CN101935793A - A high-strength molybdenum-doped plate and its preparation method - Google Patents
A high-strength molybdenum-doped plate and its preparation method Download PDFInfo
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- CN101935793A CN101935793A CN 201010505794 CN201010505794A CN101935793A CN 101935793 A CN101935793 A CN 101935793A CN 201010505794 CN201010505794 CN 201010505794 CN 201010505794 A CN201010505794 A CN 201010505794A CN 101935793 A CN101935793 A CN 101935793A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000011733 molybdenum Substances 0.000 claims abstract description 34
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 34
- 239000011246 composite particle Substances 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 229910016006 MoSi Inorganic materials 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000005096 rolling process Methods 0.000 claims abstract description 7
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 34
- 239000011159 matrix material Substances 0.000 claims description 7
- 230000003014 reinforcing effect Effects 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 4
- 238000005098 hot rolling Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 238000009827 uniform distribution Methods 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 9
- 238000004663 powder metallurgy Methods 0.000 abstract description 3
- 229910021193 La 2 O 3 Inorganic materials 0.000 abstract 2
- 238000005452 bending Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910017311 Mo—Mo Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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Abstract
本发明涉及了一种高性能钼掺杂板材及其制备方法。将MoSi2与Y2O3、CeO2中的一种，或是与Y2O3和La2O3和CeO2中的两种，或是与Y2O3和La2O3和CeO2三者的混合物经过高能球磨后，制备成MoSi2/稀土氧化物超细复合微粒；然后将超细复合微粒按0.1wt％～3wt％的比例掺杂到微细钼粉中，采用粉末冶金方法经混合、压制、烧结工序制备出Mo5Si3/稀土复合微粒强化钼板坯；最后经大变形轧制得到所需板材。用该方法生产的掺杂钼板材具有优异的高温和室温强度，其室温抗拉强度可达921MPa，抗弯强度可达1674MPa，1000℃时的抗拉强度可达558.7MPa，可广泛应用于高温领域，如高温舟皿、电极等。The invention relates to a high-performance molybdenum-doped plate and a preparation method thereof. Combine MoSi 2 with one of Y 2 O 3 and CeO 2 , or with two of Y 2 O 3 and La 2 O 3 and CeO 2 , or with Y 2 O 3 and La 2 O 3 and CeO 2 After the mixture of the three is subjected to high-energy ball milling, MoSi 2 /rare earth oxide ultrafine composite particles are prepared; then the ultrafine composite particles are doped into fine molybdenum powder at a ratio of 0.1wt% to 3wt%, and powder metallurgy is used to Mo 5 Si 3 /rare earth composite particles reinforced molybdenum slabs are prepared through mixing, pressing and sintering processes; finally, the required plates are obtained through large deformation rolling. The doped molybdenum sheet produced by this method has excellent high temperature and room temperature strength, its room temperature tensile strength can reach 921MPa, its bending strength can reach 1674MPa, and its tensile strength at 1000°C can reach 558.7MPa, which can be widely used in high temperature Fields, such as high temperature boats, electrodes, etc.
Description
Technical field
The present invention relates to a kind of high-performance doped molybdenum board material, be specifically related to a kind of high temperature boat sheet material and preparation technology thereof with excellent hot strength and room temperature strength.
Background technology
Molybdenum and alloy thereof because have the fusing point height, intensity is big, electrical and thermal conductivity performance good, etch resistant properties reaches advantages such as mechanical behavior under high temperature is good by force, is widely used in high temperature fields such as heat, glass melting, thermal structure strut member.At present, the series that is applied to the high temperature field mainly contains TZM plate, Mo-La doping sheet material, Mo-Re plate and ASK doping sheet material.Wherein, the sheet material that is used for the high temperature sintering boat mainly is TZM plate and Mo-La doping sheet material.Although they all have the good high-temperature performance, still exist weak point at present.As the low-temperature flexibility deficiency of TZM plate, plastic making difficulty; Although Mo-Re sheet material excellent performance because Re is rare metal, costs an arm and a leg, tooling cost is difficult to control; Mo-La doping sheet material room-temperature property is good, but has red brittleness during high temperature, and intensity and plasticity can reduce simultaneously, and is affected its work-ing life, thereby improves production cost.
