CN105458266A - Method for manufacturing molybdenum plate blank through sintering - Google Patents
Method for manufacturing molybdenum plate blank through sintering Download PDFInfo
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- CN105458266A CN105458266A CN201510902205.3A CN201510902205A CN105458266A CN 105458266 A CN105458266 A CN 105458266A CN 201510902205 A CN201510902205 A CN 201510902205A CN 105458266 A CN105458266 A CN 105458266A
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- molybdenum powder
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 46
- 239000011733 molybdenum Substances 0.000 title claims abstract description 46
- 238000005245 sintering Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims description 42
- 239000002245 particle Substances 0.000 claims description 24
- 238000004321 preservation Methods 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000009694 cold isostatic pressing Methods 0.000 abstract 1
- 238000005429 filling process Methods 0.000 abstract 1
- 239000012856 weighed raw material Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a method for manufacturing a molybdenum plate blank through sintering. The method includes the steps that firstly, raw materials are weighed, and the weighed raw materials are evenly mixed, and mixed molybdenum powder is obtained; secondly, the mixed molybdenum powder is pressed into a plate blank in a cold isostatic pressing manner; and thirdly, under the hydrogen atmosphere, the plate blank is heated and sintered, and the molybdenum plate blank is obtained after being naturally cooled. Heating and sintering include the specific steps that firstly, the plate blank is firstly heated to 900 DEG C and sintered for 1 hour to 2 hours at the temperature of 900 DEG C, then the plate blank is heated to 1,500 DEG C and sintered for 2 hours to 4 hours at the temperature of 1,500 DEG C, and then the plate blank is heated to 750 DEG C to 1,780 DEG C and sintered for 6 hours to 10 hours at the temperature of 750 DEG C to 1,780 DEG C. According to the method, molybdenum powder used in the method is common brands of molybdenum powder in the market, cost is controllable, and purchase is easy; the apparent density of the mixed molybdenum powder is increased, fluidity is improved, a rubber sleeve is filled with the molybdenum powder more easily in the powder filling process, and the plate profile of the pressed blank is improved; and the maximum sintering temperature is lowered, and the loss of equipment and the like and energy consumption are reduced.
Description
Technical field
The invention belongs to powder metallurgical technology, be specifically related to a kind ofly sinter the method preparing molybdenum plate blank.
Background technology
Produce in LED display, solar energy film process, the conventional magnetic control spattering target that does of Mo uses.Therefore, require that the Mo used as target has high-purity and the uniform feature of microscopic structure, and the performance process of molybdenum target material is by the impact of process, the purity of the molybdenum plate blank of raw materials for production and structural homogenity just seem particularly important.As the important raw and processed materials of target, molybdenum plate blank generally adopts powder metallurgic method to prepare, and key step is: the compacting of powder pre-treating, isostatic cool pressing, hydrogen sintering.Mainly there is following problem in the preparation method of existing molybdenum plate blank: when adopting the large substance slab of fine grained preparation of molybdenum powder, due to molybdenum powder easily reunite cause poor fluidity and apparent density on the low side, therefore in dress powder process, easily " bridging " is produced between powder, repeatedly need knock jolt ramming, and jolt ramming effect is uncontrollable, the filling amount situation of different slab is inconsistent, causes slab template poor, uneven thickness; When adopting single coarse particle molybdenum powder to prepare large substance slab, sintering densification process is comparatively slow, and the sintering temperature of needs is higher, and sintering time is longer; And adopt the molybdenum powder of submicron order, although can reduce sintering temperature, reduce sintering time, submicron molybdenum powder complex manufacturing, cost is high, not easily promotes.
Mention in patent CN102699327A and adopt the molybdenum powder of granularity 2.4 μm ~ 3.2 μm, after shaping, need in hydrogen Intermediate frequency sintering furnace 1900 DEG C of heating 30h.When this shows that the single coarse particle molybdenum powder of use prepares blank, sintering temperature is higher, and sintering time is long, and energy consumption is high.
