CN113471034B - 一种氧化镁次级发射体的制备方法 - Google Patents
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 63
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 30
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001704 evaporation Methods 0.000 claims abstract description 30
- 230000008020 evaporation Effects 0.000 claims abstract description 30
- SJCKRGFTWFGHGZ-UHFFFAOYSA-N magnesium silver Chemical compound [Mg].[Ag] SJCKRGFTWFGHGZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052709 silver Inorganic materials 0.000 claims abstract description 30
- 239000004332 silver Substances 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 230000007704 transition Effects 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 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 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims description 68
- 239000010935 stainless steel Substances 0.000 claims description 34
- 229910001220 stainless steel Inorganic materials 0.000 claims description 34
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- 229910052759 nickel Inorganic materials 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- 238000000151 deposition Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000004544 sputter deposition Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000007872 degassing Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000010453 quartz Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- HZZOEADXZLYIHG-UHFFFAOYSA-N magnesiomagnesium Chemical compound [Mg][Mg] HZZOEADXZLYIHG-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 abstract description 20
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 abstract description 20
- 159000000003 magnesium salts Chemical class 0.000 abstract description 8
- 239000011159 matrix material Substances 0.000 abstract description 8
- 239000013077 target material Substances 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 description 13
- 238000012360 testing method Methods 0.000 description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000010953 base metal Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
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- 206010070834 Sensitisation Diseases 0.000 description 2
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- 238000007885 magnetic separation Methods 0.000 description 2
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- 238000005036 potential barrier Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- 101100327917 Caenorhabditis elegans chup-1 gene Proteins 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
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- AKTIAGQCYPCKFX-FDGPNNRMSA-L magnesium;(z)-4-oxopent-2-en-2-olate Chemical compound [Mg+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O AKTIAGQCYPCKFX-FDGPNNRMSA-L 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
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- 238000002207 thermal evaporation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开来了一种氧化镁次级发射体的制备方法,本发明以金属镍、银、银镁合金作为靶材材料,交替溅射在发射极表面获得复合过渡层。然后将复合过渡层的基体发射极与可挥发有机镁盐和氧化铝粉制成的蒸发源分别放入真空设备中,抽真空后,对蒸发源加热至200℃~300℃,对基体发射极加热至600℃~900℃,再充入氧气和氮气,使发射极表面的复合层在氧气氛围中敏化,同时使镁盐在发射极表面分解并与氧气反应生成氧化镁直接附着在基体表面,即制成氧化镁次级发射体。本发明铯束管用电子倍增器的次级发射体的制作方法,制得的氧化镁膜更加致密和牢固,装配此次级发射体的电子倍增器能满足铯束管长时间连续使用的要求和铯束管的寿命要求。
Description
技术领域
本发明涉及电子倍增器,具体涉及一种磁选态铯束管用电子倍增器的次级发射体的制作方法。
背景技术
铯原子钟是导航定位系统及深空探测器中衡量空间定位精度的的关键设备,应用于高速通信网等地、海、空、天测控与通讯系统。电子倍增器是铯原子钟最为重要的部件,直接决定了铯原子钟的使用寿命、主要技术性能指标以及可靠性等。长期以来,电子倍增器一直未解决的使用寿命短的问题严重制约了铯原子钟工程化应用,根本原因在于现有电子倍增器增益低,且次级发射体在轰击能量较高的离子或较强电子束流长期作用下耐轰击能力弱,增益衰减过快。
电子倍增器主要由电子倍增系统与分压器共两个部分组成,工作时利用电场加速由前级次级发射体发射出的次级电子,使其进入后级次级发射体激发出更多次级电子,实现电子束流逐级放大,从而保证铯原子钟的准确度、信噪比等性能指标。其中,分压器由一串电阻组成,作用是为电子倍增系统提供加速电场,结构相对简单,其设计与加工技术已经非常成熟。
