CN108129138B - TiO2衰减瓷及其制备方法 - Google Patents
TiO2衰减瓷及其制备方法 Download PDFInfo
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- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 85
- 238000005245 sintering Methods 0.000 claims abstract description 51
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000001465 metallisation Methods 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 15
- 238000007731 hot pressing Methods 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 14
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 14
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 14
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 14
- 238000003466 welding Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 36
- 229910052739 hydrogen Inorganic materials 0.000 claims description 36
- 239000001257 hydrogen Substances 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 25
- 238000012360 testing method Methods 0.000 claims description 23
- 229910052593 corundum Inorganic materials 0.000 claims description 17
- 238000009713 electroplating Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 13
- 229910052759 nickel Inorganic materials 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 238000007639 printing Methods 0.000 claims description 6
- 238000009472 formulation Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 238000005219 brazing Methods 0.000 claims description 4
- 230000001680 brushing effect Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 4
- 238000003754 machining Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000000523 sample Substances 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 claims description 4
- 229910000679 solder Inorganic materials 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims 1
- 238000007780 powder milling Methods 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract description 11
- 238000012216 screening Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract 1
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 19
- 239000002245 particle Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 10
- 238000001514 detection method Methods 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical group O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- 229910017309 Mo—Mn Inorganic materials 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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Abstract
本发明公开了一种TiO2衰减瓷及其制备方法,它由Al2O3、TiO2、SiO2和MnO、MgO制成。本发明所述的TiO2衰减瓷,各组分配比科学合理,具有致密性高,孔隙率低,强度高,热导率较高,衰减量大、经900℃后衰减值稳定等性能。本发明所述的TiO2衰减瓷的制备方法,通过大量实验筛选出最佳的配方、热压烧结成型工艺、金属化工艺及焊接工艺和镀层烧结等工艺,制备得到的TiO2衰减瓷性能稳定,适用范围广泛,可用于速调管、毫米波行波管以及磁控管等微波电子真空器件。
Description
技术领域
本发明涉及一种TiO2衰减瓷及其制备方法。
背景技术
TiO2衰减瓷主要应用的管型有速调管、磁控管、毫米波行波管等。在速调管中,一般将 TiO2衰减瓷焊接在谐振腔内,通过吸收微波,降低谐振腔的品质因素Q,从而实现工作频带的展宽。从TiO2衰减瓷的工艺制备流程来看,一般采用干压或等静压成型,在氢气氛围中进行烧结,但对TiO2衰减瓷的金属化及与无氧铜腔体焊接的方法报道较少。TiO2衰减瓷除了本身的性能以及满足管子在使用频率范围内的匹配特性以外,还必须实现与无氧铜的牢固焊接,并且能够在各种环境试验考核下,衰减瓷不出现脱落、衰减性能变化等现象。
发明内容
发明目的:本发明的目的是为了提升现有制备技术,提供一种组分配比科学合理,具有高密度、气孔率低的特性,采用的金属化及封接技术能实现与无氧铜的牢固焊接,不会出现脱落、衰减性能变化的的微波衰减材料,实现封接后耐热冲击性能强,且具有优异的耐高、低温性能,衰减瓷不发生脱落,衰减性能不发生改变的TiO2衰减瓷。本发明另一个目的是提供TiO2衰减瓷的制备方法。
技术方案:为了实现以上目的,本发明采取的技术方案为:
一种TiO2衰减瓷,它由下列原料制成:
Al2O3、TiO2、SiO2、MnO、MgO。
作为优选方案,以上所述的TiO2衰减瓷,它由下列重量份数的原料制成:
Al2O365~85份、TiO212~20份、SiO21~3份、MnO 2~5份,MgO 1~3份。
作为优选方案,以上所述的TiO2衰减瓷,所述的Al2O3粒径为5~10μm,TiO2的粒径为 10~15μm,SiO2的粒径为1~2μm、MnO的粒径为2~5μm、MgO的粒径为2~4μm。
本发明所述的TiO2衰减瓷的制备方法,其包括以下步骤:
a、将Al2O3粉末、TiO2粉末、SiO2粉末、MnO粉末、MgO粉末按一定比例混合,在行星球磨机上球磨;
b、装模、热压烧结成型:
将步骤a球磨混合后的粉末装入石墨模具中,并进行预压制,再将石墨模具置于热压烧结炉内,烧结温度为1350~1450℃,保温30~45min,施加的压力为25~30MPa;
c、机械加工
将烧结的衰减瓷,加工成长宽高17×8×1毫米或长宽高34×10×1毫米等需求的尺寸;
d、清洗
将衰减瓷置于丙酮溶液中超声15~30min,用刷子沾去污粉后刷若干遍,再将衰减瓷置于去离子水中煮沸,保持10~15min,最后用酒精脱水后烘干备用;
e、烧氢净化
在卧式烧氢炉中600~650℃,保温10~15min烧氢处理,然后冷却至室温;
f、TiO2衰减瓷的膏剂配制及金属化层的印刷
将Mo粉末,MnO粉末,刚玉微粉、CaCO3按比例混合,并加入粘结剂,在行星球磨机上球磨,制得金属化膏剂;
采用丝网印刷机在TiO2衰减瓷的一面分1~3次印刷厚度为35~40μm的金属化层;
g、金属化层的烧结
在卧式氢炉中1100~1200℃,保温15~20min烧结处理,氢气露点为-60°;
h、电镀镍
将烧结后的TiO2衰减瓷进行电镀镍处理,镍层厚度控制在5~7μm;
i、镀层烧结
电镀结束后,在卧式氢炉中800~900℃,保温15~20min进行镀层烧结处理,氢气露点为 -60°;
j、Q值的测试