Mentioning in patent CN88103458.4 can 1300 DEG C ~ 1600 DEG C temperature, sinters the molybdenum blank of the high pure and ultra-fine compacting of granularity≤0.5 μm through 120min ~ 360min.But compare conventional molybdenum powder, complex manufacturing from the known submicron order of patent CN201010107245 (granularity≤1.0 μm) molybdenum powder, and need special reduction apparatus, production cost is high.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of and sinters the method preparing molybdenum plate blank.The molybdenum powder that the method uses is all the common commercially available trade mark, and cost is controlled, and is easy to buying; Through mixed molybdenum powder, apparent density is improved, and mobility improves, and is easier to the filling of molybdenum powder at gum cover, improves the blank template after compacting in dress powder process; Most high sintering temperature decreases, and decreases loss and the energy consumption of equipment etc.The molybdenum plate blank grain size adopting the method to prepare is moderate, and number of die is 1700/mm
3~ 2300/mm
3, grain size distribution is narrower, and density is 9.92g/cm
3~ 9.98g/cm
3.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, comprises the following steps:
Step one, take each raw material according to following percentage by weight: particle mean size is the molybdenum powder 20% ~ 30% of 1.5 μm ~ 2.5 μm, particle mean size is the molybdenum powder 55% ~ 65% of 3.0 μm ~ 3.5 μm, particle mean size is the molybdenum powder 10% ~ 20% of 4.5 μm ~ 5.0 μm, is mixed by the raw material taken and obtains mixing molybdenum powder;
Step 2, employing isostatic cool pressing mode are pressed into slab by mixing molybdenum powder described in step one;
Step 3, in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, naturally obtain molybdenum plate blank after cooling; The detailed process of described heat-agglomerating is: first by heating of plate blank to 900 DEG C heat preservation sintering 1h ~ 2h, be then heated to 1500 DEG C of heat preservation sintering 2h ~ 4h, then is heated to 1750 DEG C ~ 1780 DEG C heat preservation sintering 6h ~ 10h.
Above-mentioned a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, adopt drum mixer to mix in step one, batch mixing ball is the molybdenum ball of diameter 8mm ~ 16mm, and the rotating speed of drum mixer is 40r/min ~ 60r/min, and mixing time is 1h ~ 4h.
Above-mentioned a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, the quality of described batch mixing ball is 1:(2 ~ 3 with the mass ratio mixing molybdenum powder).
Above-mentioned a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, the apparent density mixing molybdenum powder described in step one is 1.3g/cm
3~ 1.8g/cm
3, mobility is 10s/50g ~ 25s/50g.
Above-mentioned a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, to be molybdenum powder, the particle mean size of 1.5 μm ~ 2.5 μm the be molybdenum powder of 3.0 μm ~ 3.5 μm of particle mean size described in step one and particle mean size are that the quality purity of the molybdenum powder of 4.5 μm ~ 5.0 μm is all not less than 99.95%.
Above-mentioned a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, the pressure suppressed described in step 2 is 150MPa ~ 250MPa, and the dwell time is 1min ~ 10min.
Above-mentioned a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, in step 3, heating of plate blank to the 900 DEG C time used is 3h ~ 5h, and it is 2h ~ 3h that slab is heated to 1500 DEG C of times used from 900 DEG C, and being heated to 1750 DEG C ~ 1780 DEG C times used from 1500 DEG C is 2h ~ 4h.
The present invention compared with prior art has the following advantages:
1, the molybdenum powder that the present invention uses is all the common commercially available trade mark, and cost is controlled, and is easy to buying; Through mixed molybdenum powder, apparent density is improved, and mobility improves, and is easier to the filling of molybdenum powder at gum cover, improves the blank template after compacting in dress powder process; Most high sintering temperature decreases, and decreases loss and the energy consumption of equipment etc.
