CN100460111C - A kind of high-strength molybdenum disilicide composite material and preparation method thereof - Google Patents
A kind of high-strength molybdenum disilicide composite material and preparation method thereof Download PDFInfo
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- CN100460111C CN100460111C CNB2007100632406A CN200710063240A CN100460111C CN 100460111 C CN100460111 C CN 100460111C CN B2007100632406 A CNB2007100632406 A CN B2007100632406A CN 200710063240 A CN200710063240 A CN 200710063240A CN 100460111 C CN100460111 C CN 100460111C
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- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 229910021343 molybdenum disilicide Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000011863 silicon-based powder Substances 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000010802 sludge Substances 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 238000005452 bending Methods 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229910016006 MoSi Inorganic materials 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910020968 MoSi2 Inorganic materials 0.000 description 1
- 229910017311 Mo—Mo Inorganic materials 0.000 description 1
- 229910017305 Mo—Si Inorganic materials 0.000 description 1
- 229910008045 Si-Si Inorganic materials 0.000 description 1
- 229910008423 Si—B Inorganic materials 0.000 description 1
- 229910006411 Si—Si Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明属于无机材料技术领域，特别是提供了一种高强度的二硅化钼复合材料及其制备方法。具体是一种包含有Mo(Si1-xAlx)2和蒙脱石的混合物制备成的复合材料。The invention belongs to the technical field of inorganic materials, and in particular provides a high-strength molybdenum disilicide composite material and a preparation method thereof. Specifically, it is a composite material prepared from a mixture of Mo(Si 1-x Al x ) 2 and montmorillonite.
背景技术 Background technique
在MoSi2晶体结构中，Si-Si原子组成共价键链，Mo-Mo原子属于金属键结合，Mo-Si原子介于其间，因此MoSi2具有金属键和共价键共存的特征。二硅化钼材料可以制备成发热材料、涂层材料、电极材料，二硅化钼还是一种非常有前途的高温结构材料。In the MoSi 2 crystal structure, Si-Si atoms form a covalent bond chain, Mo-Mo atoms belong to metal bonding, and Mo-Si atoms are in between, so MoSi 2 has the characteristics of coexistence of metal bonds and covalent bonds. Molybdenum disilicide materials can be prepared into heating materials, coating materials, electrode materials, and molybdenum disilicide is also a very promising high-temperature structural material.
但是二硅化钼存在室温韧性低、高温强度低，烧结温度高、原材料成本高的缺点。这些缺点都限制了二硅化钼的应用。However, molybdenum disilicide has the disadvantages of low room temperature toughness, low high temperature strength, high sintering temperature and high cost of raw materials. These disadvantages limit the application of molybdenum disilicide.
中国专利CN1583669A公布了一种制备二硅化钼/三氧化二铝复合材料的方法，采用热压工艺，所得复合材料的断裂韧性最高为3.9MPa.m1/2。中国专利CN1560302A公布了一种快速制备MoSi2基复合材料的方法，其烧结温度达到1400～1600度。中国专利CN1391539A公布了一种具有高强度的硅化钼材料，其添加的增强相为ZrO2。中国专利CN1642875A公布了硅化钼型加热元件的制造方法，形成化合物Mo(Si1-xAlx)2和Al2O3，其中X处于0.4～0.6的范围之内，Al含量较高。Summer E等制备了一种Mo—Si—B金属间化合物材料，在制备过程中采用石蜡基粘结剂(Summer E，et al，Intermetallics，2000，8：1169—1174)。Chinese patent CN1583669A discloses a method for preparing a molybdenum disilicide/aluminum oxide composite material. The fracture toughness of the obtained composite material is up to 3.9 MPa.m 1/2 by using a hot pressing process. Chinese patent CN1560302A discloses a method for rapidly preparing MoSi2- based composite materials, and its sintering temperature reaches 1400-1600 degrees. Chinese patent CN1391539A discloses a molybdenum silicide material with high strength, and the added reinforcing phase is ZrO 2 . Chinese patent CN1642875A discloses a method for manufacturing a molybdenum silicide heating element, forming compounds Mo(Si 1-x Al x ) 2 and Al 2 O 3 , wherein X is in the range of 0.4-0.6 and the Al content is relatively high. Summer E et al. prepared a Mo—Si—B intermetallic compound material, using a paraffin-based binder in the preparation process (Summer E, et al, Intermetallics, 2000, 8: 1169—1174).
