CN103159482A - A method for preparing Mo (Sil-x, alx)2/MoSi2complex-phase molybdenum silicide heating element - Google Patents
A method for preparing Mo (Sil-x, alx)2/MoSi2complex-phase molybdenum silicide heating element Download PDFInfo
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- CN103159482A CN103159482A CN2011104091468A CN201110409146A CN103159482A CN 103159482 A CN103159482 A CN 103159482A CN 2011104091468 A CN2011104091468 A CN 2011104091468A CN 201110409146 A CN201110409146 A CN 201110409146A CN 103159482 A CN103159482 A CN 103159482A
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Abstract
The invention relates to a preparation method for a Mo(Sil-x, Alx)2/MoSi2 complex phase (i.e. C11b and C40) molybdenum silicide material heating element. The preparation method comprises the processes of proportioning Mo powder, Si powder and Al powder along a connecting line of MoSi2-MoAl2; adding the materials into ball grinding pots; wet-grinding for 10-20 h; drying, grinding for 4-6 hours on a planetary ball mill; pressing the grinded materials into green bodies at a pressure of 200 MPa; putting the green bodies into a self-propagating synthesis device with a quartz glass observation hole; igniting a synthesis reaction by using a tungsten wire coil at a room temperature, wherein a reaction atmosphere is 0.1 MPa argon; proportioning a product of Mo(Sil-x, Alx)2/MoSi2 complex phase molybdenum silicide material obtained by the self-propagating reaction with a binding agent according to a proportion; extrusion molding after pug milling; drying at a temperature of 100-300 DEG C; sintering at a temperature of 1,400-1,550 DEG C; film processing and welding to obtain the molybdenum silicide material heating element. Difficulties of processing and transporting caused by two low toughness of a MoSi2 heating element are solved; low temperature oxidation resistance of the molybdenum silicide material is increased; and service life of the molybdenum silicide material heating element at a low temperature and under a reducing atmosphere is prolonged.
Description
Technical field
The present invention relates to a kind of preparation method who belongs to the heating element field, particularly relate to a kind of Mo (Si
1-x, Al
x)
2/ MoSi
2(x=0.1-0.6) preparation method of complex phase molybden silicide material heating element.
Background technology
MoSi
2Due to its fusing point high (2030 ℃), lower density (6.24g/cm
3), good heat-conductivity conducting and the advantage such as antioxidant property preferably, since the Si-Mo rod Heating element of the sixties by health Dynea Austria GmbH development of Sweden, as the main flow of industrial resistance heating element, be used widely in industries such as metallurgy, electronics, glass, pottery and magneticsubstances.Simultaneously, MoSi
2It is also one of high-temperature structural material that has most the research and development potentiality.But, single-phase molybdenum disilicide material room temperature poor toughness, high-temperature area intensity is low, and creep very easily occurs again, at middle temperature area (400
700 ℃) the accelerated oxidation behavior easily occurs, and be not suitable for using under reducing atmosphere such as nitrogen, vacuum, this has all limited transportation, the processing of molybdenum disilicide material and has further used.
Because the defective that above-mentioned existing molybdenum disilicide material exists, the inventor is based on being engaged in this type of product design manufacturing abundant practical experience and expertise for many years, and coordinates the utilization of scientific principle, and positive research and innovation in addition is to founding a kind of new Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element can improve general existing molybdenum disilicide material, makes it have more practicality.Through constantly research, design, and through after repeatedly studying sample and improvement, finally create the present invention who has practical value.
Summary of the invention
Main purpose of the present invention is, overcomes the defective that existing molybdenum disilicide material exists, and a kind of new Mo (Si is provided
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, technical problem to be solved make its low temperature antioxidant property that has improved molybden silicide material, have extended its work-ing life under low temperature and reducing atmosphere.The invention provides a kind of Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of compound phase molybden silicide material heating element can improve the low temperature antioxidant property of molybden silicide material, extends its work-ing life under low temperature and reducing atmosphere, is very suitable for practicality.
Another object of the present invention is to processing unit and execute-in-place is simple, and be conducive to save energy, reduce production costs.
