CN103924204A - Method for preparing C axis oriented aluminium nitride thin film on surface of titanium alloy substrate - Google Patents
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 76
- 239000000758 substrate Substances 0.000 title claims abstract description 63
- 239000010409 thin film Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 21
- 229910017083 AlN Inorganic materials 0.000 title abstract 12
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title abstract 12
- 239000010408 film Substances 0.000 claims abstract description 54
- 238000004544 sputter deposition Methods 0.000 claims abstract description 24
- 238000005498 polishing Methods 0.000 claims abstract description 18
- 230000003746 surface roughness Effects 0.000 claims abstract description 18
- 238000005546 reactive sputtering Methods 0.000 claims abstract description 12
- 238000000151 deposition Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 52
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000012495 reaction gas Substances 0.000 claims description 2
- 239000013077 target material Substances 0.000 claims description 2
- 238000010897 surface acoustic wave method Methods 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 11
- 239000000956 alloy Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000035882 stress Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000013590 bulk material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
Description
技术领域technical field
本发明属于薄膜材料制备技术领域，涉及氮化铝薄膜制备工艺以及薄膜型声表面波传感器件技术，尤其涉及在钛合金表面制备取向氮化铝薄膜的方法。The invention belongs to the technical field of thin film material preparation, and relates to an aluminum nitride thin film preparation process and a thin film surface acoustic wave sensor technology, in particular to a method for preparing an orientation aluminum nitride thin film on the surface of a titanium alloy.
背景技术Background technique
氮化铝为典型的宽带隙III-V化合物，具有一系列优良的物理化学性质：化学稳定性好、硬度高、高压电系数、高热导率、低热膨胀系数、直带隙宽度比较宽、声波传播速度快等。在声表面波器件领域中，随着无线通信系统和数据传输技术的快速发展，使声表面波器件向GHz以上的频段发展，而氮化铝薄膜具有所有无机非贴点性压电材料中最高的声表面波速度，因此可以成为有效提高声表面波器件中心频率的压电材料。而且制作声表面波器件所需要的高化学稳定性好、高热导率、低热膨胀系数、大击穿电场、高声速、高机电耦合系数以及与半导体工艺相兼容的压电材料，氮化铝薄膜能够很好的满足这些要求。因此氮化铝成为研制薄膜型声表面波器件的首选压电材料。Aluminum nitride is a typical wide bandgap III-V compound with a series of excellent physical and chemical properties: good chemical stability, high hardness, high piezoelectric coefficient, high thermal conductivity, low thermal expansion coefficient, wide straight bandgap width, Sound waves travel fast. In the field of surface acoustic wave devices, with the rapid development of wireless communication systems and data transmission technologies, surface acoustic wave devices have developed to frequency bands above GHz, and aluminum nitride films have the highest performance among all inorganic non-stick piezoelectric materials. Therefore, it can become a piezoelectric material that can effectively improve the center frequency of surface acoustic wave devices. Moreover, the high chemical stability, high thermal conductivity, low thermal expansion coefficient, large breakdown electric field, high sound velocity, high electromechanical coupling coefficient and piezoelectric materials compatible with semiconductor technology required for the production of surface acoustic wave devices, aluminum nitride film These requirements can be well met. Therefore, aluminum nitride has become the preferred piezoelectric material for the development of thin-film surface acoustic wave devices.
钛合金因其具有强度高、耐腐蚀性好、耐热性高等特点被广泛应用于各个领域。在航空领域特别是航空发动机压气机部件使用的大量的高温钛合金材料，因此能够准确测量出这些应用于各种部件的钛合金材料在日常工作中的所承受的应力和温度是当前研究的热点。而目前制作用于测量钛合金表面的应力与温度声表面波传感器的方法主要是：通过在单晶压电敏感块材上制作声表面波传感器，然后通过粘接剂将其贴附于待测的钛合金板材上来敏感钛合金所承受的应力与温度变化。由于这种方法对粘接剂的粘接强度还有人为的粘接操作有很高的要求，而且随着使用时间的推移，粘接剂的老化脱落也会导致传感器的性能减弱或消失，甚至脱落。这些都对传感器的可靠性和使用寿命有着巨大影响。Titanium alloys are widely used in various fields because of their high strength, good corrosion resistance, and high heat resistance. A large number of high-temperature titanium alloy materials are used in the aviation field, especially aeroengine compressor parts. Therefore, it is a current research hotspot to be able to accurately measure the stress and temperature of these titanium alloy materials used in various parts in daily work. . At present, the method of making a surface acoustic wave sensor for measuring the stress and temperature of the titanium alloy surface is mainly: by making a surface acoustic wave sensor on a single crystal piezoelectric sensitive block material, and then attaching it to the surface to be tested by an adhesive The titanium alloy plate is sensitive to the stress and temperature changes of the titanium alloy. Because this method has high requirements on the bonding strength of the adhesive and the artificial bonding operation, and as the use time goes by, the aging and falling off of the adhesive will also cause the performance of the sensor to weaken or disappear, or even fall off. These all have a huge impact on the reliability and service life of the sensor.
