CN114908332B - Method for Accurately Measuring the Thinnest Contribution Thickness of Materials with Low Secondary Electron Emission Coefficient - Google Patents
Method for Accurately Measuring the Thinnest Contribution Thickness of Materials with Low Secondary Electron Emission Coefficient Download PDFInfo
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Abstract
Description
技术领域technical field
本发明属于材料表征领域，涉及一种精确测量低二次电子发射系数材料最薄贡献厚度的方法。The invention belongs to the field of material characterization, and relates to a method for accurately measuring the thinnest contribution thickness of a low secondary electron emission coefficient material.
背景技术Background technique
二次电子的产生是基于入射电子能量，入射角和材料的二次电子发射(SEE)系数。材料的二次电子发射(SEE)系数定义为发射的二次电子与入射在表面上的一次电子的比率。物理过程为一次电子入射到材料一定的入射深度出碰撞产生内二次电子，部分内二次电子碰撞在材料内部耗散，部分内二次电子接力碰撞表层的材料产生内二次电子，不断接力，最后逃逸出表面产生发射的二次电子。材料过薄时，测量得到的二次电子不能代表材料的二次电子发射系数；材料过厚时，在深处产生的内二次电子并不能逃逸出材料表面，不能对材料发射的二次电子有所贡献，所以材料存在一个最薄贡献厚度。不同材料产生SEE系数的最薄贡献厚度不一，为应对航天器微波部件和电子倍增器等器件的科研需求，需要不同材料的最薄贡献厚度进行精确测量。过去都是通过磁控溅射等方式生长薄膜然后进行粗略测试的，因一次电子的入射深度在几纳米到几十纳米之间，原子层沉积技术可以通过循环次数精确控制埃米级薄膜的厚度，近些年在研究最薄贡献厚度的问题上成为关键的技术之一。通常将不同循环次数的薄膜生长在硅衬底上，放入二次电子测试系统进行测试如图2。The generation of secondary electrons is based on the incident electron energy, incident angle and the secondary electron emission (SEE) coefficient of the material. The secondary electron emission (SEE) coefficient of a material is defined as the ratio of emitted secondary electrons to primary electrons incident on a surface. The physical process is that the primary electrons are incident on the material at a certain depth of incidence and collide to generate internal secondary electrons. Part of the internal secondary electron collisions dissipate inside the material, and some internal secondary electrons relay collide with the surface material to generate internal secondary electrons. , and finally escape from the surface to generate emitted secondary electrons. When the material is too thin, the measured secondary electrons cannot represent the secondary electron emission coefficient of the material; when the material is too thick, the internal secondary electrons generated deep in the material cannot escape from the surface of the material, and the secondary electrons emitted by the material cannot contributes, so there is a thinnest contributing thickness in the material. The thinnest contribution thickness of the SEE coefficient produced by different materials is different. In order to meet the scientific research needs of spacecraft microwave components and electron multipliers and other devices, it is necessary to accurately measure the thinnest contribution thickness of different materials. In the past, films were grown by magnetron sputtering and then roughly tested. Because the incident depth of primary electrons is between several nanometers and tens of nanometers, atomic layer deposition technology can precisely control the thickness of angstrom-level films through the number of cycles. , has become one of the key technologies in the study of the thinnest contribution thickness in recent years. Usually, thin films with different cycle times are grown on silicon substrates, and put into the secondary electron test system for testing, as shown in Figure 2.
目前的测试难点为：高SEE系数的材料与硅衬底的SEE系数区别较大，即使是易于潮解的材料，也较为容易获得最少循环次数进而获得材料的最薄贡献厚度，但低SEE系数的材料与硅衬底的SEE系数区别很小，不同循环数的材料二次电子产额差别不大，且有些易于潮解的材料，在测量过程中变得更加难以区分，无法获得最小循环次数如图3。The current test difficulty is: the SEE coefficient of the material with a high SEE coefficient is quite different from that of the silicon substrate. Even for a material that is easy to deliquescence, it is easier to obtain the minimum number of cycles and the thinnest contribution thickness of the material, but the material with a low SEE coefficient The difference between the SEE coefficient of the material and the silicon substrate is very small, and the secondary electron yield of materials with different cycle numbers is not much different, and some materials that are easy to deliquescence become more difficult to distinguish during the measurement process, and the minimum number of cycles cannot be obtained as shown in the figure 3.