将TiO2衰减瓷置于腔体中,用上模具固定住TiO2衰减瓷使其不能发生移动,用连接矢量网络分析仪的探针伸入腔体,在谐振点查看Q值;
k、衰减瓷与腔体的钎焊
采用Q值合格的TiO2衰减瓷,用AgCu28焊料将其焊接至腔体,再次测试Q值,取Q值合格的TiO2衰减瓷,既得。
作为优选方案,以上所述的TiO2衰减瓷的制备方法,步骤a将Al2O365~85份、TiO212~ 20份、SiO21~3份、MnO2~5份,MgO 1~3份混合,在行星球磨机上以180r/min的转速球磨8h。
作为优选方案,以上所述的TiO2衰减瓷的制备方法,将步骤b混合后的粉末装入石墨模具中,并进行预压制,再将石墨模具置于热压烧结炉内,烧结温度为1350~1380℃,保温 45min,施加的压力为30MPa。
作为优选方案,以上所述的TiO2衰减瓷的制备方法,步骤e烧氢净化,在卧式烧氢炉中 650℃,保温15min烧氢处理,然后冷却至室温。
作为优选方案,以上所述的TiO2衰减瓷的制备方法,步骤f中将Mo粉50~65份,MnO16~20份、刚玉微粉10~15份和CaCO31~5份混合,并加入粘结剂醋酸丁酯和硝棉溶液,在行星球磨机上以180r/min的转速球磨12h,制得金属化膏剂;更加优选Mo粉65份,MnO20 份、刚玉微粉12份、CaCO33份。
在TiO2衰减瓷的一面涂覆厚度为30~50μm的金属化膏剂(更加优选40μm),然后在氢炉中烧结1200℃,保温15min,氢气露点为-60°,使TiO2衰减瓷一面金属化。
步骤i中镀层烧结:电镀结束后,在卧式氢炉中850~900℃,保温15~20min进行镀层烧结处理,氢气露点为-60°。
作为优选方案,以上所述的TiO2衰减瓷的制备方法,步骤k制备得到的TiO2衰减瓷的体积密度:≥3.8g/cm3;气孔率:≤0.01%;热导率:≥2.8W/m.K;金属化封接强度≥55Mpa。(封接强度的测试如图3所示)。
一、本发明TiO2衰减瓷的原料筛选实验:
(1)本发明通过筛选不同的原料组成,来优选出性能最佳的TiO2衰减瓷,筛选实验如下表所示:
通过选择不同的原料组合,最终优选的最佳原料组成为:Al2O3、TiO2、SiO2、MnO和MgO。
(2)衰减瓷配方设计。在配方设计的过程中,要全面考虑多个指标如衰减量、致密性之间的关联。配方的最终确定通过指标对比实现。本发明通过大量实验筛选不同原料组成,具体筛选实验如表1所示。这是本发明创新点。
谐振腔的Q值测定结果:
表1不同TiO2含量的衰减瓷对应的Q值
序号 | 氧化铝/g | 二氧化钛/g | 二氧化硅/g | 一氧化锰/g | 一氧化镁/g | Q值 |
1 | 73 | 21 | 3 | 2 | 1 | 600 |
2 | 75 | 19 | 3 | 2 | 1 | 350 |
3 | 80 | 8 | 3 | 2 | 1 | 220 |
由表1可以看出,TiO2含量为19%左右时,最优的Q值为350,具有较优的性能。
(3)热压烧结工艺曲线的确定,本发明通过大量实验筛选烧结保温温度、保温时间、升温速率、热压压力及保压时间等参数,具体试验结果如表2:
表2热压烧结工艺筛选实验结果
根据以上筛选试验结果,本发明优选的最佳热压烧结工艺为:烧结温度为1380℃,保温 45min,施加的压力为30MPa。
(4)步骤f中TiO2衰减瓷的膏剂配方的设计与相关工艺参数如涂覆厚度、露点、烧结温度及烧结时间的筛选实验。该步骤中必须避免由于烧结温度过高而造成衰减瓷变形,并且还要兼顾封接强度、电镀等因素。
具体筛选实验如表3所示:
由以上表3筛选实验结果表明,TiO2衰减瓷的膏剂配方为Mo粉65份,MnO20份、刚玉微粉12份、CaCO33份时,涂覆厚度为40μm的金属化膏剂,然后在氢炉中烧结1200℃,保温15min,氢气露点为-60°,使TiO2衰减瓷一面金属化,具有最优的封接强度。
有益效果:本发明提供的TiO2衰减瓷及其制备方法与现有技术相比具有以下优点:
1、本发明所述的TiO2衰减瓷,经过大量实验筛选各组份及重量份数,实验研究表明,各组分配比科学合理,所制备得到的微波衰减材料致密性高,孔隙率低,强度高,热导率高,经高温处理,介电性能稳定可靠,且能与无氧铜实现牢固焊接,应用范围广泛。
2、本发明所述的TiO2衰减瓷的制备方法,可操作性强,工艺设计合理,尤其是通过大量实验筛选出最佳的专用模具预压成型工艺,热压烧结成型工艺和金属化工艺和Mo-Mn法+ 电镀Ni,镀层烧结等工艺,制备得到的TiO2衰减瓷性能优,适用范围广泛。
附图说明
图1为本发明TiO2衰减瓷的制备过程中模具装配的结构示意图。
图2为本发明TiO2衰减瓷的制备工艺流程图。
图3为本发明TiO2衰减瓷封接强度测试件的结构示意图。