发明内容 Contents of the invention
本发明的目的在于提供一种高强度的二硅化钼复合材料及其制备方法，实现了比单一MoSi2性能优越，室温弯曲强度、断裂韧性和压缩强度高的二硅化钼复合材料。The object of the present invention is to provide a high-strength molybdenum disilicide composite material and its preparation method, which realizes a molybdenum disilicide composite material with superior performance than single MoSi 2 and high room temperature bending strength, fracture toughness and compressive strength.
本发明二硅化钼复合材料的基体为Mo(Si1-xAlx)2，其中X处于0.025～0.300的范围之内；是一种包含有80～95wt％Mo(Si1-xAlx)2和5～20wt％蒙脱石制备成的复合材料。The matrix of the molybdenum disilicide composite material of the present invention is Mo(Si 1 - x Al x ) 2 , where X is in the range of 0.025-0.300; 2 and 5-20wt% montmorillonite prepared composite material.
本发明的制备工艺为：The preparation process of the present invention is:
1、原料的准备1. Preparation of raw materials
a、将纯度大于98％的铝粉、纯度大于98％的钼粉、纯度大于98％的硅粉，按照1.675mol％～20.1mol％铝、33mol％钼、46.9mol％～65.325mol％硅的摩尔比例混合均匀，采用自蔓延反应合成的工艺得到Mo(Si1-xAlx)2，其中X处于0.025～0.300的范围之内。a. The aluminum powder with a purity greater than 98%, the molybdenum powder with a purity greater than 98%, and the silicon powder with a purity greater than 98% are mixed according to the formula of 1.675mol% to 20.1mol% aluminum, 33mol% molybdenum, and 46.9mol% to 65.325mol% silicon The molar ratio is mixed evenly, and Mo(Si 1-x Al x ) 2 is obtained by adopting a self-propagating reaction synthesis process, wherein X is in the range of 0.025-0.300.
b、将所得Mo(Si1-xAlx)2；按照80～95wt％Mo(Si1-xAlx)2和5～20wt％蒙脱石粉末的重量比例配料；再加入6～13重量％蒸馏水；混合均匀；形成泥料。b. The obtained Mo(Si 1-x Al x ) 2 ; according to the weight ratio of 80-95wt% Mo(Si 1-x Alx ) 2 and 5-20wt% montmorillonite powder; add 6-13 wt% % distilled water; mix well; form a slurry.
2、二硅化钼复合材料的制备2. Preparation of molybdenum disilicide composite material
a、将所得泥料转入双螺旋挤出机中，挤出直径3～18毫米的棒材。a. Transfer the obtained sludge into a twin-screw extruder to extrude rods with a diameter of 3-18 mm.
b、将挤出后的棒材在20～80度恒温下干燥，使棒材中的水分降低到0.3％以下。b. Dry the extruded rod at a constant temperature of 20-80 degrees to reduce the moisture in the rod to below 0.3%.
c、将干燥后的棒材在1200～1500度下烧结，保温时间为1～3小时，烧结气氛为保护性气氛，得到高强度的二硅化钼复合材料。c. Sintering the dried bar at 1200-1500 degrees, holding time for 1-3 hours, the sintering atmosphere is a protective atmosphere, to obtain a high-strength molybdenum disilicide composite material.
与已有技术相比，本发明具有如下优点：Compared with the prior art, the present invention has the following advantages:
a、本发明材料中的Mo(Si1-xAlx)2能有效增强材料的强度和韧性。a. Mo(Si 1-x Al x ) 2 in the material of the present invention can effectively enhance the strength and toughness of the material.
b、本发明材料中蒙脱石起到活化烧结的作用，降低了MoSi2的烧结温度。b. The montmorillonite in the material of the present invention plays the role of activation and sintering, which reduces the sintering temperature of MoSi2 .