The object of the invention to solve the technical problems realizes by the following technical solutions.A kind of Mo (Si according to the present invention's proposition
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase (being C40 and C11b) molybden silicide material heating element is characterized in that the concrete technology step is: with Mo powder, Si powder and Al powder along MoSi
2-MoAl
2Line is prepared burden, and take alcohol as the medium wet mixing, dry rear ball milling is suppressed into base substrate under the pressure of 200MPa, then material base is put into from propagating synthesizer, carries out building-up reactions.The product wedding agent that self-propagating reaction obtains is prepared burden in proportion, extrusion moulding after mud refining, drying, sintering, film forming obtain the molybden silicide material heating element after processing and welding.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaid Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, the particle diameter of wherein said Mo powder is 1
10 μ m, purity is greater than 99%; The particle diameter of described Si powder is 6
18 μ m, purity is greater than 99%; The particle diameter of described Al powder is 6
40 μ m, purity is greater than 99%.
Aforesaid Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein the raw material wet ball-milling 10
20h, 100
Regrind 4 after 200 ℃ of dryings on planetary ball mill
6h.
Aforesaid Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein said oneself spreads in product, Mo (Si
1-x, Al
x)
2With MoSi
2Mass ratio be 1: 1
30; Described Mo (Si
1-x, Al
x)
2X=0.1 in material
0.6.
Aforesaid Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein said wedding agent is a kind of in polyvinyl alcohol, dextrin, epoxy resin, clay, aluminium dihydrogen phosphate, silicone resin type tackiness agent; The content of described wedding agent is Mo (Si
1-x, Al
x)
2/ MoSi
25 of composite diphase material quality
35%.
Aforesaid Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein mud refining to mix, fine and smooth, without till bubble and crackle; Extrusion moulding pressure is 25
45MPa.
Aforesaid Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein said heating element is incubated 100h respectively under 200,400,600 and 800 ℃, and rate of oxidation is all lower than 0.010gm
-2H
-1The fracture toughness property of described heating element is up to 10MPam
1/2
The present invention compared with prior art has obvious advantage and beneficial effect.By technique scheme, the present invention's (title) can reach suitable technical progress and practicality, and has the extensive utility value on industry, and it has following advantages at least:
The invention solves MoSi
2Heating element has improved the low temperature antioxidant property of molybden silicide material because of the difficulty of the too low processing that causes of toughness, transportation, has extended its work-ing life under low temperature and reducing atmosphere.
Processing unit of the present invention and execute-in-place are simple, and are conducive to save energy, reduce production costs.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, for can clearer understanding technique means of the present invention, and can be implemented according to the content of specification sheets, and for above and other purpose of the present invention, feature and advantage can be become apparent, below especially exemplified by preferred embodiment, and the cooperation accompanying drawing, be described in detail as follows.
Description of drawings
Nothing
Embodiment
Reach for further setting forth the present invention technique means and the effect that predetermined goal of the invention is taked, below in conjunction with accompanying drawing and preferred embodiment, to the Mo (Si of foundation the present invention proposition
1-x, Al
x)
2/ MoSi
2(x=0.1-0.6) complex phase (being C11b and the C40)) preparation method of molybden silicide material heating element, its embodiment, step, feature and effect thereof are described in detail as follows.
Studies show that in recent years is to MoSi
2Carry out alloying and Composite and can improve its performance.Al alloying MoSi wherein
2The Mo (Si, Al) that forms
2The powder phenomenon-tion of temperature area during matrix material not only can suppress effectively, and the protectiveness Al that forms under high temperature
2O
3Film can protect matrix not reduced the erosion of sever atmosphere.To MoSi
2Add second-phase and can improve mechanical behavior under high temperature and Toughness, wherein Al
2O
3Has chemical stability preferably, high intensity and and MoSi
2Have similar thermal expansivity and good chemical compatibility, be considered to strengthen MoSi
2One of the most effective reinforcement.
A kind of Mo (Si
1-x, Al
x)
2/ MoSi
2Complex phase (being C11b and C40)) preparation method of molybden silicide material heating element, its concrete technology step is: with Mo powder, Si powder and Al powder along MoSi
2-MoAl
2Line is prepared burden, and puts into ball grinder take alcohol as medium wet mixing 20h, and the dry rear 4h that regrinds on planetary ball mill is pressed into base substrate under the pressure of 200MPa.Then material base is put into silica window from propagating synthesizer, at room temperature ignite with tungsten filament coil and carry out building-up reactions, reaction atmosphere is the argon gas of 0.1MPa.Product Mo (the Si that self-propagating reaction is obtained
1-x, Al
x)
2/ MoSi
2Compound phase (being C11b and C40) molybden silicide material and wedding agent are prepared burden in proportion, and extrusion moulding after mud refining is through 100
Drying, 1400 under 300 ℃
After 1550 ℃ of sintering, film forming are processed and welded, obtain the molybden silicide material heating element.