具体实施方式
下面结合具体实施例,进一步阐明本发明,应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定的范围。
实施例1
1、一种TiO2衰减瓷,它由下列重量份数的原料制成:
Al2O375份、TiO219份、SiO23份、MnO 2份,MgO 1份。
所述的Al2O3粒径为5~10μm,TiO2的粒径为10~15μm,SiO2的粒径为1~2μm、MnO的粒径为2~5μm、MgO的粒径为2~4μm。
2、本发明所述的TiO2衰减瓷的制备方法,其包括以下步骤:流程如图2所示;
a、将Al2O375份、TiO219份、SiO23份、MnO 2份,MgO 1份混合,在行星球磨机上以180r/min的转速球磨8h;
b、装模、热压烧结成型:
将步骤a球磨混合后的粉末1装入石墨模具中,如图1所示,并进行预压制,再将石墨模具置于热压烧结炉内,烧结温度为1380℃,保温45min,施加的压力为30MPa;
c、机械加工
将烧结的衰减瓷,加工成长宽高17×8×1毫米;
d、清洗
将衰减瓷置于丙酮溶液中超声30min,用刷子沾去污粉后刷3遍,再将衰减瓷置于去离子水中煮沸,保持15min,最后用酒精脱水后烘干备用;
e、烧氢净化
在卧式烧氢炉中650℃,保温15min烧氢处理,然后冷却至室温;
f、TiO2衰减瓷的膏剂配制及金属化层的印刷
将Mo粉65份,MnO 20份、刚玉微粉12份、CaCO33份,混合,并加入粘结剂醋酸丁酯和硝棉溶液,在行星球磨机上以180r/min的转速球磨12h,制得金属化膏剂;
采用丝网印刷机在TiO2衰减瓷的一面分3次印刷厚度为40μm的金属化层;
g、金属化层的烧结
在卧式氢炉中1200℃,保温15min烧结处理,氢气露点为-60°;
h、电镀镍
将烧结后的TiO2衰减瓷进行电镀镍处理,镍层厚度控制在6μm;
i、镀层烧结
电镀结束后,在卧式氢炉中850℃,保温20min进行镀层烧结处理,氢气露点为-60°;
j、Q值的测试
将TiO2衰减瓷置于腔体中,用上模具固定住TiO2衰减瓷使其不能发生移动,用连接矢量网络分析仪的探针伸入腔体,在谐振点查看Q值;
k、衰减瓷与腔体的钎焊
采用Q值合格的TiO2衰减瓷,用AgCu28焊料将其焊接至腔体,再次测试Q值,取Q值合格的TiO2衰减瓷,既得。
3、将上述2制备得到的TiO2衰减瓷进行性能检测,检测结果如下:
1)体积密度:≥3.9g/cm3;
2)气孔率:≤0.01%;
3)热导率:≥2.8W/m.K;
4)金属化后,衰减瓷片不出现显著变形现象,平面度优于±0.15mm;
5)建立封接强度的考核标准,初步设定为抗拉强度≥50Mpa。
4、将上述2制备得到的TiO2衰减瓷进行性能检测,检测结果如下:
1)耐热冲击性能:试验条件为650℃至室温,反复6次,衰减瓷不发生脱落,衰减性能不发生改变;
2)耐热烘烤试验:试验条件为在550℃下烘烤35h,衰减瓷不发生脱落,衰减性能不发生改变;
3)高低温循环试验:试验条件为高温:70℃,低温:-55℃,各保持一小时;转换时间5min;循环3次,衰减瓷不发生脱落,衰减性能不发生改变。
4)耐高温性能:试验条件为810℃,30min,衰减性能不发生改变。
5、应用情况
将上述制备得到TiO2衰减瓷装配在大功率速调管5151上应用,采用矢网测试其Q值。具体要求为,2腔:320~350,本发明制备得到的TiO2衰减瓷可推广至毫米波行波管、空间磁控管等管型应用。
实施例2
1、一种TiO2衰减瓷,它由下列重量份数的原料制成:
Al2O385份、TiO220份、SiO23份、MnO 5份,MgO 3份。
所述的Al2O3粒径为5~10μm,TiO2的粒径为10~15μm,SiO2的粒径为1~2μm、MnO的粒径为2~5μm、MgO的粒径为2~4μm。
2、本发明所述的TiO2衰减瓷的制备方法,其包括以下步骤:流程如图2所示;
a、将Al2O385份、TiO220份、SiO23份、MnO 5份,MgO 3份混合,在行星球磨机上以180r/min的转速球磨8h;
b、装模、热压烧结成型:
将步骤a球磨混合后的粉末装入石墨模具中,如图1所示,并进行预压制,再将石墨模具置于热压烧结炉内,烧结温度为1350℃,保温30min,施加的压力为40MPa;
c、机械加工
将烧结的衰减瓷,加工成长宽高34×10×1毫米;
d、清洗
将衰减瓷置于丙酮溶液中超声20min,用刷子沾去污粉后刷3遍,再将衰减瓷置于去离子水中煮沸,保持15min,最后用酒精脱水后烘干备用;
e、烧氢净化
在卧式烧氢炉中600℃,保温15min烧氢处理,然后冷却至室温;
f、TiO2衰减瓷的膏剂配制及金属化层的印刷
