CN105458266B - It is a kind of to sinter the method for preparing molybdenum plate blank - Google Patents
It is a kind of to sinter the method for preparing molybdenum plate blank Download PDFInfo
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- CN105458266B CN105458266B CN201510902205.3A CN201510902205A CN105458266B CN 105458266 B CN105458266 B CN 105458266B CN 201510902205 A CN201510902205 A CN 201510902205A CN 105458266 B CN105458266 B CN 105458266B
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- molybdenum
- plate blank
- molybdenum powder
- sintering
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 45
- 239000011733 molybdenum Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 56
- 238000002156 mixing Methods 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000004321 preservation Methods 0.000 claims abstract description 16
- 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
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 abstract description 13
- 238000011049 filling Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000007423 decrease Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000005516 engineering process 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
- 239000013077 target material Substances 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 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
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
Abstract
The invention discloses a kind of method for sintering and preparing molybdenum plate blank, this method is:First, each raw material is weighed, the raw material weighed is well mixed and obtains mixing molybdenum powder;2nd, slab is pressed into by molybdenum powder is mixed using isostatic cool pressing mode;3rd, in a hydrogen atmosphere, heat-agglomerating is carried out to slab, molybdenum plate blank is obtained after natural cooling;The detailed process of the heat-agglomerating is:First by heating of plate blank to 900 DEG C of heat preservation sintering 1h~2h, 1500 DEG C of heat preservation sintering 2h~4h are then heated to, are again heated to 1750 DEG C~1780 DEG C heat preservation sintering 6h~10h.The molybdenum powder that the present invention uses all is the common commercially available trade mark, and cost is controllable, and is easy to purchase;It is improved by mixed molybdenum powder apparent density, mobility is improved, and is easier to filling of the molybdenum powder in gum cover during dress powder, is improved the blank template after compacting;Maximum sintering temperature decreases, and reduces loss and the energy consumption of equipment etc..
Description
Technical field
The invention belongs to powder metallurgical technology, and in particular to a kind of to sinter the method for preparing molybdenum plate blank.
Background technology
During producing LED display, solar energy film, Mo is conventional to do magnetic control spattering target use.It is therefore desirable to
The characteristics of there is high-purity and uniform microscopic structure as the Mo that target uses, and the processing of the performance of molybdenum target material is by processed
The influence of journey, the purity and structural homogenity of the molybdenum plate blank of raw materials for production are just particularly important.Important former material as target
Material, molybdenum plate blank are typically prepared using powder metallurgic method, mainly comprised the following steps:Powder pre-treating, isostatic cool pressing compacting, hydrogen sintering.
The preparation method of existing molybdenum plate blank is primarily present following problem:When preparing big substance slab using fine grained molybdenum powder, due to
Molybdenum powder, which is easily reunited, causes poor fluidity and apparent density relatively low, therefore is also easy to produce " bridging " between powder during filling powder, needs
Jolt ramming is repeatedly tapped, and jolt ramming effect is uncontrollable, the filling amount situation of different slabs is inconsistent, causes slab template poor, thickness
It is uneven;When preparing big substance slab using single coarse particle molybdenum powder, sintering densification process it is relatively slow, it is necessary to sintering temperature compared with
Height, sintering time are longer;And the molybdenum powder of submicron order is used, although sintering temperature can be reduced, reduce sintering time, sub-micro
Meter level Mo powder production complex process, cost is high, is not easy to promote.
The molybdenum powder using 2.4 μm~3.2 μm of granularity is mentioned in patent CN 102699327A, need to be in hydrogen after shaping
1900 DEG C of heating 30h in frequency sintering furnace.It can be seen that when preparing blank using single coarse particle molybdenum powder, sintering temperature compared with
Height, sintering time is long, high energy consumption.