电子倍增系统是电子倍增器的核心关键件,由多个相同的次级发射体组合而成。故单个次级发射体性能的好坏直接决定了电子倍增器的技术指标水平,也是影响铯原子钟性能指标与可靠性的关键因素,因而研究高次级电子发射特性、高稳定性的次级发射体制备工艺对于提高电子倍增器使用寿命至关重要。
目前磁选态铯原子钟所用的铯信号检测铯束管内的电子倍增器的次级发射体都是用基金属附着一层氧化镁(氧化镁)膜形成的,现有氧化镁膜的制作通常有用两种方法,第一种方法是使用银镁合金在真空中升温氧化使其表面自然生成氧化镁膜,第二种方法是在真空中利用磁控溅射的方法在基金属上生成氧化镁膜。但这两种方法制作的氧化镁膜次级发射体的次级发射系数都不稳定,随着使用时间的增加,次级发射系数下降过快,其装配的电子倍增器不能满足铯束管长时间连续使用的要求,更达不到铯束管的寿命要求,并且第二种方法不仅设备复杂,还要求操作人员具有专业技术水平和较强的操作能力,目前只在实验室和研究所进行制作。
发明内容
发明目的:本发明的目的就是针对上述技术的不足,提供一种磁选态铯束管用电子倍增器的次级发射体的制作方法,使制得的氧化镁膜更加致密和牢固,解决现有电子倍增器增益低,且次级发射体在轰击能量较高的离子或较强电子束流长期作用下耐轰击能力弱,增益衰减过快问题,使装配此次级发射体的电子倍增器能满足铯束管长时间连续使用的要求和铯束管的寿命要求。
技术方案:为了实现以上目的,本发明采取的技术方案为:
2、根据权利要求1所述的一种氧化镁次级发射体的制备方法,其特征在于,包括如下步骤:
(1)复合过渡层的制备
(1.1)将加工好的无磁不锈钢发射极基底放置磁控溅射台中;
(1.2)将发射极基底衬底温度加热至500℃,
(1.3)通入1:10比的氩气与氧气,在无磁不锈钢发射极基底上磁控溅射镍层,厚度为100 Å ~200Å;
(1.4)在制备镍层基础上磁控溅射纯银层,厚度为500 Å ~1000 Å;
(1.5)在制备银层基础上,磁控溅射银镁合金层,厚度为200 Å ~1000 Å;
(1.6)将制备好复合过渡层的无磁不锈钢发射极基底冷却至室温,取出,待用;
(2)氧化镁次级发射层制备
(2.1)将可恢复的有机镁盐乙酰丙酮镁与氧化铝粉末充分研磨混合均匀后制备成蒸发源后倒入石英杯(1)中;
(2.2)将步骤(1)制备好复合过渡层的发射极基底置于陶瓷支架(8)上,然后放置于工键盘(2)处;
(2.3)用玻璃钟罩(3)将蒸发源和发射极基底置于封闭腔体中,并开启真空系统(4),抽真空;
(2.4)待真空度达到5×10-4Pa后,开启中频线圈(5)将石墨(6)加热到微红;
(2.5)待石墨(6)变回黑色,且真空度回到5×10-4Pa后,关闭真空系统(4)中的分子泵,仅保留干泵工作;
(2.6)开启电炉丝(7)对蒸发源加热,加热温度至200℃~300℃之间;
(2.7)再次开启中频线圈(5)对发射极基底加热,加热温度至600℃~900℃之间;
(2.8)再按1:4充入氧气和氮气;
(2.9)保持反应时间为20min~30min,得到;
(3)倍增极发射体的组装
将步骤(2)制备有氧化镁次级发射层的发射极基底与盒栅式倍增极基底进行组合,组装得到倍增极发射体。
作为具体技术方案,一种氧化镁次级发射体的制备方法,其包括如下步骤:
(1)复合过渡层的制备
(1.1)将加工好的无磁不锈钢发射极基底放置磁控溅射台中,需要镀膜的一侧向上摆放,零件间彼此不得互相遮挡;
(1.2)当腔体真空度达到优于5. 0×10-4Pa时启动加热系统,将发射极基底衬底温度加热至300℃~500℃并保温1小时,对无磁不锈钢倍增极片进行除气处理;
(1.3)烘烤除气结束后,当温度降到低于150℃时,打开气体质量流量计阀门,调整氩气流量,使真空度保持在2.0×10-2Pa状态下,打开辅助沉积高压电源,调整电压到200V,打开磁控轰击高压电源和膜厚监测仪,调整轰击电压到800V,对镍靶、银靶和银镁合金靶进行预热轰击,预热轰击30s后,当磁控溅射状态稳定后打开镍靶挡板,在无磁不锈钢发射极基底上磁控溅射镍层,厚度为100 Å ~200Å;
(1.4)关闭镍靶挡板,打开银靶挡板继续在无磁不锈钢倍增极片上沉积厚度约为500 Å ~1000 Å银膜;
(1.5)关闭银靶挡板,打开银镁合金靶挡板继续在无磁不锈钢倍增极片上沉积约200 Å ~1000 Å的磁控溅射银镁合金层。
(1.6)迅速关闭银镁合金靶挡板及磁控轰击高压电源、气体质量流量计的阀门,使真空度恢复到优于5.0×10-4Pa,当腔体温度低于80℃后破除腔体真空取出无磁不锈钢倍增极片流转到下工序备用。
