybdenum plate blank obtained by the present embodiment, through detecting, outward appearance is regular, and length is 1060(+5/-5) mm, width is 545(+5/-5) mm, thickness is 105(+2/-2) mm; The density of molybdenum plate blank reaches 9.76g/cm
3, substance is 592kg, and molybdenum plate blank interior tissue is even, and metallographic detection molybdenum plate blank section grain size is 4 grades of number of die is 2000/mm
2; Inner flawless, zero defect is detected through ultrasonic examination, best in quality.
Embodiment 5
The first step, choosing and process of molybdenum powder
Choose that particle mean size is 3.5 μm, pine is than being 1.10g/cm
3molybdenum powder, carry out the ultrasonic screening of 325 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, dress powder
Punching block 1 is vertically placed on ground, and the upper base of punching block 1 is long is 840mm, and wide is 175mm, and going to the bottom long is 836mm, and wide is 175mm, and the height of punching block 1 is 1400mm; Sling with hoisting ring to punching block 1 by latex rubber moulding 4, wherein the upper base of latex rubber moulding 4 is long is 830mm, and wide is 165mm, and going to the bottom long is 826mm, and wide is 165mm, and the height of latex rubber moulding 4 is 1600mm; Again slowly decline latex rubber moulding 4 until the distance from bottom 15mm of the bottom of latex rubber moulding 4 and punching block 1 time, stop declining, latex rubber moulding 4 be fixedly connected with punching block 1; Now again the molybdenum powder that the first step is handled well is put into latex rubber moulding 4, according to the capacity of latex rubber moulding 4, first load the molybdenum powder of 85%, then vibrate punching block 1, make that molybdenum powder is evenly distributed in latex rubber moulding 4, consolidation, then continue to load molybdenum powder until latex rubber moulding 4 is filled;
3rd step, die mould
The punching block 1 installing molybdenum powder in second step is put into cold isostatic press, liquid in cold isostatic press enters punching block 1 inside by inlet opening 2 and applies pressure to latex rubber moulding 4, the rate of rise of cold isostatic press is set to 15Mpa/min, open cold isostatic pressing machine, until when the pressure of cold isostatic press is 200Mpa, suppresses 7 minutes, then with 8 minutes, release is carried out to cold isostatic press, complete die mould, obtained molybdenum plate pressed compact;
4th step, the demoulding
Take out the punching block after die mould 1, removed the backplate 3 on punching block 1, latex rubber moulding 4 is exposed, then latex rubber moulding is turned over for 4 times molybdenum plate pressed compact is exposed, lifting rope be bundled in the exposed portion of molybdenum plate pressed compact thus hang out molybdenum plate pressed compact;
5th step, sintering
The molybdenum plate pressed compact 4th step taken out drops in intermediate frequency furnace, and first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1900 DEG C from 1840 DEG C, then be incubated 6 hours, then take out, obtained length is 980mm, and width is 530mm, and thickness is the molybdenum plate blank of 110mm.
The design of prismatic table shape mould is to offset because molybdenum powder deadweight is excessive, depositing the base substrate lower thick upper thin caused downwards, to ensure that final molybdenum plate blank is for the uniform cuboid of appearance and size in preparation process.