Grain can be sintered in 1300 DEG C~1600 DEG C temperature through 120min~360min by being mentioned in patent CN88103458.4
The molybdenum blank of the high pure and ultra-fine compacting of≤0.5 μm of degree.But understand the submicron order (μ of granularity≤1.0 from patent CN201010107245
M) molybdenum powder compares conventional molybdenum powder, complex manufacturing, and needs special reduction apparatus, and production cost is high.
The content of the invention
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of sintering prepares molybdenum
The method of slab.The molybdenum powder that this method uses all is the common commercially available trade mark, and cost is controllable, and is easy to purchase;After mixing
Molybdenum powder, apparent density is improved, and mobility is improved, and is filled and is easier to filling of the molybdenum powder in gum cover during powder, improves
Blank template after compacting;Maximum sintering temperature decreases, and reduces loss and the energy consumption of equipment etc..Using party's legal system
Standby molybdenum plate blank grain size is moderate, and number of die is 1700/mm3~2300/mm3, grain size distribution is narrower, and density is
9.92g/cm3~9.98g/cm3。
In order to solve the above technical problems, the technical solution adopted by the present invention is:It is a kind of to sinter the method for preparing molybdenum plate blank, its
It is characterised by, comprises the following steps:
Step 1: weigh each raw material according to following percentage by weight:Particle mean size is 1.5 μm~2.5 μm of molybdenum powder
20%~30%, particle mean size is 3.0 μm~3.5 μm of molybdenum powder 55%~65%, and particle mean size is 4.5 μm~5.0 μm
Molybdenum powder 10%~20%, the raw material weighed is well mixed and obtains mixing molybdenum powder;
Step 2: molybdenum powder will be mixed described in step 1 using isostatic cool pressing mode is pressed into slab;
Step 3: in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, molybdenum plate is obtained after natural cooling
Base;The detailed process of the heat-agglomerating is:Heating of plate blank is first then heated to 1500 to 900 DEG C of heat preservation sintering 1h~2h
DEG C heat preservation sintering 2h~4h, is again heated to 1750 DEG C~1780 DEG C heat preservation sintering 6h~10h.
The method that a kind of above-mentioned sintering prepares molybdenum plate blank, it is characterised in that entered in step 1 using drum mixer
Row mixing, batch mixing ball are diameter 8mm~16mm molybdenum ball, and the rotating speed of drum mixer is 40r/min~60r/min, batch mixing
Time is 1h~4h.
The method that a kind of above-mentioned sintering prepares molybdenum plate blank, it is characterised in that the quality of the batch mixing ball is with mixing molybdenum powder
The mass ratio at end is 1:(2~3).
The method that a kind of above-mentioned sintering prepares molybdenum plate blank, it is characterised in that the pine of molybdenum powder is mixed described in step 1
Dress density is 1.3g/cm3~1.8g/cm3, mobility is 10s/50g~25s/50g.
The method that a kind of above-mentioned sintering prepares molybdenum plate blank, it is characterised in that particle mean size described in step 1 is 1.5 μm
~2.5 μm of molybdenum powder, the molybdenum powder that particle mean size is 3.0 μm~3.5 μm and molybdenum powder that particle mean size is 4.5 μm~5.0 μm
The quality purity at end is not less than 99.95%.
The method that a kind of above-mentioned sintering prepares molybdenum plate blank, it is characterised in that the pressure suppressed described in step 2 is
150MPa~250MPa, dwell time are 1min~10min.
The method that a kind of above-mentioned sintering prepares molybdenum plate blank, it is characterised in that in step 3 used in heating of plate blank to 900 DEG C
Time be 3h~5h, slab is 2h~3h from 900 DEG C of times being heated to used in 1500 DEG C, and 1750 DEG C are heated to from 1500 DEG C
Time used in~1780 DEG C is 2h~4h.
The present invention has advantages below compared with prior art:
1st, the molybdenum powder that the present invention uses all is the common commercially available trade mark, and cost is controllable, and is easy to purchase;By mixed
Molybdenum powder, apparent density are improved, and mobility is improved, and are easier to filling of the molybdenum powder in gum cover during dress powder, are improved
Blank template after compacting;Maximum sintering temperature decreases, and reduces loss and the energy consumption of equipment etc..
