CN107010928A - 一种MoSi2/Al2O3耐高温吸波材料、制备方法及其应用 - Google Patents
一种MoSi2/Al2O3耐高温吸波材料、制备方法及其应用 Download PDFInfo
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- 229910020968 MoSi2 Inorganic materials 0.000 title claims abstract description 52
- 239000011358 absorbing material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 58
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 57
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 25
- 229920001353 Dextrin Polymers 0.000 claims abstract description 15
- 239000004375 Dextrin Substances 0.000 claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 15
- 235000019425 dextrin Nutrition 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 15
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 14
- 229910016006 MoSi Inorganic materials 0.000 claims description 12
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- 238000009413 insulation Methods 0.000 claims description 11
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- 238000003756 stirring Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 abstract description 14
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- 239000011230 binding agent Substances 0.000 abstract description 9
- 229910052796 boron Inorganic materials 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 239000003963 antioxidant agent Substances 0.000 abstract description 5
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- 230000003078 antioxidant effect Effects 0.000 abstract description 2
- 235000006708 antioxidants Nutrition 0.000 abstract description 2
- 230000003026 anti-oxygenic effect Effects 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 10
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- 238000005485 electric heating Methods 0.000 description 8
- 239000003822 epoxy resin Substances 0.000 description 8
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- 150000001875 compounds Chemical class 0.000 description 5
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- 239000004632 polycaprolactone Substances 0.000 description 4