发明内容Contents of the invention
本发明针对上述问题，提出了一种精确测量低二次电子发射系数材料最薄贡献厚度的方法。Aiming at the above problems, the present invention proposes a method for accurately measuring the thinnest contribution thickness of materials with low secondary electron emission coefficient.
本发明的技术方案如下：一中精确测量低二次电子发射系数材料最薄贡献厚度的方法，述的方法包括如下步骤：The technical scheme of the present invention is as follows: a method for accurately measuring the thinnest contribution thickness of a low secondary electron emission coefficient material, said method comprising the following steps:
S1、首先选择比目标材料二次电子发射系数高的材料作为衬底，并超过其最薄贡献厚度；S1. First select a material with a higher secondary electron emission coefficient than the target material as the substrate, and exceed its thinnest contribution thickness;
S2、先将衬底放入原子层沉积设备中的反应腔室，进行不同循环次数的目标材料的沉积，制得样品；S2, firstly put the substrate into the reaction chamber of the atomic layer deposition equipment, and deposit the target material with different cycle numbers to obtain samples;
S3、然后将样品放入二次电子测试系统中测量；S3, then put the sample into the secondary electronic testing system for measurement;
S4、获得循环数和二次电子发射产额的对应关系，确定最少循环数；S4. Obtain the corresponding relationship between the number of cycles and the yield of secondary electron emission, and determine the minimum number of cycles;
S5、最后在硅衬底上生长最少循环次数的目标材料，进行薄膜厚度测量。S5. Finally, the target material with the minimum number of cycles is grown on the silicon substrate, and the thickness of the film is measured.
进一步地，步骤1中所述的比相对目标材料二次电子发射系数高的材料作为衬底，并超过其最薄贡献厚度，例如当目标材料为Cu、ZnO、B2O3等二次电子发射系数约为2时，超过8nm的Al2O3二次电子发射系数约为4，超过20nm的MgO二次电子发射系数约为8，此时超过20nm的MgO、超过8nm的Al2O3都可以作为衬底，当目标材料为Al2O3时，则可以选择超过20nm的MgO作为衬底。Further, the material with a higher secondary electron emission coefficient than the target material mentioned in step 1 is used as the substrate, and exceeds its thinnest contribution thickness, for example, when the target material is Cu, ZnO, B2O3 , etc. When the emission coefficient is about 2, the secondary electron emission coefficient of Al 2 O 3 over 8nm is about 4, and the secondary electron emission coefficient of MgO over 20nm is about 8. At this time, MgO over 20nm and Al 2 O 3 over 8nm Both can be used as the substrate. When the target material is Al 2 O 3 , you can choose MgO over 20nm as the substrate.
步骤S1中所述的超过20nm的MgO，通过Mg(Cp)2和水蒸气反应生成，将Mg(Cp)2加热到50～60℃，反应腔室温度为200℃，原子层沉积技术生长一层MgO原子层的循环通气时间和顺序:Mg(Cp)2/N2/H2O/N2＝150ms/4s/150ms/4s，上述过程循环180次以上；The MgO exceeding 20nm described in step S1 is generated by the reaction of Mg(Cp) 2 and water vapor, the Mg(Cp) 2 is heated to 50-60°C, the temperature of the reaction chamber is 200°C, and the atomic layer deposition technique is used to grow a The cycle ventilation time and sequence of the MgO atomic layer: Mg(Cp) 2 /N 2 /H 2 O/N 2 = 150ms/4s/150ms/4s, the above process is cycled more than 180 times;
步骤S1中所述超过8nm的Al2O3，通过三甲基铝TMA和水蒸气反应生成，反应腔室温度为200℃，原子层沉积生长一层Al2O3原子层的循环通气时间和顺序：TMA/N2/H2O/N2＝150ms/4s/150ms/4s，上述过程循环50次以上；The Al 2 O 3 exceeding 8nm described in step S1 is generated by the reaction of trimethylaluminum TMA and water vapor, the temperature of the reaction chamber is 200°C, the cycle aeration time and Sequence: TMA/N 2 /H 2 O/N 2 = 150ms/4s/150ms/4s, the above process cycled more than 50 times;
进一步地，步骤S4中所述的最少循环数，通过获得循环次数和二次电子发射产额的对应关系图获得，邻近循环次数的二次电子发射产额差值第一次出现在0.3范围内，这两个邻近循环数中最小即可认定为最少循环次数。Further, the minimum number of cycles described in step S4 is obtained by obtaining the correspondence relationship between the number of cycles and the yield of secondary electron emission, and the difference in yield of secondary electron emission adjacent to the number of cycles appears within the range of 0.3 for the first time , the smallest of these two adjacent cycle numbers can be identified as the minimum number of cycles.