2, total sintering time of the present invention is short, adds with stove temperature fall time, within the cooling of every heat molybdenum plate blank sintering can be controlled in 42h total time; 900 DEG C of insulations are conducive to reducing the impurity contents such as the rear molybdenum plate blank oxygen of sintering; Most high sintering temperature is 1750 DEG C ~ 1780 DEG C, and the sintering temperature of relatively general molybdenum plate blank 1900 DEG C, not only reduce loss and the energy consumption of equipment etc., and lower sintering temperature more easily obtains evenly tiny tissue.
3, the molybdenum plate blank grain size adopting method of the present invention to prepare is moderate, and number of die is 1700/mm
3~ 2300/mm
3, grain size distribution is narrower, and density is 9.92g/cm
3~ 9.98g/cm
3.
Below by embodiment, technical solution of the present invention is described in further detail.
Detailed description of the invention
Embodiment 1
The preparation method of the present embodiment comprises the following steps:
Step one, take each raw material according to following percentage by weight: particle mean size is the molybdenum powder 30% of 1.5 μm, and particle mean size is the molybdenum powder 55% of 3.0 μm, and particle mean size is the molybdenum powder 15% of 4.5 μm, and the quality purity of each raw material is all not less than 99.95%; The raw material taken is placed in drum mixer mix obtain mix molybdenum powder, batch mixing ball is the molybdenum ball of diameter 8mm, and the rotating speed of drum mixer is 40r/min, and mixing time is 4h, and the apparent density of the mixing molybdenum powder obtained is 1.42g/cm
3, mobility is 22s/50g; The quality of described batch mixing ball is 1:2 with the mass ratio mixing molybdenum powder;
Step 2, take described in 75kg step one and mix molybdenum powder, the mixing molybdenum powder taken is loaded in the gum cover of 90mm × 400mm × L (L represents length), vibration limit, limit dress powder, then adopts isostatic cool pressing mode that the mixing molybdenum powder loaded in gum cover is pressed into slab; The pressure of compacting is 170MPa, and the dwell time is 8min;
Step 3, in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, naturally obtain molybdenum plate blank after cooling; The detailed process of described heat-agglomerating is: first by heating of plate blank to 900 DEG C heat preservation sintering 2h, be then heated to 1500 DEG C of heat preservation sintering 2h, then be heated to 1755 DEG C of heat preservation sintering 6h; Heating of plate blank to the 900 DEG C time used is 3h, and it is 2h that slab is heated to 1500 DEG C of times used from 900 DEG C, and being heated to 1755 DEG C of times used from 1500 DEG C is 3h.
Molybdenum plate blank substance prepared by the present embodiment is 73.5kg, is of a size of 63mm × 270mm × 435mm after sintering, and actual density is 9.92g/cm
3, number of die is 1780/mm
2.
Embodiment 2
The preparation method of the present embodiment comprises the following steps:
Step one, take each raw material according to following percentage by weight: particle mean size is the molybdenum powder 20% of 2.0 μm, and particle mean size is the molybdenum powder 60% of 3.2 μm, and particle mean size is the molybdenum powder 20% of 4.8 μm, and the quality purity of each raw material is all not less than 99.95%; The raw material taken is placed in drum mixer mix obtain mix molybdenum powder, batch mixing ball is the molybdenum ball of diameter 10mm, and the rotating speed of drum mixer is 60r/min, and mixing time is 3h, and the apparent density of the mixing molybdenum powder obtained is 1.58g/cm
3, mobility is 18s/50g; The quality of described batch mixing ball is 1:3 with the mass ratio mixing molybdenum powder;
Step 2, take described in 140kg step one and mix molybdenum powder, the mixing molybdenum powder taken is loaded in the gum cover of 100mm × 590mm × L, vibration limit, limit dress powder, then adopt isostatic cool pressing mode that the mixing molybdenum powder loaded in gum cover is pressed into slab; The pressure of compacting is 200MPa, and the dwell time is 2min;
Step 3, in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, naturally obtain molybdenum plate blank after cooling; The detailed process of described heat-agglomerating is: first by heating of plate blank to 900 DEG C heat preservation sintering 2h, be then heated to 1500 DEG C of heat preservation sintering 3h, then be heated to 1780 DEG C of heat preservation sintering 9h; Heating of plate blank to the 900 DEG C time used is 5h, and it is 3h that slab is heated to 1500 DEG C of times used from 900 DEG C, and being heated to 1780 DEG C of times used from 1500 DEG C is 2h.