Summary of the invention
The object of the present invention is to provide a kind of high temperature field that is used for, high-strength molybdenum board material in high temperature boat field and preparation method thereof particularly, this molybdenum materials not only has higher intensity under hot conditions, and be difficult for deforming and rupturing in pushing away under boat mechanical force and the thermal stresses effect repeatedly, this preparation methods is simple simultaneously, cost is low, easily realizes producing in enormous quantities.
Technical scheme of the present invention is achieved in that
A kind of high strength molybdenum doping sheet material, its composition is by close grain Mo matrix phase and disperse uniform distribution superfine Mo therein
5Si
3The phase composite of/rare earth composite particles reinforcing and toughening, described reinforcing and toughening is with MoSi mutually
2With Y
2O
3, CeO
2In a kind of, or and Y
2O
3And La
2O
3And CeO
2In two kinds, or and Y
2O
3And La
2O
3And CeO
2Three's mixture mixes pure molybdenum powder through the compound ultra-fine composite particles that is prepared into of high-energy ball milling, high temperature sintering, and reaction in generates.
Described MoSi
2With Y
2O
3, CeO
2In a kind of, or and Y
2O
3And La
2O
3And CeO
2In two kinds, or and Y
2O
3And La
2O
3And CeO
2Three's mixture makes ultra-fine composite particles in 2: 3～4: 1 ratio high-energy ball milling.
The median size of described ultra-fine composite particles is 80～400nm.
Described ultra-fine composite particles is 0.1%～3% to add in the pure molybdenum powder by mass ratio.
Described MoSi
2Purity is 99%～99.99%, median size＜5 μ m.
Described Y
2O
3, CeO
2Or La
2O
3Purity is 99.5～99.99%, median size＜2 μ m.
Described pure molybdenum powder median size＜8 μ m.
Described high strength molybdenum doping preparation of plates method: add to described ultra-fine composite particles in the pure molybdenum powder of median size＜8 μ m by mass ratio 0.1%～3%, mix, compacting, sintering make the sintering slab, again with sintering slab hot rolling cogging, and through the rolling molybdenum board material that obtains, last stress relieving by annealing gets final product.
Described sintering temperature is that 1850 ℃～2050 ℃, sintering time 5～10 hours, sintering atmosphere are pure hydrogen; To the sintering slab hot rolling cogging under 1350 ℃～1500 ℃ temperature that obtains, the rolling molybdenum board material that obtains, total deformation is not less than 80%; Under 850 ℃～1050 ℃ annealing temperature, eliminate stress at last.
Adopt the molybdenum board material of technique scheme preparation, on the one hand, because the MoSi that doping agent has adopted high energy ball mill method to produce
2The ultra-fine composite particles of/rare earth oxide, particle size is thin, and is active high, not only can effectively improve its solid solution capacity in the Mo matrix, the more evenly (see figure 1) that in matrix, distributes also simultaneously, the mechanics and the pressure machining characteristics of preparation sintering molybdenum are significantly increased; On the other hand, because ultra-fine composite particles is active high, in sintering process, under the acting in conjunction in stress field and temperature field, MoSi
2Easy and the matrix molybdenum generation reaction in of the ultra-fine composite particles of/rare earth oxide generates Mo
5Si
3, this Mo
5Si
3Have higher high temperature creep-resisting performance, make and molybdenum between interface bond strength far above between the Mo-Mo and the interface bond strength between the Mo-rare earth, stop on the interface room nucleation and it disappeared on the interface, thereby improve the hot strength of material; In addition, rare earth oxide, the Mo of highly dispersed distribution
5Si
3, not only improved dispersion-strengthened effect, but simultaneously also crystal grain thinning, purify crystal boundary, these all can reach the purpose of the weave construction of remarkable improvement and control material, make the Mo intensity and the tough performance of preparation reach perfect coupling, high comprehensive performance.