(2)氧化镁次级发射层制备
(2.1)将可恢复的有机镁盐乙酰丙酮镁与氧化铝粉末充分研磨混合均匀后制备成蒸发源后倒入石英杯(1)中;
(2.2)将步骤(1)制备好复合过渡层的发射极基底置于陶瓷支架(8)上,然后放置于工键盘(2)处;
(2.3)用玻璃钟罩(3)将蒸发源和发射极基置于封闭腔体中,并开启真空系统(4),抽真空;
(2.4)待真空度达到要求后,开启中频线圈(5)将石墨(6)加热到微红;
(2.5)待石墨(6)变回黑色,且真空度达到要求后,关闭真空系统(4)中的分子泵,仅保留干泵工作;
(2.6)开启电炉丝(7)对蒸发源加热;
(2.7)再次开启中频线圈(5)对发射极基底加热;
(2.8)再充入氧气和氮气;
(2.9)保持一段反应时间,得到;
(3)倍增极发射体的组装
将步骤(2)制备有氧化镁次级发射层的发射极基底与盒栅式倍增极基底进行组合,组装得到倍增极发射体。
作为优选方案,以上所述的一种氧化镁次级发射体的制备方法,其包括如下步骤:
(1)复合过渡层的制备
(1.1)将加工好的无磁不锈钢发射极基底放置磁控溅射台中,需要镀膜的一侧向上摆放,零件间彼此不得互相遮挡;
(1.2)当腔体真空度达到优于5. 0×10-4Pa时启动加热系统,将发射极基底衬底温度加热至300℃~500℃并保温1小时,对无磁不锈钢倍增极片进行除气处理;
(1.3)烘烤除气结束后,当温度降到低于150℃时,打开气体质量流量计阀门,调整氩气流量,使真空度保持在2.0×10-2Pa状态下,打开辅助沉积高压电源,调整电压到200V,打开磁控轰击高压电源和膜厚监测仪,调整轰击电压到800V,对镍靶、银靶和银镁合金靶进行预热轰击,预热轰击30s后,当磁控溅射状态稳定后打开镍靶挡板,在无磁不锈钢发射极基底上磁控溅射镍层,厚度为100 Å ~200Å;
(1.4)关闭镍靶挡板,打开银靶挡板继续在无磁不锈钢倍增极片上沉积厚度约为500 Å ~1000 Å银膜;
(1.5)关闭银靶挡板,打开银镁合金靶挡板继续在无磁不锈钢倍增极片上沉积约200 Å ~1000 Å的磁控溅射银镁合金层。
(1.6)迅速关闭银镁合金靶挡板及磁控轰击高压电源、气体质量流量计的阀门,使真空度恢复到优于5.0×10-4Pa,当腔体温度低于80℃后破除腔体真空取出无磁不锈钢倍增极片流转到下工序备用。
(2)氧化镁次级发射层制备
(2.1)将可恢复的有机镁盐乙酰丙酮镁与氧化铝粉末充分研磨混合均匀后制备成蒸发源后倒入石英杯(1)中;
(2.2)将步骤(1)制备好复合过渡层的发射极基底置于陶瓷支架(8)上,然后放置于工键盘(2)处;
(2.3)用玻璃钟罩(3)将蒸发源和发射极基底置于封闭腔体中,并开启真空系统(4),抽真空;
(2.4)待真空度达到5×10-4Pa后,开启中频线圈(5)将石墨(6)加热到微红;
(2.5)待石墨(6)变回黑色,且真空度回到5×10-4Pa后,关闭真空系统(4)中的分子泵,仅保留干泵工作;
(2.6)开启电炉丝(7)对蒸发源加热,加热温度至200℃~300℃之间;
(2.7)再次开启中频线圈(5)对发射极基底加热,加热温度至600℃~900℃之间;
(2.8)再按1:4充入氧气和氮气;
(2.9)保持反应时间为20min~30min,得到;
(4)倍增极发射体的组装
将步骤(2)制备有氧化镁次级发射层的发射极基底与盒栅式倍增极基底进行组合,组装得到倍增极发射体。
有益效果:
本发明通过将盒栅式倍增极基底和发射极基底二合一结构,以金属镍、银、银镁合金制备复合过渡层,再用可挥发性镁盐在高温通氧的氛围中热解沉积的方式制备氧化镁次级发射体,本发明铯束管用电子倍增器的次级发射体的制作方法,使制得的氧化镁膜更加致密和牢固,使装配此次级发射体的电子倍增器能满足铯束管长时间连续使用的要求和铯束管的寿命要求。
创新点:
1、发射极基体设计;
传统的典型盒栅式倍增极结构(如图1所示)银镁合金敏化工艺中,镁在合金中扩散到达合金表面后,即与周围的氧分子结合生成氧化镁而存留在表面,形成氧化镁发射层,这样敏化后的银镁合金倍增极便具有二次电子发射性能。密实型氧化镁涂层制备工艺是在倍增极的内表面直接蒸涂氧化镁,倍增极两侧的挡板会对蒸涂在内表面的发射层产生影响,内表面两侧的发射层厚度很小甚至近乎没有,这样就会造成有效发射面积减小,甚至会对倍增系统中的电子轨迹造成偏移,从而降低电子倍增器的增益指标,缩短试用寿命。