Molybdenum plate blank substance prepared by the present embodiment is 138.3kg, is of a size of 70mm × 410mm × 487mm after sintering, and actual density is 9.98g/cm
3, number of die is 2300/mm
2.
Embodiment 3
The preparation method of the present embodiment comprises the following steps:
Step one, take each raw material according to following percentage by weight: particle mean size is the molybdenum powder 25% of 2.5 μm, and particle mean size is the molybdenum powder 65% of 3.5 μm, and particle mean size is the molybdenum powder 10% of 5.0 μm, and the quality purity of each raw material is all not less than 99.95%; The raw material taken is placed in drum mixer mix obtain mix molybdenum powder, batch mixing ball is the molybdenum ball of diameter 16mm, and the rotating speed of drum mixer is 50r/min, and mixing time is 1h, and the apparent density of the mixing molybdenum powder obtained is 1.3g/cm
3, mobility is 25s/50g; The quality of described batch mixing ball is 1:2.5 with the mass ratio mixing molybdenum powder;
Step 2, take described in 75kg step one and mix molybdenum powder, the mixing molybdenum powder taken is loaded in the gum cover of 90mm × 400mm × L, vibration limit, limit dress powder, then adopt isostatic cool pressing mode that the mixing molybdenum powder loaded in gum cover is pressed into slab; The pressure of compacting is 150MPa, and the dwell time is 10min;
Step 3, in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, naturally obtain molybdenum plate blank after cooling; The detailed process of described heat-agglomerating is: first by heating of plate blank to 900 DEG C heat preservation sintering 1h, be then heated to 1500 DEG C of heat preservation sintering 4h, then be heated to 1750 DEG C of heat preservation sintering 10h; Heating of plate blank to the 900 DEG C time used is 4h, and it is 2.5h that slab is heated to 1500 DEG C of times used from 900 DEG C, and being heated to 1750 DEG C of times used from 1500 DEG C is 4h.
Molybdenum plate blank substance prepared by the present embodiment is 73.5kg, is of a size of 65mm × 260mm × 430mm after sintering, and actual density is 9.95g/cm
3, number of die is 1700/mm
2.
Embodiment 4
The preparation method of the present embodiment comprises the following steps:
Step one, take each raw material according to following percentage by weight: particle mean size is the molybdenum powder 25% of 1.8 μm, and particle mean size is the molybdenum powder 60% of 3.2 μm, and particle mean size is the molybdenum powder 15% of 5.0 μm, and the quality purity of each raw material is all not less than 99.95%; The raw material taken is placed in drum mixer mix obtain mix molybdenum powder, batch mixing ball is the molybdenum ball of diameter 12mm, and the rotating speed of drum mixer is 50r/min, and mixing time is 4h, and the apparent density of the mixing molybdenum powder obtained is 1.8g/cm
3, mobility is 10s/50g; The quality of described batch mixing ball is 1:2 with the mass ratio mixing molybdenum powder;
Step 2, take described in 140kg step one and mix molybdenum powder, the mixing molybdenum powder taken is loaded in the gum cover of 100mm × 590mm × L, vibration limit, limit dress powder, then adopt isostatic cool pressing mode that the mixing molybdenum powder loaded in gum cover is pressed into slab; The pressure of compacting is 250MPa, and the dwell time is 1min;
Step 3, in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, naturally obtain molybdenum plate blank after cooling; The detailed process of described heat-agglomerating is: first by heating of plate blank to 900 DEG C heat preservation sintering 2h, be then heated to 1500 DEG C of heat preservation sintering 3h, then be heated to 1770 DEG C of heat preservation sintering 8h; Heating of plate blank to the 900 DEG C time used is 4h, and it is 2h that slab is heated to 1500 DEG C of times used from 900 DEG C, and being heated to 1770 DEG C of times used from 1500 DEG C is 3h.