具体实施方式 Detailed ways
例1：example 1:
1、原料准备1. Raw material preparation
a、将纯度为98％的铝粉、纯度为98％的钼粉、纯度为98％的硅粉，按照1.675mol％铝、33mol％钼、65.325mol％硅的摩尔比例混合均匀，采用自蔓延反应合成的工艺得到Mo(Si0.975Al0.025)2。a. Mix aluminum powder with a purity of 98%, molybdenum powder with a purity of 98%, and silicon powder with a purity of 98% according to the molar ratio of 1.675mol% aluminum, 33mol% molybdenum, and 65.325mol% silicon. Mo(Si 0.975 Al 0.025 ) 2 was obtained through the process of reactive synthesis.
b、按照95wt％Mo(Si0.975Al0.025)2和5wt％蒙脱石粉末的重量比例配料；再加入6wt％蒸馏水；混合均匀；形成泥料。b. Dosing according to the weight ratio of 95wt% Mo(Si 0.975 Al 0.025 ) 2 and 5wt% montmorillonite powder; then add 6wt% distilled water; mix evenly; form mud.
2、二硅化钼复合材料的制备2. Preparation of molybdenum disilicide composite material
a、将所得泥料转入双螺旋挤出机中，挤出直径3和6毫米的棒材。a. Transfer the resulting mud into a twin-screw extruder to extrude rods with a diameter of 3 and 6 mm.
b、将挤出后的棒材在50度恒温下干燥，使棒材中的水分降低到0.3％。b. Dry the extruded rod at a constant temperature of 50 degrees to reduce the moisture in the rod to 0.3%.
c、将干燥后的棒材在1500度下烧结，保温时间为1小时，烧结气氛为氨分解气氛，得到高强度的二硅化钼复合材料。c. Sinter the dried bar at 1500°C for 1 hour, and the sintering atmosphere is an ammonia decomposition atmosphere to obtain a high-strength molybdenum disilicide composite material.
所得二硅化钼复合材料的弯曲强度为420MPa、断裂韧性为3.98MPa·m1/2、压缩强度为1740MPa。The obtained molybdenum disilicide composite material had a flexural strength of 420 MPa, a fracture toughness of 3.98 MPa·m 1/2 , and a compressive strength of 1740 MPa.
例2：Example 2:
1、原料准备1. Raw material preparation
a、将纯度为98％的铝粉、纯度为98％的钼粉、纯度为98％的硅粉，按照20.1mol％铝、33mol％钼、46.9mol％硅的摩尔比例混合均匀，采用自蔓延反应合成的工艺得到Mo(Si0.7Al0.3)2。a. Mix aluminum powder with a purity of 98%, molybdenum powder with a purity of 98%, and silicon powder with a purity of 98%, according to the molar ratio of 20.1mol% aluminum, 33mol% molybdenum, and 46.9mol% silicon. The process of reactive synthesis yields Mo(Si 0.7 Al 0.3 ) 2 .
b、按照80wt％Mo(Si0.7Al0.3)2和20wt％蒙脱石粉末的重量比例配料；再加入12wt％蒸馏水；混合均匀；形成泥料。b. Dosing according to the weight ratio of 80wt% Mo(Si 0.7 Al 0.3 ) 2 and 20wt% montmorillonite powder; then add 12wt% distilled water; mix evenly; form mud.
2、二硅化钼复合材料的制备2. Preparation of molybdenum disilicide composite material
a、将所得泥料转入双螺旋挤出机中，挤出直径6和12毫米的棒材。a. Transfer the obtained mud into a twin-screw extruder to extrude rods with a diameter of 6 and 12 mm.
b、将挤出后的棒材在80度恒温下干燥，使棒材中的水分降低到0.3％。b. Dry the extruded rod at a constant temperature of 80 degrees to reduce the moisture in the rod to 0.3%.
c、将干燥后的棒材在1200度下烧结，保温时间为3小时，烧结气氛为氢气，得到高强度的二硅化钼复合材料。c. Sinter the dried bar at 1200°C for 3 hours, and the sintering atmosphere is hydrogen to obtain a high-strength molybdenum disilicide composite material.
