CN103159482B - A kind of Mo (Sil-x, Alx)2/ MoSi2the preparation method of complex phase molybden silicide material heater - Google Patents
A kind of Mo (Sil-x, Alx)2/ MoSi2the preparation method of complex phase molybden silicide material heater Download PDFInfo
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Abstract
A kind of Mo (Si1‑x, Alx)2/MoSi2The preparation method of (x=0.1 0.6) complex phase (i.e. C11b and C40) molybden silicide material heater, technique is: by Mo powder, Si powder and Al powder along MoSi2‑MoAl2Line carries out dispensing, puts in ball grinder with ethanol for medium wet mixing 10 20h, and regrind on planetary ball mill 4 6h after drying, is pressed into base substrate under the pressure of 200MPa.Then material base being put into the self-propagating synthesis device with silica window, at room temperature ignites with tungsten filament coil and carry out synthetic reaction, reaction atmosphere is the argon of 0.1MPa.Product M0 (the Si that self-propagating reaction is obtained1‑x, Alx)2/MoSi2Compound phase molybden silicide material and bonding agent dispensing in proportion, extrusion molding after mud refining, process through dry at 100 300 DEG C, 1,400 1550 DEG C of sintering, film forming and after welding, obtain molybden silicide material heater.Solve MoSi2Processing that heater causes because toughness is the lowest, the difficulty of transport, improve the low temperature antioxygenic property of molybden silicide material, extends the service life under low temperature and reducing atmosphere.
Description
Technical field
The present invention relates to a kind of preparation method belonging to heater field, particularly relate to one
Mo(Si1-x, Alx)2/MoSi2(x=0.1-0.6) preparation method of complex phase molybden silicide material heater.
Background technology
MoSi2Due to its fusing point high (2030 DEG C), relatively low density (6.24g/cm3), good heat conduction
The advantages such as electric conductivity and preferably antioxygenic property, from the sixties by health Dynea Austria GmbH development of Sweden
Since Si-Mo rod heater element, as the main flow of industrial resistance heater, metallurgy, electronics,
The industries such as glass, pottery and magnetic material are used widely.Meanwhile, MoSi2Also it is most to have research to open
Send out one of high-temperature structural material of potentiality.But, single-phase molybdenum disilicide material room temperature poor toughness, high temperature
Field strength is low the most easily there is creep, at middle temperature area (400
700 DEG C) easily there is accelerated oxidation
Behavior, and be not suitable under reducing atmosphere such as nitrogen, vacuum using, this all limits molybdenum disilicide
The transport of material, processing and apply further.
Because the defect that above-mentioned existing molybdenum disilicide material exists, the present inventor is based on being engaged in this type of
Product design manufactures practical experience abundant for many years and Professional knowledge, and coordinates the utilization of scientific principle, actively
Research and innovation in addition, to founding a kind of new Mo (Si1-x, Alx)2/MoSi2The preparation side of complex phase heater
Method, it is possible to improve general existing molybdenum disilicide material so that it is have more practicality.Through constantly
Research, design, and after repeatedly studying sample and improving, finally create the basis having practical value
Invention.
Summary of the invention
Present invention is primarily targeted at, overcome the defect that existing molybdenum disilicide material exists, and carry
For a kind of new Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, technology to be solved is asked
Topic is to make which raises the low temperature antioxygenic property of molybden silicide material, extends it in low temperature and reproducibility
Service life under atmosphere.The invention provides a kind of Mo (Si1-x, Alx)2/MoSi2Compound phase silication molybdenum materials
Material heater preparation method, the low temperature antioxygenic property of molybden silicide material can be improved, extend its
In service life under low temperature and reducing atmosphere, it is very suitable for practicality.
Another object of the present invention is to process equipment and execute-in-place is simple, and be conducive to saving energy
Source, reduces production cost.