- 238000003303 reheating Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明涉及一种新型抗氧化耐高温吸波材料及其制备工艺。具体涉及一种MoSi2/Al2O3耐高温吸波材料、制备方法及其应用。按下列步骤操作:将MoSi2,Al2O3,Al粉和SiO2作为原料,糊精作为粘结剂,B2O3作为烧结助剂,经配料及混匀,加入少量去离子水后困料;用液压式压力试验机在250MPa压力下制成尺寸为的圆片状试样,干燥48h,在高温重烧试验炉中加热至1300~1450℃。该硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料的显气孔率20.81%~35.43%,体积密度2.89~4.11g·cm‑3。实验表明本发明提供硼掺杂MoSi2/Al2O3的吸波材料,其抗氧化性能好、耐高温,在吸波材料领域有好的应用前景。
Description
技术领域
本发明涉及一种化工材料的制备方法,特别涉及一种MoSi2/Al2O3耐高温吸波材料、制备方法及其应用。
背景技术
现代战争中,先敌发现,先敌攻击是克敌制胜的重要保障。由此可见,武器装备隐身化可以显著提高军事效益,是当前世界军事高技术发展的重要方向之一。
理想的吸波材料应该具有吸收强、频段宽、质量轻等特点。传统的磁性吸波材料的比重较大,且在高温可能会失去磁性,其在一些领域中的应用受到限制,因而利用合适的金属或金属合金微粉制备宽频吸收、轻质高强的高温抗氧化吸波材料,是可行而必要的。金属间化合物MoSi2因具有金属和陶瓷的双重特性、具有熔点高、适中的比重、较低的热膨胀系数、良好的高温抗氧化性(抗氧化温度可达1600℃以上)、优良的导电性及热导率等特点,而被广泛研究,成为目前最有前途的高温结构材料之一。
然而,MoSi2因晶体结构中非金属键比例高,结构对称性低,突出的缺点是韧脆转变温度太高,室温时很脆,断裂韧性仅为2.5MPa·m1/2左右,高温(>1250℃)强度,特别是蠕变强度明显不足,目前国内尚未见到能高效耐高温抗氧化的优质吸波材料,本发明提供了这种优良吸波材料。
发明内容
针对现有技术中存在的不足,本发明的目的在于提供一种MoSi2/Al2O3耐高温吸波材料、制备方法及其应用。
为实现上述目标,本发明采取如下的技术方案:
一种MoSi2/Al2O3耐高温吸波材料,按质量百分比计,所述的吸波材料包括以下原料:6wt.%~33wt.%的MoSi2,10wt.%~35wt.%的SiO2,9wt.%~26wt.%的Al粉,15wt.%~30wt.%的Al2O3,8wt.%~10wt.%的糊精以及10wt.%~12wt.%的B2O3。
优选的,所述MoSi2/Al2O3耐高温吸波材料,按质量百分比计,所述的吸波材料包括以下原料:24wt.%含量的MoSi2,15wt.%的SiO2,17wt.%的Al粉,25wt.%的Al2O3,9wt.%的糊精以及10wt.%的B2O3。
一种MoSi2/Al2O3耐高温吸波材料的制备方法,包含以下步骤:
步骤一:取6wt.%~33wt.%的MoSi2,10wt.%~35wt.%的SiO2,9wt.%~26wt.%的Al粉,15wt.%~30wt.%的Al2O3,8wt.%~10wt.%的糊精以及10wt.%~12wt.%的B2O3,加入无水乙醇,研磨8~10h,得到混合料浆;
步骤二:将混合料浆在80~100℃下干燥36~48h,至混合粉状;
步骤三:研磨混合粉状料浆,研磨4~6h;加入适量去离子水搅拌后困料4~6h;
步骤四:在250~300MPa压力下制成试样,将试样在80~100℃下干燥36~48h,制得干燥试样;
步骤五:将干燥试样加热至650~850℃保温120min,继续加热至1300~1450℃保温120min,停止加热,自然冷却至20~30℃,得到MoSi2/Al2O3耐高温吸波材料。
优选的,所述步骤四中制成试样尺寸为的圆柱状。
所述的MoSi2/Al2O3耐高温吸波材料用于吸波涂层的应用。
相较于现有技术,本发明的技术效果为:
Al2O3陶瓷的主晶相是α-Al2O3,为刚玉型结构,具有熔点高、密度低的特点,并且与MoSi2在化学上和物理上具有相容性,能改变Al2O3-MoSi2的界面能和MoSi2的晶界能,是MoSi2最适合的增强相,通过MoSi2与Al2O3的复合可以有效增强其室温韧性和高温强度。
本发明制备吸波材料密度较小,为2.89~4.11g/m3,电导率为3.92~5.53S·m-1,在8.2~12.4GHz频率下,最大吸波损耗为23~29dB;本发明制备吸波材料耐高温抗氧化性能好。
附图说明
图1是本发明一种新型硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料的制备方法的流程图。
图2是本发明方法实施例3的硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料XRD衍射图。
图3是本发明方法实施例3制备的硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料SEM照片。
图4是本发明方法实施例1制备的硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料反射率图。