进一步地，步骤S5中所述的薄膜厚度测量，可通过椭偏仪、膜厚仪等进行测量纳米级薄膜的厚度。Further, the thickness measurement of the film in step S5 can be performed by using an ellipsometer, a film thickness meter, etc. to measure the thickness of the nanoscale film.
本发明的优点和积极效果如下：Advantage of the present invention and positive effect are as follows:
1、本发明通过选择高二次电子发射系数的材料作为衬底,成功解决了精确测量低二次电子发射系数材料最薄贡献厚度问题见图4。1. The present invention successfully solves the problem of accurately measuring the thinnest contribution thickness of a material with a low secondary electron emission coefficient by selecting a material with a high secondary electron emission coefficient as the substrate, as shown in FIG. 4 .
2、通过这种测试方法选择了MgO材料作为衬底，成功测量得到了低二次电子发射系数且易潮解的B2O3的最薄贡献厚度见图5。2. Through this test method, MgO material was selected as the substrate, and the thinnest contribution thickness of B 2 O 3 with low secondary electron emission coefficient and deliquescence was successfully measured, as shown in Figure 5.
3、过去需要大量制备样品进行测量求平均值，通过这种测试方法需要测量样品的数量减少到几个样品，就可以顺利寻找到低二次电子发射系数材料最薄贡献厚度的生长循环次数。3. In the past, it was necessary to prepare a large number of samples for measurement and average value. With this test method, the number of measured samples needs to be reduced to a few samples, and the growth cycle number of the thinnest contribution thickness of the low secondary electron emission coefficient material can be found smoothly.
附图说明Description of drawings
图1为测试低二次电子发射系数材料的方法示意图。Fig. 1 is a schematic diagram of a method for testing a material with a low secondary electron emission coefficient.
图2为在硅衬底上生长不同循环次数的Al2O3二次电子发射系数随入射电子能量的变化。Figure 2 shows the variation of the secondary electron emission coefficient of Al 2 O 3 grown on a silicon substrate with different cycle times with the incident electron energy.
图3为在硅衬底上生长不同循环次数的B2O3二次电子发射系数随入射电子能量的变化。Fig. 3 shows the variation of the secondary electron emission coefficient of B 2 O 3 grown on silicon substrates with different cycle times with the energy of incident electrons.
图4为在硅衬底上生长315次循环的MgO，然后再生长不同循环次数的B2O3的样品的二次电子发射系数随入射电子能量的变化。Fig. 4 shows the change of the secondary electron emission coefficient of the sample grown on the silicon substrate for 315 cycles of MgO, and then B 2 O 3 with different cycles as a function of the energy of the incident electrons.
图5为在硅衬底上生长315次循环的MgO，然后再生长不同循环次数的B2O3。在相同入射电子能量下，二次电子发射系数随不同循环次数的B2O3的变化。Figure 5 shows the growth of MgO on a silicon substrate for 315 cycles, followed by the growth of B 2 O 3 with different cycles. Variation of secondary electron emission coefficient with different cycle numbers of B2O3 at the same incident electron energy.
图6为在硅衬底上生长315次循环的MgO，然后再生长不同循环次数的Al2O3。在相同入射电子能量下，二次电子发射系数随不同循环次数的Al2O3的变化。Figure 6 shows MgO grown on a silicon substrate for 315 cycles, and then Al 2 O 3 grown with different cycles. Variation of secondary electron emission coefficient with different cycle numbers of Al2O3 at the same incident electron energy.
附图标注说明：1-目标材料；2-高SEE材料，3-硅衬底。Notes on drawings: 1-target material; 2-high SEE material, 3-silicon substrate.
具体实施方式Detailed ways
下面将结合附图和具体实例对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific examples.
根据本发明的一个实施例，提出一种高二次电子发射系数薄膜的制备方法，包括以下步骤：According to one embodiment of the present invention, a kind of preparation method of high secondary electron emission coefficient film is proposed, comprising the following steps:
S1、首先选择比B2O3的SEE系数高的高SEE材料2，MgO作为衬底。S1. First, select a high SEE material 2 with a higher SEE coefficient than B 2 O 3 , MgO as the substrate.