2nd, total sintering time of the invention is short, and plus with stove temperature fall time, cooling total time per heat molybdenum plate blank sintering can
Control is within 42h;900 DEG C of insulations advantageously reduce the impurity content such as molybdenum plate blank oxygen after sintering;Maximum sintering temperature is
1750 DEG C~1780 DEG C, for the sintering temperature of relatively general 1900 DEG C of molybdenum plate blank, not only reduce loss and the energy of equipment etc.
Consumption, and relatively low sintering temperature is easier to obtain uniformly tiny tissue.
3rd, the molybdenum plate blank grain size prepared using the method for the present invention is moderate, and number of die is 1700/mm3~2300/
mm3, grain size distribution is narrower, density 9.92g/cm3~9.98g/cm3。
Technical solution of the present invention is described in further detail below by embodiment.
Embodiment
Embodiment 1
The preparation method of the present embodiment comprises the following steps:
Step 1: weigh each raw material according to following percentage by weight:Particle mean size is 1.5 μm of molybdenum powder 30%, average
Granularity is 3.0 μm of molybdenum powder 55%, and particle mean size is 4.5 μm of molybdenum powder 15%, and the quality purity of each raw material is not less than
99.95%;The raw material weighed is placed in drum mixer to be well mixed and obtains mixing molybdenum powder, batch mixing ball is diameter 8mm
Molybdenum ball, the rotating speed of drum mixer is 40r/min, mixing time 4h, and the apparent density of obtained mixing molybdenum powder is
1.42g/cm3, mobility 22s/50g;The quality of the batch mixing ball is 1 with the mass ratio for mixing molybdenum powder:2;
Mix molybdenum powder described in 75kg step 1 Step 2: weighing, by the mixing molybdenum powder weighed load 90mm ×
In 400mm × L (L represents length) gum cover, powder is filled in vibration, is then loaded into using isostatic cool pressing mode mixed in gum cover
Close molybdenum powder and be pressed into slab;The pressure of compacting is 170MPa, dwell time 8min;
Step 3: in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, molybdenum plate is obtained after natural cooling
Base;The detailed process of the heat-agglomerating is:First by heating of plate blank to 900 DEG C of heat preservation sintering 2h, 1500 DEG C of guarantors are then heated to
Temperature sintering 2h, is again heated to 1755 DEG C of heat preservation sintering 6h;Time used in heating of plate blank to 900 DEG C is 3h, and slab adds from 900 DEG C
Heat to the time used in 1500 DEG C is 2h, and the time being heated to from 1500 DEG C used in 1755 DEG C is 3h.
Molybdenum plate blank substance manufactured in the present embodiment is 73.5kg, and size is 63mm × 270mm × 435mm after sintering, actual measurement
Density is 9.92g/cm3, number of die is 1780/mm2。
Embodiment 2
The preparation method of the present embodiment comprises the following steps:
Step 1: weigh each raw material according to following percentage by weight:Particle mean size is 2.0 μm of molybdenum powder 20%, average
Granularity is 3.2 μm of molybdenum powder 60%, and particle mean size is 4.8 μm of molybdenum powder 20%, and the quality purity of each raw material is not less than
99.95%;The raw material weighed is placed in drum mixer to be well mixed and obtains mixing molybdenum powder, batch mixing ball is diameter 10mm
Molybdenum ball, the rotating speed of drum mixer is 60r/min, mixing time 3h, and the apparent density of obtained mixing molybdenum powder is
1.58g/cm3, mobility 18s/50g;The quality of the batch mixing ball is 1 with the mass ratio for mixing molybdenum powder:3;
Mix molybdenum powder described in 140kg step 1 Step 2: weighing, by the mixing molybdenum powder weighed load 100mm ×
In 590mm × L gum cover, powder is filled in vibration, the mixing molybdenum powder pressure being then loaded into using isostatic cool pressing mode in gum cover
Slab is made;The pressure of compacting is 200MPa, dwell time 2min;
Step 3: in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, molybdenum plate is obtained after natural cooling
Base;The detailed process of the heat-agglomerating is:First by heating of plate blank to 900 DEG C of heat preservation sintering 2h, 1500 DEG C of guarantors are then heated to
Temperature sintering 3h, is again heated to 1780 DEG C of heat preservation sintering 9h;Time used in heating of plate blank to 900 DEG C is 5h, and slab adds from 900 DEG C
Heat to the time used in 1500 DEG C is 3h, and the time being heated to from 1500 DEG C used in 1780 DEG C is 2h.