The object of the invention to solve the technical problems realizes by the following technical solutions.Foundation
A kind of Mo (Si that the present invention proposes1-x, Alx)2/MoSi2Complex phase (i.e. C40 and C11b) molybden silicide material is sent out
The preparation method of hot body, it is characterised in that concrete technology step is: by Mo powder, Si powder and Al powder edge
MoSi2-MoAl2Line carries out dispensing, and with ethanol for medium wet mixing, dried ball milling, at 200MPa
Pressure under be suppressed into base substrate, then material base is put into self-propagating synthesis device, carries out synthesis anti-
Should.The product bonding agent dispensing in proportion obtained by self-propagating reaction, extrusion molding after mud refining, through dry
Dry, sintering, film forming process and after welding, obtain molybden silicide material heater.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaid Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said Mo powder
Particle diameter be 1
10 μm, purity is more than 99%；The particle diameter of described Si powder is 6
18 μm, purity is big
In 99%；The particle diameter of described Al powder is 6
40 μm, purity is more than 99%.
Aforesaid Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein raw material wet ball-milling
10
20h, 100
On planetary ball mill, regrind after drying 4 for 200 DEG C
6h。
Aforesaid Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said self-propagating
In product, Mo (Si1-x, Alx)2With MoSi2Mass ratio be 1: 1
30；Described Mo (Si1-x, Alx)2
X=0.1 in material
0.6。
Aforesaid Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said bonding agent
For in polyvinyl alcohol, dextrin, epoxy resin, clay, aluminium dihydrogen phosphate, silicone type adhesive
A kind of；The content of described bonding agent is Mo (Si1-x, Alx)2/MoSi2The 5 of composite diphase material quality
35%.
Aforesaid Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein mud refining is to mixing all
Till even, fine and smooth, bubble-free and crackle；Extrusion molding pressure is 25
45MPa。
Aforesaid Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said heater
Being incubated 100h respectively at 200,400,600 and 800 DEG C, oxidation rate is below 0.010g m-2·h-1；
The fracture toughness of described heater is up to 10MPa m1/2。
The present invention compared with prior art has clear advantage and beneficial effect.By above-mentioned technical side
Case, the present invention (title) can reach suitable technological progress and practicality, and have in industry extensive
Value, it at least has the advantage that
The present invention solves MoSi2Processing that heater causes because toughness is the lowest, the difficulty of transport, carry
The high low temperature antioxygenic property of molybden silicide material, extends its making under low temperature and reducing atmosphere
Use the life-span.
Present invention process equipment and execute-in-place are simple, and are conducive to saving the energy, reduce production cost.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the present invention's
Technological means, and can being practiced according to the content of description, and in order to allow the above-mentioned of the present invention and
Other objects, features and advantages can become apparent, and below especially exemplified by preferred embodiment, and coordinates attached
Figure, describes in detail as follows.
Accompanying drawing explanation
Nothing
Detailed description of the invention
By further illustrating the technological means and merit that the present invention taked by reaching predetermined goal of the invention
Effect, below in conjunction with accompanying drawing and preferred embodiment, to propose according to the present invention
Mo(Si1-x, Alx)2/MoSi2(x=0.1-0.6) complex phase (i.e. C11b and C40)) molybden silicide material heater
Preparation method, its detailed description of the invention, step, feature and effect thereof, describe in detail as after.
Recent studies indicate that, to MoSi2Carry out alloying and Composite can improve its performance.Its
Middle Al alloying MoSi2The Mo (Si, Al) formed2Composite can not only effectively suppress in warm area
The powder phenomenon-tion in territory, and protectiveness Al formed under high temperature2O3Film can protect matrix not invaded by reduction
The erosion of erosion property atmosphere.To MoSi2Add the second phase and can improve mechanical behavior under high temperature and Toughness,
Wherein Al2O3There is preferable chemical stability, high intensity and and MoSi2There is similar thermal expansion
Coefficient and good chemical compatibility are it is considered to be strengthen MoSi2One of maximally effective reinforcement.
A kind of Mo (Si1-x, Alx)2/MoSi2Complex phase (i.e. C11b and C40)) molybden silicide material heater
Preparation method, its concrete technology step is: by Mo powder, Si powder and Al powder along MoSi2-MoAl2
Line carries out dispensing, puts into ethanol for medium wet mixing 20h in ball grinder, after drying at planetary type ball-milling
Regrind on machine 4h, is pressed into base substrate under the pressure of 200MPa.Then material base is put into quartz glass
In the self-propagating synthesis device of glass observation port, at room temperature ignite with tungsten filament coil and carry out synthetic reaction,
Reaction atmosphere is the argon of 0.1MPa.Product Mo (the Si that self-propagating reaction is obtained1-x, Alx)2/MoSi2
Compound phase (i.e. C11b and C40) molybden silicide material and bonding agent dispensing in proportion, extrusion molding after mud refining,
Through 100
At 300 DEG C be dried, 1400
1550 DEG C of sintering, film forming process and after welding, obtain silication
Mo heater.