为了解决上述利用单晶压电块材制作声表面波传感器应用于测量钛合金应力与温度变化可靠性低、寿命短的问题，若能在钛合金表面直接沉积高(002)轴取向、低表面粗糙度的氮化铝压电敏感薄膜，则有望解决氮化铝薄膜型声表面波器件在航空、航天领域的应用中的可靠性问题。In order to solve the problems of low reliability and short service life of the surface acoustic wave sensor made of single crystal piezoelectric bulk material for measuring the stress and temperature changes of titanium alloy, if the high (002) axis orientation and low surface area can be directly deposited on the surface of titanium alloy The rough aluminum nitride piezoelectric sensitive thin film is expected to solve the reliability problem of aluminum nitride thin film surface acoustic wave devices in the application of aviation and aerospace fields.
发明内容Contents of the invention
本发明提供一种在钛合金基片表面制备取向氮化铝薄膜的方法，该方法所制备的基于钛合金的氮化铝薄膜具有垂直于(002)晶面(即C轴)取向、低表面粗糙度的特点，适于在钛合金表面直接制作声表面波传感器，为氮化铝薄膜型声表面波传感器在航空、航天领域的高可靠性应用提供了一种可能。The invention provides a method for preparing an oriented aluminum nitride film on the surface of a titanium alloy substrate. The aluminum nitride film based on a titanium alloy prepared by the method has an orientation perpendicular to the (002) crystal plane (ie, the C axis) and a low surface area. The characteristics of roughness are suitable for directly manufacturing surface acoustic wave sensors on the surface of titanium alloys, which provides a possibility for the high reliability application of aluminum nitride thin film surface acoustic wave sensors in the field of aviation and aerospace.
本发明技术方案如下：Technical scheme of the present invention is as follows:
一种在钛合金基片表面制备C轴取向氮化铝薄膜的方法，包括以下步骤：A method for preparing a C-axis orientation aluminum nitride film on the surface of a titanium alloy substrate, comprising the following steps:
步骤1：对钛合金基片表面进行抛光处理，以尽量降低钛合金基片的表面粗糙度；Step 1: Polishing the surface of the titanium alloy substrate to minimize the surface roughness of the titanium alloy substrate;
步骤2：高温阶段氮化铝薄膜的预溅射沉积。采用反应溅射薄膜制备工艺，在钛合金基片表面预溅射沉积氮化铝薄膜；预溅射时，钛合金基片温度控制在350～450℃温度范围内。Step 2: Pre-sputter deposition of aluminum nitride film in high temperature stage. The reactive sputtering film preparation process is used to pre-sputter and deposit the aluminum nitride film on the surface of the titanium alloy substrate; during the pre-sputtering, the temperature of the titanium alloy substrate is controlled within the temperature range of 350-450°C.
步骤2：低温阶段氮化铝薄膜的溅射沉积。当步骤2所述高温阶段氮化铝薄膜的预溅射沉积厚度超过步骤1抛光处理后钛合金基片的表面粗糙度后，让钛合金基片自然降温至100～150℃温度范围内，在钛合金基片自然降温及120～150℃温度范围内，持续进行磁控反应溅射沉积氮化铝薄膜直至氧化铝薄膜达到需要的厚度。Step 2: Sputtering deposition of aluminum nitride film in low temperature stage. When the pre-sputtering deposition thickness of the aluminum nitride film in the high temperature stage described in step 2 exceeds the surface roughness of the titanium alloy substrate after the polishing treatment in step 1, let the titanium alloy substrate naturally cool down to a temperature range of 100-150° C. The titanium alloy substrate is cooled naturally and within the temperature range of 120-150°C, and the aluminum nitride film is continuously deposited by magnetron reactive sputtering until the aluminum oxide film reaches the required thickness.