S2、先将MgO衬底放入原子层沉积设备中的反应腔室，进行不同循环数的B2O3的沉积，制得样品。S2. First put the MgO substrate into the reaction chamber of the atomic layer deposition equipment, and deposit B 2 O 3 with different cycle numbers to prepare samples.
S3、然后将样品放入二次电子测试系统中测量。S3, and then put the sample into the secondary electronic testing system for measurement.
S4、不断重复S2和S3获得循环次数和二次电子发射产额的对应关系，确定最少循环次数。S4. Constantly repeating S2 and S3 to obtain the corresponding relationship between the number of cycles and the yield of secondary electron emission, and determine the minimum number of cycles.
S5、最后在硅衬底3上生长最少循环次数的目标材料1，进行薄膜厚度测量。S5. Finally, the target material 1 with the minimum number of cycles is grown on the silicon substrate 3, and the thickness of the film is measured.
进一步地，步骤S1中所述的MgO，通过Mg(Cp)2和水蒸气反应生成，将Mg(Cp)2加热到50～80℃，反应腔室温度为200℃，原子层沉积技术生长一层MgO原子层的循环通气时间和顺序:Mg(Cp)2/N2/H2O/N2＝150ms/4s/150ms/4s，上述过程循环180次以上。Further, the MgO described in step S1 is generated by the reaction of Mg(Cp) 2 and water vapor, the Mg(Cp) 2 is heated to 50-80°C, the temperature of the reaction chamber is 200°C, and the atomic layer deposition technique is used to grow a The cycle ventilation time and sequence of MgO atomic layer: Mg(Cp) 2 /N 2 /H 2 O/N 2 =150ms/4s/150ms/4s, the above process cycled more than 180 times.
进一步地，步骤S2中所述的不同循环数的B2O3，通过BCl3和水蒸气反应生成，反应腔室温度为20～50℃，原子层沉积生长一层B2O3原子层的循环通气时间和顺序：BCl3/N2/H2O/N2＝150ms/4s/300ms/4s生长一层B2O3，样品一：循环1次，样品二：循环2次，样品三：循环3次，样品四：循环4次，样品五：循环5次，样品六：循环6次，样品六：循环9次；Further, B 2 O 3 with different cycle numbers described in step S2 is generated by the reaction of BCl 3 and water vapor, the temperature of the reaction chamber is 20-50°C, and a layer of B 2 O 3 atomic layer is grown by atomic layer deposition Cycle aeration time and sequence: BCl 3 /N 2 /H 2 O/N 2 =150ms/4s/300ms/4s to grow a layer of B 2 O 3 , sample 1: cycle 1 time, sample 2: cycle 2 times, sample 3 : Cycle 3 times, Sample 4: Cycle 4 times, Sample 5: Cycle 5 times, Sample 6: Cycle 6 times, Sample 6: Cycle 9 times;
进一步地，步骤S4中所述的B2O3最少循环次数为5，B2O3循环次数和二次电子发射产额的对应关系见图5，循环次数在5和9之间的二次电子发射产额差值在0.3范围内，因此认定5为B2O3最少循环次数。Further, the minimum cycle number of B 2 O 3 described in step S4 is 5, and the corresponding relationship between the cycle number of B 2 O 3 and the secondary electron emission yield is shown in Figure 5, and the secondary electron emission yield between 5 and 9 cycles The difference of electron emission yield is in the range of 0.3, so 5 is considered as the minimum cycle number of B 2 O 3 .
进一步地，步骤S5中所述的进行薄膜厚度测量，通过椭偏仪进行测量拟合得到。Further, the film thickness measurement described in step S5 is obtained through measurement and fitting by ellipsometer.
根据本发明的另一个实施例，提出一种高二次电子发射系数薄膜的制备方法，包括以下步骤：According to another embodiment of the present invention, a kind of preparation method of high secondary electron emission coefficient film is proposed, comprising the following steps:
S1、首先选择比Al2O3的SEE系数高的高SEE材料2，MgO作为衬底。S1. First, select a high SEE material 2 with a higher SEE coefficient than Al 2 O 3 , MgO as the substrate.
S2、先将MgO衬底放入原子层沉积设备中的反应腔室，进行不同循环数的Al2O3的沉积，制得样品。S2. First, put the MgO substrate into the reaction chamber of the atomic layer deposition equipment, and deposit Al 2 O 3 with different cycle numbers to prepare samples.