A kind of Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said Mo powder
Particle diameter is 1
10 μm, purity is more than 99%；The particle diameter of described Si powder is 6
18 μm, purity is more than
99%；The particle diameter of described Al powder is 6
40 μm, purity is more than 99%.
A kind of Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein raw material wet ball-milling
10
20h, 100
On planetary ball mill, regrind after drying 4 for 200 DEG C
6h。
A kind of Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said self-propagating produces
In thing, Mo (Si1-x, Alx)2With MoSi2Mass ratio be 1: 1
30；Described Mo (Si1-x, Alx)2Material
X=0.1 in material
0.6。
A kind of Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said bonding agent is
In polyvinyl alcohol, dextrin, epoxy resin, clay, aluminium dihydrogen phosphate, silicone type adhesive one
Kind；The content of described bonding agent is Mo (Si1-x, Alx)2/MoSi2The 5 of composite diphase material quality
35%.
A kind of Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein mud refining is to mixing all
Till even, fine and smooth, bubble-free and crackle；Extrusion molding pressure is 25
45MPa。
A kind of Mo (Si1-x, Alx)2/MoSi2The preparation method of complex phase heater, wherein said heater divides
Not being incubated 100h at 200,400,600 and 800 DEG C, oxidation rate is below 0.010g m-2·h-1；
The fracture toughness of described heater is up to 10MPa m1/2。
Embodiment 1
By 1260g Mo powder, 700gSi powder and 40gAl powder along Mo (Si0.9, Al0.1)2/MoSi2Line
Carrying out dispensing, put into ethanol for medium wet mixing 20h in ball grinder, 200 DEG C dried at planetary ball
Regrind on grinding machine 6h, is suppressed into the base substrate of Φ 360 × 300mm under the pressure of 200MPa.Then will
Material base puts into the self-propagating synthesis device with silica window, at room temperature uses tungsten filament coil
Igniting and carry out synthetic reaction, reaction atmosphere is the argon of 0.1MPa, obtains Mo (Si0.9, Al0.1)2/MoSi2
Composite diphase material, Mo (Si0.9, Al0.1)2And MoSi2Mass ratio be 1: 1.By Mo (Si0.9, Al0.1)2/MoSi2
Composite diphase material and 100g polyvinyl alcohol, mud refining to mix homogeneously, exquisiteness, bubble-free and crackle are
Only, extrusion molding under 45MPa pressure, dry at 100 DEG C, 1400 DEG C of sintering, film forming process and weldering
After connecing, obtain molybden silicide material heater.Heater is incubated 100h, oxidation speed respectively at 600 DEG C
Rate is 0.009g m-2·h-1, the fracture toughness of heater is 9.5MPa m1/2。
Embodiment 2
By 1260g Mo powder, 500gSi powder and 240gAl powder along Mo (Si0.4, Al0.6)2/MoSi2Line
Carry out dispensing, put into ethanol for medium wet mixing 10h in ball grinder, be expert at after drying after drying for 100 DEG C
Regrind on planetary ball mill 4h, is suppressed into the base substrate of Φ 360 × 300mm under the pressure of 200MPa.