所得二硅化钼复合材料的弯曲强度为430MPa、断裂韧性为3.95MPa·m1/2、压缩强度为1650MPa。The obtained molybdenum disilicide composite material had a flexural strength of 430 MPa, a fracture toughness of 3.95 MPa·m 1/2 , and a compressive strength of 1650 MPa.
例3：Example 3:
1、原料准备1. Raw material preparation
a、将纯度为99％的铝粉、纯度为99％的钼粉、纯度为98％的硅粉，按照6.7mol％铝、33mol％钼、60.3mol％硅的摩尔比例混合均匀，采用自蔓延反应合成的工艺得到Mo(Si0.9Al0.1)2。a. Mix aluminum powder with a purity of 99%, molybdenum powder with a purity of 99%, and silicon powder with a purity of 98%, according to the molar ratio of 6.7mol% aluminum, 33mol% molybdenum, and 60.3mol% silicon. The process of reactive synthesis yields Mo(Si 0.9 Al 0.1 ) 2 .
b、按照91wt％Mo(Si0.9Al0.1)2和9wt％蒙脱石粉末的重量比例配料；再加入10wt％蒸馏水；混合均匀；形成泥料。b. Dosing according to the weight ratio of 91wt% Mo(Si 0.9 Al 0.1 ) 2 and 9wt% montmorillonite powder; then add 10wt% distilled water; mix evenly; form mud.
2、二硅化钼复合材料的制备2. Preparation of molybdenum disilicide composite material
a、将所得泥料转入双螺旋挤出机中，挤出直径9和18毫米的棒材。a. Transfer the obtained mud into a twin-screw extruder to extrude rods with diameters of 9 and 18 mm.
b、将挤出后的棒材在70度恒温下干燥，使棒材中的水分降低到0.3％。b. Dry the extruded rod at a constant temperature of 70 degrees to reduce the moisture in the rod to 0.3%.
c、将干燥后的棒材在1460度下烧结，保温时间为3小时，烧结气氛为氨分解气氛，得到高强度的二硅化钼复合材料。c. Sinter the dried bar at 1460°C for 3 hours, and the sintering atmosphere is an ammonia decomposition atmosphere to obtain a high-strength molybdenum disilicide composite material.
所得二硅化钼复合材料的弯曲强度为500MPa、断裂韧性为4.10MPa·m1/2、压缩强度为2010MPa。The obtained molybdenum disilicide composite material had a flexural strength of 500 MPa, a fracture toughness of 4.10 MPa·m 1/2 , and a compressive strength of 2010 MPa.
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| CN103231058A (en) * | 2013-05-13 | 2013-08-07 | 中原工学院 | Preparation method of high temperature silicon molybdenum rods |
| RU2818057C1 (en) * | 2023-07-11 | 2024-04-23 | Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт химии силикатов им. И.В. Гребенщикова Российской академии наук (ИХС РАН) | Charge for producing composite material based on molybdenum disilicide |
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| ES2912404T3 (en) * | 2018-03-18 | 2022-05-25 | Kanthal Ab | Heating element containing parts of molybdenum disilicide |
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| MoSi2发热元件的微观组织结构. 冯培忠，曲选辉，杜学丽.中国有色金属学报，第15卷第2期. 2005 |
| MoSi2发热元件的微观组织结构. 冯培忠，曲选辉，杜学丽.中国有色金属学报，第15卷第2期. 2005 * |
| 二硅化钼发热元件的研究与应用进展. 冯培忠，曲选辉.中国钼业，第29卷第2期. 2005 |
| 二硅化钼发热元件的研究与应用进展. 冯培忠，曲选辉.中国钼业，第29卷第2期. 2005 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103231058A (en) * | 2013-05-13 | 2013-08-07 | 中原工学院 | Preparation method of high temperature silicon molybdenum rods |
| RU2818057C1 (en) * | 2023-07-11 | 2024-04-23 | Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт химии силикатов им. И.В. Гребенщикова Российской академии наук (ИХС РАН) | Charge for producing composite material based on molybdenum disilicide |
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| CN100999023A (en) | 2007-07-18 |
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