A kind of Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, the particle diameter of wherein said Mo powder is 1
10 μ m, purity is greater than 99%; The particle diameter of described Si powder is 6
18 μ m, purity is greater than 99%; The particle diameter of described Al powder is 6
40 μ m, purity is greater than 99%.
A kind of Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein the raw material wet ball-milling 10
20h, 100
Regrind 4 after 200 ℃ of dryings on planetary ball mill
6h.
A kind of Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein said oneself spreads in product, Mo (Si
1-x, Al
x)
2With MoSi
2Mass ratio be 1: 1
30; Described Mo (Si
1-x, Al
x)
2X=0.1 in material
0.6.
A kind of Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein said wedding agent is a kind of in polyvinyl alcohol, dextrin, epoxy resin, clay, aluminium dihydrogen phosphate, silicone resin type tackiness agent; The content of described wedding agent is Mo (Si
1-x, Al
x)
2/ MoSi
25 of composite diphase material quality
35%.
A kind of Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein mud refining to mix, fine and smooth, without till bubble and crackle; Extrusion moulding pressure is 25
45MPa.
A kind of Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, wherein said heating element is incubated 100h respectively under 200,400,600 and 800 ℃, and rate of oxidation is all lower than 0.010gm
-2H
-1The fracture toughness property of described heating element is up to 10MPam
1/2
Embodiment 1
With 1260g Mo powder, 700gSi powder and 40gAl powder along Mo (Si
0.9, Al
0.1)
2/ MoSi
2Line is prepared burden, and puts into ball grinder take alcohol as medium wet mixing 20h, and the 6h that regrinds on planetary ball mill after 200 ℃ of dryings is suppressed into the base substrate of Φ 360 * 300mm under the pressure of 200MPa.Then material base is put into silica window from propagating synthesizer, at room temperature ignite with tungsten filament coil and carry out building-up reactions, reaction atmosphere is the argon gas of 0.1MPa, obtains Mo (Si
0.9, Al
0.1)
2/ MoSi
2Composite diphase material, Mo (Si
0.9, Al
0.1)
2And MoSi
2Mass ratio be 1: 1.With Mo (Si
0.9, Al
0.1)
2/ MoSi
2Composite diphase material and 100g polyvinyl alcohol mix, mud refining to mix, fine and smooth, without till bubble and crackle, extrusion moulding under 45MPa pressure, through dry under 100 ℃, 1400 ℃ of sintering, film forming process and welding after, obtain the molybden silicide material heating element.Heating element is incubated 100h respectively under 600 ℃, rate of oxidation is 0.009gm
-2H
-1, the fracture toughness property of heating element is 9.5MPam
1/2
Embodiment 2
With 1260g Mo powder, 500gSi powder and 240gAl powder along Mo (Si
0.4, Al
0.6)
2/ MoSi
2Line is prepared burden, and puts into ball grinder take alcohol as medium wet mixing 10h, and the 4h that regrinds on planetary ball mill after dry after 100 ℃ of dryings is suppressed into the base substrate of Φ 360 * 300mm under the pressure of 200MPa.Then material base is put into silica window from propagating synthesizer, at room temperature ignite with tungsten filament coil and carry out building-up reactions, reaction atmosphere is the argon gas of 0.1MPa, obtains Mo (Si
0.4, Al
0.6)
2/ MoSi
2Composite diphase material, Mo (Si
0.4, Al
0.6)
2And MoSi
2Mass ratio be 1: 1.With Mo (Si
0.4, Al
0.6)
2/ MoSi
2Composite diphase material and 100g dextrin mix, mud refining to mix, fine and smooth, without till bubble and crackle, extrusion moulding under 25MPa pressure, through dry under 300 ℃, 1550 ℃ of sintering, film forming process and welding after, obtain the molybden silicide material heating element.Heating element is incubated 100h respectively under 800 ℃, rate of oxidation is 0.009gm
-2H
-1, the fracture toughness property of heating element is 9.8MPam
1/2
Embodiment 3
With 1260g Mo powder, 700gSi powder and 40gAl powder along Mo (Si
0.9, Al
0.1)
2/ MoSi