Then material base is put into the self-propagating synthesis device with silica window, at room temperature uses tungsten
Wire coil is ignited and is carried out synthetic reaction, and reaction atmosphere is the argon of 0.1MPa, obtains
Mo(Si0.4, Al0.6)2/MoSi2Composite diphase material, Mo (Si0.4, Al0.6)2And MoSi2Mass ratio be 1: 1.Will
Mo(Si0.4, Al0.6)2/MoSi2Composite diphase material and 100g dextrin mixing, mud refining to mix homogeneously, exquisiteness,
Till bubble-free and crackle, extrusion molding under 25MPa pressure, be dried at 300 DEG C, 1550 DEG C of sintering,
Film forming processes and after welding, obtains molybden silicide material heater.Heater is incubated respectively at 800 DEG C
100h, oxidation rate is 0.009g m-2·h-1, the fracture toughness of heater is 9.8MPa m1/2。
Embodiment 3
By 1260g Mo powder, 700gSi powder and 40gAl powder along Mo (Si0.9, Al0.1)2/MoSi2Line
Carry out dispensing, put into ethanol for medium wet mixing 20h in ball grinder, be expert at after drying after drying for 200 DEG C
Regrind on planetary ball mill 6h, is suppressed into the base substrate of Φ 360 × 300mm under the pressure of 200MPa.
Then material base is put into the self-propagating synthesis device with silica window, at room temperature uses tungsten
Wire coil is ignited and is carried out synthetic reaction, and reaction atmosphere is the argon of 0.1MPa, obtains
Mo(Si0.9, Al0.1)2/MoSi2Composite diphase material, Mo (Si0.9, Al0.1)2And MoSi2Mass ratio be 1: 1.Will
Mo(Si0.9, Al0.1)2/MoSi2Composite diphase material and 700g clay mixing, mud refining to mix homogeneously, exquisiteness,
Till bubble-free and crackle, extrusion molding under 45MPa pressure, be dried at 100 DEG C, 1400 DEG C of sintering,
Film forming processes and after welding, obtains molybden silicide material heater.Heater is incubated respectively at 400 DEG C
100h, oxidation rate is 0.008g m-2·h-1, the fracture toughness of heater is 9.5MPa m1/2。
Embodiment 4
By 1260g Mo powder, 500gSi powder and 240gAl powder along Mo (Si0.4, Al0.6)2/MoSi2Line
Carrying out dispensing, put into ethanol for medium wet mixing 10h in ball grinder, 100 DEG C dried at planetary ball
Regrind on grinding machine 4h, is suppressed into the base substrate of Φ 360 × 300mm under the pressure of 200MPa.Then will
Material base puts into the self-propagating synthesis device with silica window, at room temperature uses tungsten filament coil
Igniting and carry out synthetic reaction, reaction atmosphere is the argon of 0.1MPa, obtains Mo (Si0.4, Al0.6)2/MoSi2
Composite diphase material, Mo (Si0.4, Al0.6)2And MoSi2Mass ratio be 1: 1.By Mo (Si0.4, Al0.6)2/MoSi2
Composite diphase material and the mixing of 100g aluminium dihydrogen phosphate, mud refining to mix homogeneously, exquisiteness, bubble-free and crackle
Till, extrusion molding under 25MPa pressure, be dried at 300 DEG C, the process of 1550 DEG C of sintering, film forming and
After welding, obtain molybden silicide material heater.Heater is incubated 100h, oxidation respectively at 200 DEG C
Speed is 0.006g m-2·h-1, the fracture toughness of heater is 9.8MPa m1/2。
Embodiment 5
By 1260g Mo powder, 700gSi powder and 40gAl powder along Mo (Si0.9, Al0.1)2/MoSi2Line
Carrying out dispensing, put into ethanol for medium wet mixing 20h in ball grinder, 200 DEG C dried at planetary ball
Regrind on grinding machine 6h, is suppressed into the base substrate of Φ 360 × 300mm under the pressure of 200MPa.Then will
Material base puts into the self-propagating synthesis device with silica window, at room temperature uses tungsten filament coil
Igniting and carry out synthetic reaction, reaction atmosphere is the argon of 0.1MPa, obtains Mo (Si0.9, Al0.1)2/MoSi2
Composite diphase material, Mo (Si0.9, Al0.1)2And MoSi2Mass ratio be 1: 1.By Mo (Si0.9, Al0.1)2/MoSi2
Composite diphase material and the mixing of 700g epoxy resin, mud refining to mix homogeneously, exquisiteness, bubble-free and crackle are
Only, extrusion molding under 45MPa pressure, dry at 300 DEG C, 1400 DEG C of sintering, film forming process and weldering
After connecing, obtain molybden silicide material heater.Heater is incubated 100h, oxidation speed respectively at 400 DEG C
Rate is 0.008g m-2·h-1, the fracture toughness of heater is 9.5MPa m1/2。
Embodiment 6
By 19530g Mo powder, 11230gSi powder and 240gAl powder along Mo (Si0.4, Al0.6)2/MoSi2
Line carries out dispensing, puts into ethanol for medium wet mixing 10h in ball grinder, and 100 DEG C dried at planet
Regrind on formula ball mill 6h, is suppressed into the base substrate of Φ 360 × 300mm under the pressure of 200MPa.So
After material base is put into the self-propagating synthesis device with silica window, at room temperature use tungsten filament
Coil ignites and carries out synthetic reaction, and reaction atmosphere is the argon of 0.1MPa, obtains
Mo(Si0.4, Al0.6)2/MoSi2Composite diphase material, Mo (Si0.4, Al0.6)2And MoSi2Mass ratio be 1: 30.