Molybdenum plate blank substance manufactured in the present embodiment is 138.3kg, and size is 70mm × 410mm × 487mm after sintering, actual measurement
Density is 9.98g/cm3, number of die is 2300/mm2。
Embodiment 3
The preparation method of the present embodiment comprises the following steps:
Step 1: weigh each raw material according to following percentage by weight:Particle mean size is 2.5 μm of molybdenum powder 25%, average
Granularity is 3.5 μm of molybdenum powder 65%, and particle mean size is 5.0 μm of molybdenum powder 10%, and the quality purity of each raw material is not less than
99.95%;The raw material weighed is placed in drum mixer to be well mixed and obtains mixing molybdenum powder, batch mixing ball is diameter 16mm
Molybdenum ball, the rotating speed of drum mixer is 50r/min, mixing time 1h, and the apparent density of obtained mixing molybdenum powder is
1.3g/cm3, mobility 25s/50g;The quality of the batch mixing ball is 1 with the mass ratio for mixing molybdenum powder:2.5;
Mix molybdenum powder described in 75kg step 1 Step 2: weighing, by the mixing molybdenum powder weighed load 90mm ×
In 400mm × L gum cover, powder is filled in vibration, the mixing molybdenum powder pressure being then loaded into using isostatic cool pressing mode in gum cover
Slab is made;The pressure of compacting is 150MPa, dwell time 10min;
Step 3: in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, molybdenum plate is obtained after natural cooling
Base;The detailed process of the heat-agglomerating is:First by heating of plate blank to 900 DEG C of heat preservation sintering 1h, 1500 DEG C of guarantors are then heated to
Temperature sintering 4h, is again heated to 1750 DEG C of heat preservation sintering 10h;Time used in heating of plate blank to 900 DEG C is 4h, and slab is from 900 DEG C
It is 2.5h to be heated to the time used in 1500 DEG C, and the time being heated to from 1500 DEG C used in 1750 DEG C is 4h.
Molybdenum plate blank substance manufactured in the present embodiment is 73.5kg, and size is 65mm × 260mm × 430mm after sintering, actual measurement
Density is 9.95g/cm3, number of die is 1700/mm2。
Embodiment 4
The preparation method of the present embodiment comprises the following steps:
Step 1: weigh each raw material according to following percentage by weight:Particle mean size is 1.8 μm of molybdenum powder 25%, average
Granularity is 3.2 μm of molybdenum powder 60%, and particle mean size is 5.0 μm of molybdenum powder 15%, and the quality purity of each raw material is not less than
99.95%;The raw material weighed is placed in drum mixer to be well mixed and obtains mixing molybdenum powder, batch mixing ball is diameter 12mm
Molybdenum ball, the rotating speed of drum mixer is 50r/min, mixing time 4h, and the apparent density of obtained mixing molybdenum powder is
1.8g/cm3, mobility 10s/50g;The quality of the batch mixing ball is 1 with the mass ratio for mixing molybdenum powder:2;
Mix molybdenum powder described in 140kg step 1 Step 2: weighing, by the mixing molybdenum powder weighed load 100mm ×
In 590mm × L gum cover, powder is filled in vibration, the mixing molybdenum powder pressure being then loaded into using isostatic cool pressing mode in gum cover
Slab is made;The pressure of compacting is 250MPa, dwell time 1min;
Step 3: in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, molybdenum plate is obtained after natural cooling
Base;The detailed process of the heat-agglomerating is:First by heating of plate blank to 900 DEG C of heat preservation sintering 2h, 1500 DEG C of guarantors are then heated to
Temperature sintering 3h, is again heated to 1770 DEG C of heat preservation sintering 8h;Time used in heating of plate blank to 900 DEG C is 4h, and slab adds from 900 DEG C
Heat to the time used in 1500 DEG C is 2h, and the time being heated to from 1500 DEG C used in 1770 DEG C is 3h.