Molybdenum plate blank obtained by the present embodiment, through detecting, outward appearance is regular, and length is 980(+5/-5) mm, width is 530(+5/-5) mm, thickness is 110(+2/-2) mm; The density of molybdenum plate blank reaches 9.84g/cm
3, substance is 562kg, and molybdenum plate blank interior tissue is even, and metallographic detection molybdenum plate blank section grain size is 4 grades of number of die is 2000/mm
2; Inner flawless, zero defect is detected through ultrasonic examination, best in quality.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (2)
1. the preparation method of large-scale molybdenum plate blank, is characterized in that, comprises the steps:
The first step, choosing and process of molybdenum powder
Choose that particle mean size is 3.5 μm ~ 4.5 μm, pine is than being 1.1 ~ 1.3g/cm
3molybdenum powder, carry out the ultrasonic screening of 325 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, dress powder
Punching block (1) is vertically placed on ground, opening upwards; With hoisting ring, latex rubber moulding (4) is sling to punching block, again slowly decline latex rubber moulding (4) until the distance from bottom 10 ~ 20mm of the bottom of latex rubber moulding (4) and punching block (1) time, stop declining, latex rubber moulding (4) is fixedly connected with described punching block (1); Now again the molybdenum powder that the first step is handled well is put into latex rubber moulding (4), according to the capacity of latex rubber moulding (4), first load the molybdenum powder of 80% ~ 90%, then described punching block (1) is vibrated, make that molybdenum powder is evenly distributed in latex rubber moulding (4), consolidation, then continue to load molybdenum powder until latex rubber moulding (4) is filled;
3rd step, die mould
The described punching block (1) second step being installed molybdenum powder puts into cold isostatic press, liquid in cold isostatic press enters punching block (1) inside by inlet opening (2) and applies pressure to latex rubber moulding (4), the rate of rise of cold isostatic press is set to 10 ~ 15Mpa/min, open cold isostatic pressing machine, until when the pressure of cold isostatic press is 185 ~ 200Mpa, suppress 7 ~ 9 minutes, with 8 ~ 10 minutes, release is carried out to cold isostatic press again, complete die mould, obtained molybdenum plate pressed compact;
4th step, the demoulding
Take out the described punching block (1) after die mould, remove the backplate (3) on punching block (1), latex rubber moulding (4) is exposed, again by turning under latex rubber moulding (4) to make molybdenum plate pressed compact expose, lifting rope being bundled in the exposed portion of molybdenum plate pressed compact thus hanging out molybdenum plate pressed compact;
5th step, sintering
The molybdenum plate pressed compact 4th step taken out drops in intermediate frequency furnace, adopts the method progressively heated to heat molybdenum plate pressed compact, obtained molybdenum plate blank;
The terrace with edge that described punching block (1) is inner hollow, 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) for one week along described punching block (1);
The terrace with edge that described latex rubber moulding (4) is inner hollow, 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 upper base, the base square of described punching block (1) respectively.
2. the preparation method of large-scale molybdenum plate blank as claimed in claim 1, it is characterized in that, the method progressively heated described in the 5th step is: first heating makes furnace temperature rise to 1000 DEG C from room temperature for 6 hours, then is incubated 4 hours; Heat and within 3 hours, make furnace temperature rise to 1200 DEG C from 1000 DEG C, then be incubated 5 hours; Heat and within 3 hours, make furnace temperature rise to 1400 DEG C from 1200 DEG C, then be incubated 4 hours; Heat and within 4.5 hours, make furnace temperature rise to 1640 DEG C from 1400 DEG C, then be incubated 6 hours; Heat and within 4 hours, make furnace temperature rise to 1840 DEG C from 1640 DEG C, then be incubated 6 hours; Heat and within 3.5 hours, make furnace temperature rise to 1920 DEG C from 1840 DEG C, then be incubated 6 hours.
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| CN104001913B (en) * | 2014-05-29 | 2016-04-20 | 金堆城钼业股份有限公司 | Tabletting type sealing device and prepare the method for large-scale 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 |
| CN104190937B (en) * | 2014-06-19 | 2017-01-04 | 洛阳科威钨钼有限公司 | A kind of preparation method of ultra-large type carefully brilliant molybdenum electrode |
| CN105458266B (en) * | 2015-12-08 | 2018-03-02 | 西安瑞福莱钨钼有限公司 | It is a kind of to sinter the method for preparing molybdenum plate blank |
| CN109894472B (en) * | 2019-03-14 | 2021-01-01 | 安泰天龙钨钼科技有限公司 | Rolling method of molybdenum plate for spinning molybdenum crucible with large length-diameter ratio |
| 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 |
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