Beneficial effect of the present invention is embodied in:
MoSi
2The ultra-fine composite particles fine size of/rare earth oxide and have higher activity adds MoSi in molybdenum
2The ultra-fine composite particles of/rare earth oxide can also increase the solid solubility of ultra-fine composite particles in matrix in the refinement matrix grain, improve its dispersed uniform, improves strengthening phase and basal body interface intensity, thereby can effectively improve the molybdenum materials over-all properties.Compare MoSi with pure molybdenum
2The room temperature and the hot strength of the ultra-fine composite particles doping of/rare earth oxide sheet material all are significantly improved, and room temperature toughness also is greatly improved simultaneously.In addition, the production cost of this sheet material is relatively low, also is easy to realize mass-producing, industrialization production.
Description of drawings
Fig. 1: the MoSi of doping 3wt%
2The molybdenum plate base SEM figure for preparing behind the ultra-fine composite particles of/rare earth oxide;
Fig. 2: the molybdenum plate base SEM figure for preparing behind the rare earth oxide of doping 3wt%.
Embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1:
Be 100～150nm and the equally distributed Mo of disperse mainly by Mo phase and median size
5Si
3/ Y
2O
3The composite particles strengthening phase is formed.Mo
5Si
3/ Y
2O
3Composite particles is with MoSi
2And Y
2O
3The form of composite particles adds, and addition is 2%, wherein, and MoSi
2With Y
2O
3Mass ratio be 1: 1.Prepare the sintering slab that thickness is 26cm through the prior powder metallurgy method, its sintering temperature is 1950 ℃, sintering time 4h.Then, it is rolling and prepare thickness and be 3.0mm boat molybdenum board material that sintering molybdenum plate base is implemented gross distortion, and total deformation is 88.5%.Its mechanical performance data is as shown in table 1.
Table 1 present embodiment material property data
Embodiment 2:
Be 130～200nm and the equally distributed Mo of disperse mainly by Mo phase and median size
5Si
3/ La
2O
3/ Y
2O
3The phase composite of composite particles reinforcing and toughening.Mo
5Si
3/ La
2O
3/ Y
2O
3Composite particles is with MoSi
2And La
2O
3And Y
2O
3The form of composite particles adds, and addition is 1.2%, MoSi
2With La
2O
3And Y
2O
3Mass ratio be 2: 1: 1.Prepare the sintering slab that thickness is 22cm through the prior powder metallurgy method, its sintering temperature is 2000 ℃, sintering time 6h.Then, it is rolling and prepare thickness and be 2.5mm boat molybdenum board material that sintering molybdenum plate base is implemented gross distortion, and total deformation is 88.6%.Its mechanical performance data is as shown in table 2.
Table 2 present embodiment material property data
Claims (9)
1. high strength molybdenum doping sheet material is characterized in that: material composition by close grain Mo matrix mutually and disperse uniform distribution superfine Mo therein
5Si
3The phase composite of/rare earth composite particles reinforcing and toughening, described reinforcing and toughening is with MoSi mutually
2With Y
2O
3, CeO
2In a kind of, or and Y
2O
3And La
2O
3And CeO
2In two kinds, or and Y
2O
3And La
2O
3And CeO
2Three's mixture mixes pure molybdenum powder through the compound ultra-fine composite particles that is prepared into of high-energy ball milling, high temperature sintering, and reaction in generates.
2. high strength molybdenum doping sheet material according to claim 1 is characterized in that described MoSi
2With Y
2O
3, CeO
2In a kind of, or and Y
2O
3And La
2O
3And CeO
2In two kinds, or and Y
2O
3And La
2O
3And CeO
2Three's mixture makes ultra-fine composite particles in 2: 3～4: 1 ratio high-energy ball milling.
3. high strength molybdenum doping sheet material according to claim 1 and 2, it is characterized in that: the median size of described ultra-fine composite particles is 80～400nm.
4. high strength molybdenum doping sheet material according to claim 3 is characterized in that, described ultra-fine composite particles is 0.1%～3% to add in the pure molybdenum powder by mass ratio.