为了解决上述倍增极内表面两侧对发射层的影响,本发明在原有设计方案的基础上,在结构上将倍增极一分为二:盒栅式倍增极基底和发射极基底(结构如图2所示)。本发明在对发射极基底进行高密度氧化镁涂层制备后,形成了镶嵌在倍增极基底内的氧化镁发射层再将两者进行组合,通过工装模具使两者更好的紧密结合成一体。
2、复合过渡层和氧化镁次级发射层制备筛选实验;
2.1常用氧化镁次级发射层制备方法
3、现有通常用于制备氧化镁次级发射层的工艺有两种,第一种方法是使用银镁合金在真空中升温氧化使其表面自然生成氧化镁膜(表1中的改进前1、2),第二种方法是在真空中利用磁控溅射的方法在基金属上生成氧化镁膜(表2中的改进前1)。
4、高温真空敏化工艺是一种以银为主体,含镁量约3%的真空熔炼银镁合金带加工成倍增极形状,在真空装置中除气后通入一定量气体(如氧、水蒸气、一氧化碳、空气等),在一定量温度下反应一定量时间,使合金内部镁不断扩散并与氧气结合形成氧化镁次级发射层。该方法制备的氧化镁次级发射层由于形成天然的银导电层相对于磁控溅射方案寿命更长,但鉴于国产银镁合金的含镁量和杂质含量指标多数比国外同类材料低,该方法制备的氧化镁次级发射层厚度远低于磁控溅射方案且一致性较差,其次级电子发射能力低于磁控溅射方案;磁控溅射方案是利用氩气作为工作气体镁靶材,在氧气氛围中形成氧化镁膜层附着在零件表面,这种方案制备的氧化镁次级发射层厚度可控,可大幅提升膜层次级发射系数,但往往性能衰减很快,无法满足产品使用要求。
2.2改进的氧化镁次级发射层制备方法
次级发射体制备工艺分层结构改进方案包括磁控溅射沉积部分和热解沉积部分。
(1)改进后的制备方法磁控溅射部分
靶材分别为金属镍靶、金属银靶,纯度均为99.99%以上,银镁合金靶的镁含量为6%~8%。
利用磁控溅射技术获得Ni衬底提高次级发射层的附着力;利用纯银薄膜良好的导电能力作为电荷缓冲层,降低电荷积累,降低MgO薄膜表面势垒,提高电子补充能力;最后在银层与次级电子发射层之间应用掺杂原理增加MgO/Ag金属膜基体结构(如图3所示)。这样做在靠近银薄膜层这一侧,可增加电荷缓冲层厚度,形成更好的电子补充通道,可以进一步消除发射层薄膜内的电荷积累,降低次级电子发射层的表面势垒,进一步提高次级电子发射层的电子补充能力。
(2)改进后的制备方法热解沉积部分
顶层MgO发射层采用镁盐热解沉积氧化镁次级发射层制备工艺,具体制备工装结构如图4所示。以镁盐作为热蒸发源,在氧气氛围中,通过加热的方式,通使镁盐在材料表面热分解并与氧气反应形成氧化镁附着在银层表面,过调节加热电流、充气压力等工艺参数来控制镁盐化学反应速率,制成牢固、致密的氧化镁次级发射层,将制成的次级发射体安装在二次电子发射系数测试台上,进行二次电子发射系数测试,具体结果如表1所示。
表1 改进前后的次级电子发射系数测试结果对比
实例 | 100V | 200V | 300V |
改进前1 | 2.05 | 3.37 | 4.8 |
改进前2 | 2.1 | 3.66 | 5.25 |
改进后1 | 2.77 | 4.79 | 6.4 |
改进后2 | 2.59 | 4.65 | 6.38 |
由表1可以看出,当前次级发射体在200eV下的次级电子发射系数从3.37~3.66提高到4.65~4.79。
并且本发明将制成的次级发射体装配九级电子倍增器,安装在电子倍增器测试台上,进行42天连续测试,取得电子倍增器的性能衰减曲线。测定结果如表2所示:由表2可以对比看出,本发明电子倍增器的预期寿命明显延长。
表2 改进前后装配的电子倍增器测试结果对比
实例 | 初始工作电压 | 工作电压平均上升幅度 | 预期寿命 |
改进前1 | 1747 | 0.408V/天 | 62个月 |
改进后1 | 1582 | 0.159V/天 | 129个月 |
附图说明
图1为现有典型盒栅式倍增极结构示意图。
图2为本发明改进后的倍增极结构示意图。
图3为次级发射体制备工艺分层结构改进示意图。
图4为氧化镁次级发射层制备的专用工装结构示意图。
具体实施方式
下面结合具体实施对本发明的技术方案进行进一步详细地说明,本发明所述的技术特征或连接关系没有进行详细描述的部分均为采用的现有技术。
实施例1
一种氧化镁次级发射体的制备方法,其包括如下步骤:
(1)复合过渡层的制备
(1.1)将加工好的无磁不锈钢发射极基底放置磁控溅射台中,需要镀膜的一侧向上摆放,零件间彼此不得互相遮挡;