将Mo粉50份,MnO 16份、刚玉微粉10份和CaCO31份,混合,并加入粘结剂醋酸丁酯和硝棉溶液,在行星球磨机上以180r/min的转速球磨12h,制得金属化膏剂;
采用丝网印刷机在TiO2衰减瓷的一面分3次印刷厚度为30μm的金属化层;
g、金属化层的烧结
在卧式氢炉中1100℃,保温20min烧结处理,氢气露点为-60°;
h、电镀镍
将烧结后的TiO2衰减瓷进行电镀镍处理,镍层厚度控制在7μm;
i、镀层烧结
电镀结束后,在卧式氢炉中900℃,保温15min进行镀层烧结处理,氢气露点为-60°;
j、Q值的测试
将TiO2衰减瓷置于腔体中,用上模具固定住TiO2衰减瓷使其不能发生移动,用连接矢量网络分析仪的探针伸入腔体,在谐振点查看Q值;
k、衰减瓷与腔体的钎焊
采用Q值合格的TiO2衰减瓷,用AgCu28焊料将其焊接至腔体,再次测试Q值,取Q值合格的TiO2衰减瓷,既得。
3、将上述2制备得到的TiO2衰减瓷进行性能检测,检测结果如下:
1)体积密度:≥3.8g/cm3;
2)气孔率:≤0.01%;
3)热导率:≥2.8W/m.K;
4)金属化后,衰减瓷片不出现显著变形现象,平面度优于±0.15mm;
5)建立封接强度的考核标准,初步设定为抗拉强度≥48Mpa。
4、将上述2制备得到的TiO2衰减瓷进行性能检测,检测结果如下:
1)耐热冲击性能:试验条件为650℃至室温,反复6次,衰减瓷不发生脱落,衰减性能不发生改变;
2)耐热烘烤试验:试验条件为在550℃下烘烤35h,衰减瓷不发生脱落,衰减性能不发生改变;
3)高低温循环试验:试验条件为高温:70℃,低温:-55℃,各保持一小时;转换时间5min;循环3次,衰减瓷不发生脱落,衰减性能不发生改变。
4)耐高温性能:试验条件为810℃,30min,衰减性能不发生改变。
5、应用情况
将上述制备得到TiO2衰减瓷装配在大功率速调管5151上应用,采用矢网测试其Q值。具体要求为,2腔:320~350,本发明制备得到的TiO2衰减瓷可推广至毫米波行波管、空间磁控管等管型应用。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (3)
1.一种TiO2衰减瓷的制备方法,其特征在于,包括以下步骤:
a、将Al2O3 粉末65~85份、TiO2 粉末12~20份、SiO2 粉末1~3份、MnO 粉末2~5份,MgO粉末 1~3份混合,在行星球磨机上以180r/min的转速球磨8h;
b、装模、热压烧结成型:
将步骤a混合后的粉末装入石墨模具中,并进行预压制,再将石墨模具置于热压烧结炉内,烧结温度为1350~1380℃,保温45min,施加的压力为30MPa;
c、机械加工
将烧结的衰减瓷,加工成需要的尺寸;
d、清洗
将衰减瓷置于丙酮溶液中超声15~30min,用刷子沾去污粉后刷若干遍,再将衰减瓷置于去离子水中煮沸,保持10~15min,最后用酒精脱水后烘干备用;
e、烧氢净化
在卧式烧氢炉中650℃,保温15min烧氢处理,然后冷却至室温;
f、TiO2衰减瓷的膏剂配制及金属化层的印刷
将Mo粉50~65份,MnO 16~20份、刚玉微粉10~15份和CaCO3 1~5份混合,并加入粘结剂醋酸丁酯和硝棉溶液,在行星球磨机上以180r/min的转速球磨12h,制得金属化膏剂,在TiO2衰减瓷的一面涂覆厚度为40μm的金属化膏剂;
采用丝网印刷机在TiO2衰减瓷的一面分1~3次印刷厚度为35~40μm的金属化层;
g、金属化层的烧结
在卧式氢炉中1200℃,保温15min烧结处理,氢气露点为-60℃,使TiO2衰减瓷一面金属化;
h、电镀镍
将烧结后的TiO2衰减瓷进行电镀镍处理,镍层厚度控制在5~7μm;
i、镀层烧结
电镀结束后,在卧式氢炉中800~900℃,保温15~20min进行镀层烧结处理,氢气露点为-60℃;
j、Q值的测试
将TiO2衰减瓷置于腔体中,用上模具固定住TiO2衰减瓷使其不能发生移动,用连接矢量网络分析仪的探针伸入腔体,在谐振点查看Q值;
k、衰减瓷与腔体的钎焊
采用Q值合格的TiO2衰减瓷,用AgCu28焊料将其焊接至腔体,再次测试Q值,取Q值合格的TiO2衰减瓷,即得。
2.根据权利要求1所述的TiO2衰减瓷的制备方法,其特征在于,步骤i中镀层烧结方法为:电镀结束后,在卧式氢炉中850~900℃,保温15~20min进行镀层烧结处理,氢气露点为-60℃。
3.根据权利要求1所述的TiO2衰减瓷的制备方法,其特征在于,步骤k制备得到的TiO2衰减瓷的体积密度≥3.9g/cm3;气孔率≤0.01%;热导率≥2.8W/m.K;金属化封接强度≥55MPa。
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