2Line is prepared burden, and puts into ball grinder take alcohol as medium wet mixing 20h, and the 6h that regrinds on planetary ball mill after dry after 200 ℃ of dryings is suppressed into the base substrate of Φ 360 * 300mm under the pressure of 200MPa.Then material base is put into silica window from propagating synthesizer, at room temperature ignite with tungsten filament coil and carry out building-up reactions, reaction atmosphere is the argon gas of 0.1MPa, obtains Mo (Si
0.9, Al
0.1)
2/ MoSi
2Composite diphase material, Mo (Si
0.9, Al
0.1)
2And MoSi
2Mass ratio be 1: 1.With Mo (Si
0.9, Al
0.1)
2/ MoSi
2Composite diphase material and 700g clay mix, mud refining to mix, fine and smooth, without till bubble and crackle, extrusion moulding under 45MPa pressure, through dry under 100 ℃, 1400 ℃ of sintering, film forming process and welding after, obtain the molybden silicide material heating element.Heating element is incubated 100h respectively under 400 ℃, rate of oxidation is 0.008gm
-2H
-1, the fracture toughness property of heating element is 9.5MPam
1/2
Embodiment 4
With 1260g Mo powder, 500gSi powder and 240gAl powder along Mo (Si
0.4, Al
0.6)
2/ MoSi
2Line is prepared burden, and puts into ball grinder take alcohol as medium wet mixing 10h, and the 4h that regrinds on planetary ball mill after 100 ℃ of dryings is suppressed into the base substrate of Φ 360 * 300mm under the pressure of 200MPa.Then material base is put into silica window from propagating synthesizer, at room temperature ignite with tungsten filament coil and carry out building-up reactions, reaction atmosphere is the argon gas of 0.1MPa, obtains Mo (Si
0.4, Al
0.6)
2/ MoSi
2Composite diphase material, Mo (Si
0.4, Al
0.6)
2And MoSi
2Mass ratio be 1: 1.With Mo (Si
0.4, Al
0.6)
2/ MoSi
2Composite diphase material and 100g aluminium dihydrogen phosphate mix, mud refining to mix, fine and smooth, without till bubble and crackle, extrusion moulding under 25MPa pressure, through dry under 300 ℃, 1550 ℃ of sintering, film forming process and welding after, obtain the molybden silicide material heating element.Heating element is incubated 100h respectively under 200 ℃, rate of oxidation is 0.006gm
-2H
-1, the fracture toughness property of heating element is 9.8MPam
1/2
Embodiment 5
With 1260g Mo powder, 700gSi powder and 40gAl powder along Mo (Si
0.9, Al
0.1)
2/ MoSi
2Line is prepared burden, and puts into ball grinder take alcohol as medium wet mixing 20h, and the 6h that regrinds on planetary ball mill after 200 ℃ of dryings is suppressed into the base substrate of Φ 360 * 300mm under the pressure of 200MPa.Then material base is put into silica window from propagating synthesizer, at room temperature ignite with tungsten filament coil and carry out building-up reactions, reaction atmosphere is the argon gas of 0.1MPa, obtains Mo (Si
0.9, Al
0.1)
2/ MoSi
2Composite diphase material, Mo (Si
0.9, Al
0.1)
2And MoSi
2Mass ratio be 1: 1.With Mo (Si
0.9, Al
0.1)
2/ MoSi
2Composite diphase material and 700g epoxy resin mix, mud refining to mix, fine and smooth, without till bubble and crackle, extrusion moulding under 45MPa pressure, through dry under 300 ℃, 1400 ℃ of sintering, film forming process and welding after, obtain the molybden silicide material heating element.Heating element is incubated 100h respectively under 400 ℃, rate of oxidation is 0.008gm
-2H
-1, the fracture toughness property of heating element is 9.5MPam
1/2
Embodiment 6
With 19530g Mo powder, 11230gSi powder and 240gAl powder along Mo (Si
0.4, Al
0.6)
2/ MoSi
2Line is prepared burden, and puts into ball grinder take alcohol as medium wet mixing 10h, and the 6h that regrinds on planetary ball mill after 100 ℃ of dryings is suppressed into the base substrate of Φ 360 * 300mm under the pressure of 200MPa.Then material base is put into silica window from propagating synthesizer, at room temperature ignite with tungsten filament coil and carry out building-up reactions, reaction atmosphere is the argon gas of 0.1MPa, obtains Mo (Si
0.4, Al
0.6)
2/ MoSi
2Composite diphase material, Mo (Si
0.4, Al
0.6)
2And MoSi
2Mass ratio be 1: 30.With Mo (Si
0.4, Al
0.6)
2/ MoSi