(1.2)当腔体真空度达到优于5. 0×10-4Pa时启动加热系统,将发射极基底衬底温度加热至400℃并保温1小时,对无磁不锈钢倍增极片进行除气处理;
(1.3)烘烤除气结束后,当温度降到低于150℃时,打开气体质量流量计阀门,调整氩气流量,使真空度保持在2.0×10-2Pa状态下,打开辅助沉积高压电源,调整电压到200V,打开磁控轰击高压电源和膜厚监测仪,调整轰击电压到800V,对镍靶、银靶和银镁合金靶进行预热轰击,预热轰击30s后,当磁控溅射状态稳定后打开镍靶挡板,在无磁不锈钢发射极基底上磁控溅射镍层,厚度为100 Å ~200Å;
(1.4)关闭镍靶挡板,打开银靶挡板继续在无磁不锈钢倍增极片上沉积厚度约为500 Å ~1000 Å银膜;
(1.5)关闭银靶挡板,打开银镁合金靶挡板继续在无磁不锈钢倍增极片上沉积约200 Å ~1000 Å的磁控溅射银镁合金层。
(1.6)迅速关闭银镁合金靶挡板及磁控轰击高压电源、气体质量流量计的阀门,使真空度恢复到优于5.0×10-4Pa,当腔体温度低于80℃后破除腔体真空取出无磁不锈钢倍增极片流转到下工序备用。
(2)氧化镁次级发射层制备
(2.1)如图4所示,将可恢复的重量比1:1比例均匀混合的有机镁盐乙酰丙酮镁与氧化铝粉末充分研磨混合均匀后制备成蒸发源后倒入石英杯1中;
(2.2)将步骤(1)制备好复合过渡层的发射极基底置于陶瓷支架8上,然后放置于工键盘2处;
(2.3)用玻璃钟罩3将蒸发源和发射极基底置于封闭腔体中,并开启真空系统4,抽真空;
(2.4)待真空度达到5×10-4Pa后,开启中频线圈5将石墨6加热到微红;
(2.5)待石墨6变回黑色,且真空度回到5×10-4Pa后,关闭真空系统4中的分子泵,仅保留干泵工作;
(2.6)开启电炉丝7对蒸发源加热,加热温度至250℃;
(2.7)再次开启中频线圈5对发射极基底加热,加热温度至800℃;
(2.8)再按1:4充入氧气和氮气;
(2.9)保持反应时间为20min,得到;
(3)倍增极发射体的组装
将步骤(2)制备有氧化镁次级发射层的发射极基底与盒栅式倍增极基底进行组合,组装得到倍增极发射体。
本发明提供经过发射极基体设计、复合过渡层制备和氧化镁次级发射层制备等方面改进,制备的电子倍增器经过测试,当前次级发射体在200eV下的次级电子发射系数从3.37~3.66提高到4.65~4.79,具有较好的次级发射体制备水平提升。次级发射性能提升幅度比较明显,体现了在镁盐热解沉积的基础上,实施发射极零件表面处理、完善多层金属膜基体制备改进具有较好的次级发射体制备水平提升。
本发明铯束管用电子倍增器的次级发射体的制作方法,通过磁控溅射复合过渡层,使不锈钢作为基体表面制得的MgO膜致密性和牢固性更高,改善了氧化镁膜的晶体结构,使装配此次级发射体的电子倍增器能满足铯束管长时间连续使用的要求和铯束管的寿命要求。
可以理解地是,以上关于本发明的具体描述,仅用于说明本发明而并非受限于本发明实施例所描述的技术方案,这里无法对所有的实施方式予以穷举,本领域的普通技术人员应当理解,仍然可以对本发明进行修改或等同替换,以达到相同的技术效果;只要满足使用需要,都在本发明的保护范围之内。
Claims (3)
1.一种氧化镁次级发射体的制备方法,其特征在于,包括如下步骤:
(1)复合过渡层的制备
(1.1)将加工好的无磁不锈钢发射极基底放置磁控溅射台中;
(1.2)将发射极基底衬底加热;
(1.3)通入氩气与氧气,在无磁不锈钢发射极基底上磁控溅射镍层;
(1.4)在发射极基底制备镍层基础上再磁控溅射纯银层;
(1.5)在发射极基底制备银层基础上,再磁控溅射银镁合金层;
(1.6)将制备好复合过渡层的无磁不锈钢发射极基底冷却至室温,取出,待用;
(2)氧化镁次级发射层制备
(2.1)将可恢复的有机镁盐乙酰丙酮镁与氧化铝粉末充分研磨混合均匀后制备成蒸发源后倒入石英杯(1)中;
(2.2)将步骤(1)制备好复合过渡层的发射极基底置于陶瓷支架(8)上,然后放置于工键盘(2)处;
(2.3)用玻璃钟罩(3)将蒸发源和发射极基置于封闭腔体中,并开启真空系统(4),抽真空;
(2.4)待真空度达到要求后,开启中频线圈(5)将石墨(6)加热到微红;
(2.5)待石墨(6)变回黑色,且真空度达到要求后,关闭真空系统(4)中的分子泵,仅保留干泵工作;
(2.6)开启电炉丝(7)对蒸发源加热;
(2.7)再次开启中频线圈(5)对发射极基底加热;
(2.8)再充入氧气和氮气;
(2.9)保持一段反应时间,得到;