S3、然后将样品放入二次电子测试系统中测量。S3, and then put the sample into the secondary electronic testing system for measurement.
S4、不断重复S2和S3获得循环次数和二次电子发射产额的对应关系，确定最少循环次数。S4. Constantly repeating S2 and S3 to obtain the corresponding relationship between the number of cycles and the yield of secondary electron emission, and determine the minimum number of cycles.
S5、最后在硅衬底3上生长最少循环次数的目标材料1，进行薄膜厚度测量。S5. Finally, the target material 1 with the minimum number of cycles is grown on the silicon substrate 3, and the thickness of the film is measured.
进一步地，步骤S1中所述的MgO，通过Mg(Cp)2和水蒸气反应生成，将Mg(Cp)2加热到50～80℃，反应腔室温度为200℃，原子层沉积技术生长一层MgO原子层的通气时间和顺序:Mg(Cp)2/N2/H2O/N2＝150ms/4s/150ms/4s，上述过程循环180次以上。Further, the MgO described in step S1 is generated by the reaction of Mg(Cp) 2 and water vapor, the Mg(Cp) 2 is heated to 50-80°C, the temperature of the reaction chamber is 200°C, and the atomic layer deposition technique is used to grow a The ventilation time and sequence of the atomic layer of MgO: Mg(Cp) 2 /N 2 /H 2 O/N 2 =150ms/4s/150ms/4s, the above process cycled more than 180 times.
进一步地，步骤S2中所述的不同循环数的Al2O3，通过TMA(三甲基铝)和水蒸气反应生成，反应腔室温度为200℃，原子层沉积生长一层Al2O3原子层的循环通气时间和顺序：TMA/N2/H2O/N2＝150ms/4s/150ms/4s生长一层Al2O3，样品一：循环3次，样品二：循环6次，样品三：循环10，样品四：循环30次，样品五：循环70次,样品六：循环100次，样品六：循环200次。Further, Al 2 O 3 with different cycle numbers described in step S2 is generated by the reaction of TMA (trimethylaluminum) and water vapor, the temperature of the reaction chamber is 200°C, and a layer of Al 2 O 3 is grown by atomic layer deposition Circulation time and sequence of atomic layer: TMA/N 2 /H 2 O/N 2 =150ms/4s/150ms/4s to grow a layer of Al 2 O 3 , sample 1: cycle 3 times, sample 2: cycle 6 times, Sample 3: 10 cycles, Sample 4: 30 cycles, Sample 5: 70 cycles, Sample 6: 100 cycles, Sample 6: 200 cycles.
进一步地，步骤S4中所述的Al2O3最少循环次数为50，B2O3循环次数和二次电子发射产额的对应关系见图6，循环次数在50和70之间的二次电子发射产额差值在0.3范围内，因此认定50为Al2O3最少循环次数。Further, the minimum cycle number of Al 2 O 3 described in step S4 is 50, and the corresponding relationship between the cycle number of B 2 O 3 and the secondary electron emission yield is shown in Figure 6, and the secondary electron emission yield between 50 and 70 cycles The electron emission yield difference is in the range of 0.3, so 50 is considered as the minimum cycle number of Al 2 O 3 .
进一步地，步骤S5中所述的进行薄膜厚度测量，通过椭偏仪进行测量拟合得到。Further, the film thickness measurement described in step S5 is obtained through measurement and fitting by ellipsometer.
需要说明的是，本发明中的选择高二次发射系数材料作为衬底，特别是选择厚度在20nm以上的MgO对本发明的实施非常重要，是本发明的关键。It should be noted that the selection of materials with high secondary emission coefficients as the substrate in the present invention, especially the selection of MgO with a thickness of more than 20 nm is very important to the implementation of the present invention and is the key of the present invention.
本发明实施例并非用以限定本发明。任何熟悉本领域的技术人员，在不脱离本发明技术方案范围情况下，都可利用上述揭示的方法和技术内容对本发明技术方案作出许多可能的变动和修饰，或修改为等同变化的等效实施例。因此，凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化及修饰，均仍属于本发明技术方案保护的范围内。The embodiments of the present invention are not intended to limit the present invention. Any person familiar with the art, without departing from the scope of the technical solution of the present invention, can use the methods and technical content disclosed above to make many possible changes and modifications to the technical solution of the present invention, or modify it into an equivalent implementation of equivalent changes example. Therefore, any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention, which do not deviate from the technical solution of the present invention, still fall within the protection scope of the technical solution of the present invention.
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