2Composite diphase material and 1510g silicone resin type tackiness agent mix, mud refining to mix, fine and smooth, without till bubble and crackle, extrusion moulding under 25MPa pressure, through dry under 300 ℃, 1550 ℃ of sintering, film forming process and welding after, obtain the molybden silicide material heating element.Heating element is incubated 600h respectively under 200 ℃, rate of oxidation is 0.001gm
-2H
-1, the fracture toughness property of heating element is 8.8MPam
1/2
the above, it is only preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, although the present invention discloses as above with preferred embodiment, yet be not to limit the present invention, any those skilled in the art, within not breaking away from the technical solution of the present invention scope, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be the content that does not break away from technical solution of the present invention, any simple modification that foundation technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (7)
1. Mo (Si
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase (being C40 and C11b) molybden silicide material heating element is characterized in that the concrete technology step is: with Mo powder, Si powder and Al powder along MoSi
2-MoAl
2Line is prepared burden, and take alcohol as the medium wet mixing, dry rear ball milling is suppressed into base substrate under the pressure of 200MPa, then material base is put into from propagating synthesizer, carries out building-up reactions.The product wedding agent that self-propagating reaction obtains is prepared burden in proportion, extrusion moulding after mud refining, drying, sintering, film forming obtain the molybden silicide material heating element after processing and welding.
2. Mo (Si according to claim 1
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element, the particle diameter that it is characterized in that described Mo powder is 1
10 μ m, purity is greater than 99%; The particle diameter of described Si powder is 6
18 μ m, purity is greater than 99%; The particle diameter of described Al powder is 6
40 μ m, purity is greater than 99%.
5. Mo (Si according to claim 1
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element is characterized in that described wedding agent is a kind of in polyvinyl alcohol, dextrin, epoxy resin, clay, aluminium dihydrogen phosphate, silicone resin type tackiness agent; The content of described wedding agent is Mo (Si
1-x, Al
x)
2/ MoSi
25 of composite diphase material quality
35%.
7. Mo (Si according to claim 1
1-x, Al
x)
2/ MoSi
2The preparation method of complex phase heating element is characterized in that described heating element is incubated 100h respectively under 200,400,600 and 800 ℃, and rate of oxidation is all lower than 0.010gm
-2H
-1The fracture toughness property of described heating element is up to 10MPam
1/2
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN106241814A (en) * | 2016-08-25 | 2016-12-21 | 金堆城钼业股份有限公司 | A kind of method of constituency self-propagating synthesis molybdenum disilicide powder body |
CN106278280A (en) * | 2016-08-09 | 2017-01-04 | 中原工学院 | A kind of preparation method of the composite ceramics resisting PEST |
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 |
CN115141021A (en) * | 2022-08-31 | 2022-10-04 | 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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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN106278280A (en) * | 2016-08-09 | 2017-01-04 | 中原工学院 | A kind of preparation method of the composite ceramics resisting PEST |
CN106278280B (en) * | 2016-08-09 | 2019-05-17 | 中原工学院 | A kind of preparation method of composite ceramics that resisting PEST |
CN106241814A (en) * | 2016-08-25 | 2016-12-21 | 金堆城钼业股份有限公司 | A kind of method of constituency self-propagating synthesis molybdenum disilicide powder body |
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 |
CN115141021A (en) * | 2022-08-31 | 2022-10-04 | 钢研昊普科技有限公司 | Modified molybdenum disilicide material and preparation method thereof |
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 |
Also Published As
Publication number | Publication date |
---|---|
CN103159482B (en) | 2016-08-24 |
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