(3)倍增极发射体的组装
将步骤(2)制备有氧化镁次级发射层的发射极基底与盒栅式倍增极基底进行组合,组装得到倍增极发射体。
2.根据权利要求1所述的一种氧化镁次级发射体的制备方法,其特征在于,包括如下步骤:
(1)复合过渡层的制备
(1.1)将加工好的无磁不锈钢发射极基底放置磁控溅射台中;
(1.2)将发射极基底衬底温度加热至500℃;
(1.3)通入1:10比的氩气与氧气,在无磁不锈钢发射极基底上磁控溅射镍层,厚度为100 Å ~200Å;
(1.4)在制备镍层基础上磁控溅射纯银层,厚度为500 Å ~1000 Å;
(1.5)在制备银层基础上,磁控溅射银镁合金层,厚度为200 Å ~1000 Å;
(1.6)将制备好复合过渡层的无磁不锈钢发射极基底冷却至室温,取出,待用;
(2)氧化镁次级发射层制备
(2.1)将可恢复的有机镁盐乙酰丙酮镁与氧化铝粉末充分研磨混合均匀后制备成蒸发源后倒入石英杯(1)中;
(2.2)将步骤(1)制备好复合过渡层的发射极基底置于陶瓷支架(8)上,然后放置于工键盘(2)处;
(2.3)用玻璃钟罩(3)将蒸发源和发射极基底置于封闭腔体中,并开启真空系统(4),抽真空;
(2.4)待真空度达到5×10-4Pa后,开启中频线圈(5)将石墨(6)加热到微红;
(2.5)待石墨(6)变回黑色,且真空度回到5×10-4Pa后,关闭真空系统(4)中的分子泵,仅保留干泵工作;
(2.6)开启电炉丝(7)对蒸发源加热,加热温度至200℃~300℃之间;
(2.7)再次开启中频线圈(5)对发射极基底加热,加热温度至600℃~900℃之间;
(2.8)再按1:4充入氧气和氮气;
(2.9)保持反应时间为20min~30min,得到;
(3)倍增极发射体的组装
将步骤(2)制备有氧化镁次级发射层的发射极基底与盒栅式倍增极基底进行组合,组装得到倍增极发射体。
3.根据权利要求2所述的一种氧化镁次级发射体的制备方法,其特征在于,包括如下步骤:
(1)复合过渡层的制备
(1.1)将加工好的无磁不锈钢发射极基底放置磁控溅射台中,需要镀膜的一侧向上摆放,零件间彼此不得互相遮挡;
(1.2)当腔体真空度达到小于5. 0×10-4Pa时启动加热系统,将发射极基底衬底温度加热至300℃~500℃并保温1小时,对无磁不锈钢倍增极片进行除气处理;
(1.3)烘烤除气结束后,当温度降到低于150℃时,打开气体质量流量计阀门,调整氩气流量,使真空度保持在2.0×10-2Pa状态下,打开辅助沉积高压电源,调整电压到200V,打开磁控轰击高压电源和膜厚监测仪,调整轰击电压到800V,对镍靶、银靶和银镁合金靶进行预热轰击,预热轰击30s后,当磁控溅射状态稳定后打开镍靶挡板,在无磁不锈钢发射极基底上磁控溅射镍层,厚度为100 Å ~200Å;
(1.4)关闭镍靶挡板,打开银靶挡板继续在无磁不锈钢倍增极片上沉积厚度为500 Å ~1000 Å银膜;
(1.5)关闭银靶挡板,打开银镁合金靶挡板继续在无磁不锈钢倍增极片上沉积200 Å ~1000 Å的磁控溅射银镁合金层;
(1.6)迅速关闭银镁合金靶挡板及磁控轰击高压电源、气体质量流量计的阀门,使真空度恢复到小于5.0×10-4Pa,当腔体温度低于80℃后破除腔体真空,取出无磁不锈钢倍增极片流转到下工序备用;
(2)氧化镁次级发射层制备
(2.1)将可恢复的有机镁盐乙酰丙酮镁与氧化铝粉末充分研磨混合均匀后制备成蒸发源后倒入石英杯(1)中;
(2.2)将步骤(1)制备好复合过渡层的发射极基底置于陶瓷支架(8)上,然后放置于工键盘(2)处;
(2.3)用玻璃钟罩(3)将蒸发源和发射极基底置于封闭腔体中,并开启真空系统(4),抽真空;
(2.4)待真空度达到5×10-4Pa后,开启中频线圈(5)将石墨(6)加热到微红;
(2.5)待石墨(6)变回黑色,且真空度回到5×10-4Pa后,关闭真空系统(4)中的分子泵,仅保留干泵工作;
(2.6)开启电炉丝(7)对蒸发源加热,加热温度至200℃~300℃之间;
(2.7)再次开启中频线圈(5)对发射极基底加热,加热温度至600℃~900℃之间;
(2.8)再按1:4充入氧气和氮气;
(2.9)保持反应时间为20min~30min,得到;
(3)倍增极发射体的组装
将步骤(2)制备有氧化镁次级发射层的发射极基底与盒栅式倍增极基底进行组合,组装得到倍增极发射体。
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