下面结合附图对本发明做出进一步解释说明。
具体实施方式
实施例1
选取MoSi2,Al2O3,Al粉和SiO2作为原料,糊精作为粘结剂,B2O3作为烧结助剂,按质量百分比计,选取6wt.%含量的MoSi2,35wt.%的SiO2,26wt.%的Al粉,15wt.%的Al2O3,8wt.%的糊精以及10wt.%的B2O3,加入无水乙醇用全方位细粉球磨机机械研磨8.5h,球磨速度为350rpm,得到混合料浆;
将混合料浆放置恒温电热干燥箱80℃干燥48h,至混合粉状;
将干燥料浆得到的混合粉用玛瑙研钵研磨4h,随后加入适量去离子水搅拌均匀后困料4h;
用液压式压力试验机在压力机上以250MPa压力制成尺寸为 的圆柱状试样,将圆柱状试样置于恒温电热干燥箱80℃干燥48h;
待试样充分干燥后,放入高温重烧试验机中加热至850℃保温120min,随后加热至1300℃保温120min后,停止加热,自然冷却至22℃,制备得到MoSi2/Al2O3耐高温吸波材料。测量MoSi2/Al2O3耐高温吸波材料的密度为:2.89g·cm-3,显气孔率为:34.30%。
将环氧树脂置于热水中,待软化后取出,将环氧树脂与低分子聚酞胺以体积比1:1混合制备得粘粘剂。然后将MoSi2/Al2O3耐高温吸波材料碾磨成粉,通过粘粘剂与MoSi2/Al2O3粉末按质量比1:1混合,加入与粘结剂质量相同的丙酮,超声分散分钟然后取出置于热水中,充分搅拌分钟使丙酮完全挥发制备得吸波涂料。然后将涂料比较均匀的涂在钢板上,控制钢板平放,使涂料向四周的流动,表面自然均匀。放置24小时后对其打磨至厚度为2mm,即可制备得吸波涂层。使用设备为Agilent Technologies E8362矢量网络分析仪测试复合材料的吸波性能,测量MoSi2/Al2O3吸波材料电导率为3.92S·m-1,在8.2~12.4GHz频率下的吸波损耗为15~20dB。
实施例2
选取MoSi2,Al2O3,Al粉和SiO2作为原料,糊精作为粘结剂,B2O3作为烧结助剂,按质量百分比计,选取16wt.%含量的MoSi2,25wt.%的SiO2,21wt.%的Al粉,20wt.%的Al2O3,9wt.%的糊精以及9wt.%的B2O3,加入无水乙醇用全方位细粉球磨机机械研磨10h,球磨速度为350rpm,得到混合料浆;
将混合料浆放置恒温电热干燥箱80℃干燥48h,至混合粉状;
将干燥料浆得到的混合粉用玛瑙研钵研磨4h,随后加入适量去离子水搅拌均匀后困料4h;
用液压式压力试验机在压力机上以250MPa压力制成尺寸为 的圆柱状试样,将圆柱状试样置于恒温电热干燥箱80℃干燥48h;
待试样充分干燥后,放入高温重烧试验机中加热至750℃保温120min,随后加热至1350℃保温120min后,停止加热,自然冷却至22℃,制备得到一种新型硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料。测量MoSi2/Al2O3耐高温吸波材料的密度为:2.80g·cm-3,显气孔率为:35.43%。
将环氧树脂置于热水中,待软化后取出,将环氧树脂与低分子聚酞胺以体积比1:1混合制备得粘粘剂。然后将MoSi2/Al2O3耐高温吸波材料碾磨成粉,通过粘粘剂与MoSi2/Al2O3粉末按质量比1:1混合,加入与粘结剂质量相同的丙酮,超声分散分钟然后取出置于热水中,充分搅拌分钟使丙酮完全挥发制备得吸波涂料。然后将涂料比较均匀的涂在钢板上,控制钢板平放,使涂料向四周的流动,表面自然均匀。放置24小时后对其打磨至厚度为2mm,即可制备得吸波涂层。使用设备为Agilent Technologies E8362矢量网络分析仪测试复合材料的吸波性能,测量MoSi2/Al2O3吸波材料电导率为4.82S·m-1,在8.2~12.4GHz的吸波损耗为17~22dB。
实施例3
选取MoSi2,Al2O3,Al粉和SiO2作为原料,糊精作为粘结剂,B2O3作为烧结助剂,按质量百分比计,选取24wt.%含量的MoSi2,15wt.%的SiO2,17wt.%的Al粉,25wt.%的Al2O3,9wt.%的糊精以及10wt.%的B2O3,加入无水乙醇用全方位细粉球磨机机械研磨8h,球磨速度为350rpm,得到混合料浆;
将混合料浆放置恒温电热干燥箱80℃干燥48h,至混合粉状;
将干燥料浆得到的混合粉用玛瑙研钵研磨4h,随后加入适量去离子水搅拌均匀后困料4h;
用液压式压力试验机在压力机上以250MPa压力制成尺寸为 的圆柱状试样,将圆柱状试样置于恒温电热干燥箱80℃干燥48h;
待试样充分干燥后,放入高温重烧试验机中加热至800℃保温120min,随后加热至1400℃保温120min后,停止加热,自然冷却至22℃,制备得到一种新型硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料。测量MoSi2/Al2O3耐高温吸波材料的密度为:4.11g·cm-3,显气孔率为:20.81%。