Molybdenum plate blank substance prepared by the present embodiment is 138.3kg, is of a size of 72mm × 415mm × 485mm after sintering, and actual density is 9.96g/cm
3, number of die is 2000/mm
2.
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (7)
1. sinter the method preparing molybdenum plate blank, it is characterized in that, comprise the following steps:
Step one, take each raw material according to following percentage by weight: particle mean size is the molybdenum powder 20% ~ 30% of 1.5 μm ~ 2.5 μm, particle mean size is the molybdenum powder 55% ~ 65% of 3.0 μm ~ 3.5 μm, particle mean size is the molybdenum powder 10% ~ 20% of 4.5 μm ~ 5.0 μm, is mixed by the raw material taken and obtains mixing molybdenum powder;
Step 2, employing isostatic cool pressing mode are pressed into slab by mixing molybdenum powder described in step one;
Step 3, in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, naturally obtain molybdenum plate blank after cooling; The detailed process of described heat-agglomerating is: first by heating of plate blank to 900 DEG C heat preservation sintering 1h ~ 2h, be then heated to 1500 DEG C of heat preservation sintering 2h ~ 4h, then is heated to 1750 DEG C ~ 1780 DEG C heat preservation sintering 6h ~ 10h.
2. according to claim 1ly a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, adopt drum mixer to mix in step one, batch mixing ball is the molybdenum ball of diameter 8mm ~ 16mm, the rotating speed of drum mixer is 40r/min ~ 60r/min, and mixing time is 1h ~ 4h.
3. according to claim 2ly a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, the quality of described batch mixing ball is 1:(2 ~ 3 with the mass ratio mixing molybdenum powder).
4. according to claim 1ly a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, the apparent density mixing molybdenum powder described in step one is 1.3g/cm
3~ 1.8g/cm
3, mobility is 10s/50g ~ 25s/50g.
5. according to claim 1ly a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, to be molybdenum powder, the particle mean size of 1.5 μm ~ 2.5 μm the be molybdenum powder of 3.0 μm ~ 3.5 μm of particle mean size described in step one and particle mean size are that the quality purity of the molybdenum powder of 4.5 μm ~ 5.0 μm is all not less than 99.95%.
6. according to claim 1ly a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, the pressure suppressed described in step 2 is 150MPa ~ 250MPa, and the dwell time is 1min ~ 10min.
7. according to claim 1ly a kind ofly sinter the method preparing molybdenum plate blank, it is characterized in that, in step 3, heating of plate blank to the 900 DEG C time used is 3h ~ 5h, it is 2h ~ 3h that slab is heated to 1500 DEG C of times used from 900 DEG C, and being heated to 1750 DEG C ~ 1780 DEG C times used from 1500 DEG C is 2h ~ 4h.
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CN106583733A (en) * | 2016-11-10 | 2017-04-26 | 洛阳科威钨钼有限公司 | Preparing method for high-density molybdenum alloy plate |
CN106735193A (en) * | 2016-12-23 | 2017-05-31 | 西安瑞福莱钨钼有限公司 | A kind of preparation method of low potassium content molybdenum plate blank |
CN108907211A (en) * | 2018-08-16 | 2018-11-30 | 北京科技大学 | A method of preparing large scale molybdenum plate blank |
CN108907211B (en) * | 2018-08-16 | 2021-10-08 | 北京科技大学 | Method for preparing large-size molybdenum plate blank |
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 |
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