5. high strength molybdenum doping sheet material according to claim 1 and 2 is characterized in that described MoSi
2Purity is 99%～99.99%, median size＜5 μ m.
6. high strength molybdenum doping sheet material according to claim 1 and 2 is characterized in that described Y
2O
3, CeO
2Or La
2O
3Purity is 99.5～99.99%, median size＜2 μ m.
7. high strength molybdenum doping sheet material according to claim 1 is characterized in that, described pure molybdenum powder median size＜8 μ m.
8. the described high strength molybdenum of claim 3 doping preparation of plates method, it is characterized in that, add to described ultra-fine composite particles in the pure molybdenum powder of median size＜8 μ m by mass ratio 0.1%～3%, mix, compacting, sintering make the sintering slab, again with sintering slab hot rolling cogging, and through the rolling molybdenum board material that obtains, last stress relieving by annealing gets final product.
9. high strength molybdenum doping preparation of plates method according to claim 8 is characterized in that, described sintering temperature is that 1850 ℃～2050 ℃, sintering time 5～10 hours, sintering atmosphere are pure hydrogen; To the sintering slab hot rolling cogging under 1350 ℃～1500 ℃ temperature that obtains, the rolling molybdenum board material that obtains, total deformation is not less than 80%; Under 850 ℃～1050 ℃ annealing temperature, eliminate stress at last.
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| CN102615282A (en) * | 2012-03-27 | 2012-08-01 | 苏州先端稀有金属有限公司 | Processing method for manufacturing wide molybdenum sheet |
| CN102990054A (en) * | 2012-04-01 | 2013-03-27 | 鹤山市沃得钨钼实业有限公司 | Rare earth molybdenum crucible blank and method for manufacturing rare earth molybdenum crucible with same |
| CN103409675A (en) * | 2013-07-04 | 2013-11-27 | 金堆城钼业股份有限公司 | Nano-second-phase-containing Mo-Si-La-Y-Ce alloy and preparation method thereof |
| CN105887029A (en) * | 2016-06-26 | 2016-08-24 | 苏州思创源博电子科技有限公司 | Preparation method of molybdenum alloy plate with hard nitrogen-yttrium-zirconium coating |
| CN105925864A (en) * | 2016-06-04 | 2016-09-07 | 苏州思创源博电子科技有限公司 | Method for preparing high-strength molybdenum alloy board |
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| CN102615282A (en) * | 2012-03-27 | 2012-08-01 | 苏州先端稀有金属有限公司 | Processing method for manufacturing wide molybdenum sheet |
| CN102990054A (en) * | 2012-04-01 | 2013-03-27 | 鹤山市沃得钨钼实业有限公司 | Rare earth molybdenum crucible blank and method for manufacturing rare earth molybdenum crucible with same |
| CN103409675A (en) * | 2013-07-04 | 2013-11-27 | 金堆城钼业股份有限公司 | Nano-second-phase-containing Mo-Si-La-Y-Ce alloy and preparation method thereof |
| CN103409675B (en) * | 2013-07-04 | 2015-04-15 | 金堆城钼业股份有限公司 | Nano-second-phase-containing Mo-Si-La-Y-Ce alloy and preparation method thereof |
| CN105950932A (en) * | 2016-06-04 | 2016-09-21 | 苏州思创源博电子科技有限公司 | Preparation method of molybdenum alloy plate provided with coating |
| CN105925864A (en) * | 2016-06-04 | 2016-09-07 | 苏州思创源博电子科技有限公司 | Method for preparing high-strength molybdenum alloy board |
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| CN106191776A (en) * | 2016-08-20 | 2016-12-07 | 苏州思创源博电子科技有限公司 | A kind of preparation method of molybdenum alloy barium titanate film |
| CN107099716A (en) * | 2017-03-02 | 2017-08-29 | 中广核研究院有限公司 | Interface enhancing molybdenum alloy and preparation method thereof |
| CN108374107A (en) * | 2018-03-07 | 2018-08-07 | 戴爱娟 | A kind of preparation method of the molybdenum alloy plank with silicon coating |
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Application publication date: 20110105 |