将环氧树脂置于热水中,待软化后取出,将环氧树脂与低分子聚酞胺以体积比1:1混合制备得粘粘剂。然后将MoSi2/Al2O3耐高温吸波材料碾磨成粉,通过粘粘剂与MoSi2/Al2O3粉末按质量比1:1混合,加入与粘结剂质量相同的丙酮,超声分散分钟然后取出置于热水中,充分搅拌分钟使丙酮完全挥发制备得吸波涂料。然后将涂料比较均匀的涂在钢板上,控制钢板平放,使涂料向四周的流动,表面自然均匀。放置24小时后对其打磨至厚度为2mm,即可制备得吸波涂层。使用设备为Agilent Technologies E8362矢量网络分析仪测试复合材料的吸波性能,测量MoSi2/Al2O3吸波材料电导率为4.72S·m-1,在8.2~12.4GHz的吸波损耗为23~29dB。
实施例4
选取MoSi2,Al2O3,Al粉和SiO2作为原料,糊精作为粘结剂,B2O3作为烧结助剂,按质量百分比计,选取33wt.%含量的MoSi2,10wt.%的SiO2,9wt.%的Al粉,30wt.%的Al2O3,10wt.%的糊精以及8wt.%的B2O3,加入无水乙醇用全方位细粉球磨机机械研磨10h,球磨速度为350rpm,得到混合料浆;
将混合料浆放置恒温电热干燥箱80℃干燥48h,至混合粉状;
将干燥料浆得到的混合粉用玛瑙研钵研磨4h,随后加入适量去离子水搅拌均匀后困料4h;
用液压式压力试验机在压力机上以250MPa压力制成尺寸为 的圆柱状试样,将圆柱状试样置于恒温电热干燥箱80℃干燥48h;
待试样充分干燥后,放入高温重烧试验机中加热至700℃保温120min,随后加热至1450℃保温120min后,停止加热,自然冷却至22℃,制备得到一种新型硼掺杂MoSi2/Al2O3抗氧化耐高温吸波材料。测量MoSi2/Al2O3耐高温吸波材料的密度为:3.75g·cm-3,显气孔率为:23.89%。
将环氧树脂置于热水中,待软化后取出,将环氧树脂与低分子聚酞胺以体积比1:1混合制备得粘粘剂。然后将MoSi2/Al2O3耐高温吸波材料碾磨成粉,通过粘粘剂与MoSi2/Al2O3粉末按质量比1:1混合,加入与粘结剂质量相同的丙酮,超声分散分钟然后取出置于热水中,充分搅拌分钟使丙酮完全挥发制备得吸波涂料。然后将涂料比较均匀的涂在钢板上,控制钢板平放,使涂料向四周的流动,表面自然均匀。放置24小时后对其打磨至厚度为2mm,即可制备得吸波涂层。使用设备为Agilent Technologies E8362矢量网络分析仪测试复合材料的吸波性能,测量MoSi2/Al2O3吸波材料电导率为5.53S·m-1,在8.2~12.4GHz的吸波损耗为20~25dB。
Claims (5)
1.一种MoSi2/Al2O3耐高温吸波材料,其特征在于:按质量百分比计,所述的吸波材料包括以下原料:6wt.%~33wt.%的MoSi2,10wt.%~35wt.%的SiO2,9wt.%~26wt.%的Al粉,15wt.%~30wt.%的Al2O3,8wt.%~10wt.%的糊精以及10wt.%~12wt.%的B2O3。
2.如权利要求1所述的MoSi2/Al2O3耐高温吸波材料,其特征在于:按质量百分比计,所述的吸波材料包括以下原料:24wt.%的MoSi2,15wt.%的SiO2,17wt.%的Al粉,25wt.%的Al2O3,9wt.%的糊精以及10wt.%的B2O3。
3.一种MoSi2/Al2O3耐高温吸波材料的制备方法,其特征在于:包含以下步骤:
步骤一:取6wt.%~33wt.%的MoSi2,10wt.%~35wt.%的SiO2,9wt.%~26wt.%的Al粉,15wt.%~30wt.%的Al2O3,8wt.%~10wt.%的糊精以及10wt.%~12wt.%的B2O3,加入无水乙醇,研磨8~10h,得到混合料浆;
步骤二:将混合料浆在80~100℃下干燥36~48h,至混合粉状;
步骤三:研磨混合粉状料浆,研磨4~6h;加入适量去离子水搅拌后困料4~6h;
步骤四:在250~300MPa压力下制成试样,将试样在80~100℃下干燥36~48h,制得干燥试样;
步骤五:将干燥试样加热至650~850℃保温120min,继续加热至1300~1450℃保温120min,停止加热,自然冷却至20~30℃,得到MoSi2/Al2O3耐高温吸波材料。
4.如权利要求3所述的MoSi2/Al2O3耐高温吸波材料,其特征在于:所述步骤四中制成试样尺寸为的圆柱状。
5.权利要求1或2所述的MoSi2/Al2O3耐高温吸波材料用于吸波涂层的应用。
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ZHIBIN HUANG ET AL.: "Dielectric and Mechanical Properties of MoSi2/Al2O3 Composites Prepared by Hot Pressing", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
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