Molybdenum plate blank substance manufactured in the present embodiment is 138.3kg, and size is 72mm × 415mm × 485mm after sintering, actual measurement
Density is 9.96g/cm3, number of die is 2000/mm2。
It is described above, only it is presently preferred embodiments of the present invention, any restrictions is not done to the present invention, it is every according to invention skill
Any simple modification, change and the equivalent structure change that art is substantially made to above example, still fall within the technology of the present invention
In the protection domain of scheme.
Claims (6)
1. a kind of sinter the method for preparing molybdenum plate blank, it is characterised in that comprises the following steps:
Step 1: weigh each raw material according to following percentage by weight:The molybdenum powder 20% that particle mean size is 1.5 μm~2.5 μm~
30%, particle mean size is 3.0 μm~3.5 μm of molybdenum powder 55%~65%, and particle mean size is 4.5 μm~5.0 μm of molybdenum powder
10%~20%, the raw material weighed is well mixed and obtains mixing molybdenum powder;
Step 2: molybdenum powder will be mixed described in step 1 using isostatic cool pressing mode is pressed into slab;
Step 3: in a hydrogen atmosphere, heat-agglomerating is carried out to slab described in step 2, molybdenum plate blank is obtained after natural cooling;
The detailed process of the heat-agglomerating is:First by heating of plate blank to 900 DEG C of heat preservation sintering 1h~2h, 1500 DEG C of guarantors are then heated to
Temperature sintering 2h~4h, is again heated to 1750 DEG C~1780 DEG C heat preservation sintering 6h~10h;Time used in heating of plate blank to 900 DEG C
For 3h~5h, slab is 2h~3h from 900 DEG C of times being heated to used in 1500 DEG C, and 1750 DEG C~1780 are heated to from 1500 DEG C
Time used in DEG C is 2h~4h.
2. a kind of method for sintering preparation molybdenum plate blank according to claim 1, it is characterised in that roller is used in step 1
Formula batch mixer is mixed, and batch mixing ball is diameter 8mm~16mm molybdenum ball, the rotating speed of drum mixer for 40r/min~
60r/min, mixing time are 1h~4h.
A kind of 3. method for sintering preparation molybdenum plate blank according to claim 2, it is characterised in that the quality of the batch mixing ball
Mass ratio with mixing molybdenum powder is 1:(2~3).
4. a kind of method for sintering preparation molybdenum plate blank according to claim 1, it is characterised in that mixed described in step 1
The apparent density of molybdenum powder is 1.3g/cm3~1.8g/cm3, mobility is 10s/50g~25s/50g.
5. a kind of method for sintering preparation molybdenum plate blank according to claim 1, it is characterised in that average described in step 1
Molybdenum powder, the molybdenum powder that particle mean size is 3.0 μm~3.5 μm and the particle mean size that granularity is 1.5 μm~2.5 μm be 4.5 μm~
The quality purity of 5.0 μm of molybdenum powder is not less than 99.95%.
6. a kind of method for sintering preparation molybdenum plate blank according to claim 1, it is characterised in that suppressed described in step 2
Pressure be 150MPa~250MPa, the dwell time is 1min~10min.
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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 |
CN108907211B (en) * | 2018-08-16 | 2021-10-08 | 北京科技大学 | Method for preparing large-size 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 |
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