By Mo (Si0.4, Al0.6)2/MoSi2Composite diphase material and the mixing of 1510g silicone type adhesive, mud refining is to mixed
Till closing uniform, fine and smooth, bubble-free and crackle, extrusion molding under 25MPa pressure, dry at 300 DEG C
Dry, 1550 DEG C of sintering, film forming process and after welding, obtain molybden silicide material heater.Heater divides
Not being incubated 600h at 200 DEG C, oxidation rate is 0.001g m-2·h-1, the fracture toughness of heater is
8.8MPa·m1/2。
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any form
On restriction, although the present invention is disclosed above with preferred embodiment, but is not limited to this
Bright, any those skilled in the art, in the range of without departing from technical solution of the present invention, when can profit
Make a little change with the technology contents of the disclosure above or be modified to the Equivalent embodiments of equivalent variations, but
Every content without departing from technical solution of the present invention, the technical spirit of the foundation present invention is to above example
Any simple modification, equivalent variations and the modification made, all still falls within the scope of technical solution of the present invention
In.
Claims (2)
1. a Mo (Si1-x,Alx)2/MoSi2The preparation method of complex phase molybden silicide material heater,
It is characterized in that concrete technology step is:
(1) by Mo powder, Si powder and Al powder along MoSi2-MoAl2Line carries out dispensing, ball
Mill wet mixing 10-20h, after drying, regrind 4-6h；
(2) self-propagating synthesis reaction is carried out after step (1) gained material being pressed into base substrate,
The product that self-propagating reaction is obtained and bonding agent dispensing in proportion, extrusion molding after mud refining, warp
Be dried, sintering, film forming process and after welding, obtain molybden silicide material heater；
(3) by step (2) gained heater at 200 DEG C or 400 DEG C or 600 DEG C or 800 DEG C
Lower insulation 100h, oxidation rate is below 0.010g m-2·h-1, obtain fracture toughness up to
10MPa·m1/2Mo (Si1-x,Alx)2/MoSi2Complex phase molybden silicide material heater.
2. according to the Mo (Si described in claim 11-x,Alx)2/MoSi2Complex phase molybden silicide material is sent out
The preparation method of hot body, it is characterised in that extrusion molding pressure is 25-45MPa.
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| CN104163629A (en) * | 2014-07-03 | 2014-11-26 | 厦门理工学院 | An embedded carbon nanotube/molybdenum disilicide composite material and a preparing method thereof |
| CN106278280B (en) * | 2016-08-09 | 2019-05-17 | 中原工学院 | A kind of preparation method of composite ceramics that resisting PEST |
| CN106241814B (en) * | 2016-08-25 | 2018-07-31 | 金堆城钼业股份有限公司 | A kind of method of constituency self-propagating synthesis molybdenum disilicide powder |
| GB2584911A (en) * | 2019-06-21 | 2020-12-23 | Tallinn Univ Of Technology | A method of direct laser shaping ceramic-intermetallic composites of MoSi2 and/or Mo(Si,Al)2 and Al and/or Al alloys |
| CN115141021B (en) * | 2022-08-31 | 2023-01-03 | 钢研昊普科技有限公司 | Modified molybdenum disilicide material and preparation method thereof |
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| CN1560302A (en) * | 2004-03-02 | 2005-01-05 | 湖南科技大学 | Speed preparing composite material powder with MoSi2 base and its method of sintered body |
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