虽然钛合金表面含有(002)晶面的钛原子，能够提供沿(002)晶面定向生长(即C轴取向)氮化铝的成核中心，但由于钛合金材料硬度很高，难以抛光至镜面标准，所以普通钛合金基片即使做了一定的抛光处理，仍然在其表面溅射沉积出C轴取向的氮化铝薄膜，得不到C轴取向的氮化铝薄膜，自然就无法在钛合金表面直接制作氮化铝薄膜型声表面波传感器。Although the surface of the titanium alloy contains titanium atoms on the (002) crystal plane, which can provide the nucleation center for AlN growth along the (002) crystal plane (that is, the C-axis orientation), but due to the high hardness of the titanium alloy material, it is difficult to polish to The mirror surface standard, so even if the ordinary titanium alloy substrate has been polished to a certain extent, a C-axis-oriented aluminum nitride film is still deposited on the surface by sputtering. If the C-axis-oriented aluminum nitride film cannot be obtained, it is naturally impossible to Aluminum nitride thin-film surface acoustic wave sensors are directly fabricated on the surface of titanium alloy.
本发明提供的在钛合金基片表面制备C轴取向氮化铝薄膜的方法，实质上是首先在高温段(350～450℃温度范围内)采用磁控反应溅射薄膜制备工艺在钛合金基片表面预溅射一层氮化铝，利用溅射粒子附着于基片表面时会因基片高温而带来粒子高表面迁移率、高流动性，而高的表面迁移率和高流动性会驱动溅射粒子优先去填补钛合金表面的不平整处，以弥补因钛合金材料高强度，高硬度所导致表面抛光难度高，基片表面难以达到镜面标准的缺陷；当预溅射的氮化铝薄膜厚度超过钛合金基片的表面粗糙度后，让钛合金基片自然降温至C轴取向氮化铝薄膜的最佳磁控反应溅射温度(100～150℃)，在钛合金基片自然降温及100～150℃温度范围内，持续进行磁控反应溅射沉积氮化铝薄膜直至氧化铝薄膜达到需要的厚度，最终得到C轴取向的氮化铝薄膜。The method for preparing a C-axis-oriented aluminum nitride film on the surface of a titanium alloy substrate provided by the present invention is essentially to first use a magnetron reactive sputtering film preparation process on a titanium alloy substrate A layer of aluminum nitride is pre-sputtered on the surface of the chip. When the sputtered particles are attached to the surface of the substrate, the high surface mobility and high fluidity of the particles will be brought about by the high temperature of the substrate, and the high surface mobility and high fluidity will cause Drive the sputtering particles to fill the unevenness of the titanium alloy surface first, so as to make up for the high strength and high hardness of the titanium alloy material, which makes the surface polishing difficult, and the surface of the substrate is difficult to meet the mirror surface defects; when the pre-sputtering nitriding After the thickness of the aluminum film exceeds the surface roughness of the titanium alloy substrate, let the titanium alloy substrate naturally cool down to the optimum magnetron reactive sputtering temperature (100-150°C) for the C-axis oriented aluminum nitride film. Naturally lowering the temperature and within the temperature range of 100-150°C, the aluminum nitride film is continuously deposited by magnetron reactive sputtering until the aluminum oxide film reaches the required thickness, and finally a C-axis oriented aluminum nitride film is obtained.
但是，在高温预溅射氮化铝时，过高的温度(大于470℃)时氮化铝薄膜会与钛合金逐渐发生反应，生成本发明不希望的化合物；而较低的温度(300℃左右)时，生长的氮化铝薄膜上会生成少量非(002)晶向，并且基片表面的粒子迁移率和流动性也会随之降低。综合考虑，本发明选择350～450℃的温度范围作为预溅射氮化铝薄膜的生长温度。But, when high temperature pre-sputtering aluminum nitride, aluminum nitride thin film can react gradually with titanium alloy during too high temperature (greater than 470 ℃), generates the compound that the present invention does not want; And lower temperature (300 ℃ or so), a small amount of non-(002) crystal orientation will be generated on the grown aluminum nitride film, and the particle mobility and fluidity on the substrate surface will also decrease accordingly. Considering comprehensively, the present invention selects a temperature range of 350-450° C. as the growth temperature of the pre-sputtered aluminum nitride film.
需要进一步说明的是：1、步骤1对钛合金基片表面进行抛光处理时，选择采用抛光机进行抛光，或者配合使用砂纸和抛光膏进行抛光；抛光完毕后应对钛合金基片表面进行清洁处理；2、所述清洁处理先后采用丙酮、酒精、去离子水对钛合金基片表面进行清洗，然后烘干待用；3、步骤2和步骤3中所述磁控反应溅射采用的靶材为铝靶，工作气体为氩气、反应气体为氮气；4、所述钛合金基片的表面粗糙度采用平均表面粗糙度或均方根表面粗糙度进行度量；步骤2中预溅射沉积的氮化铝薄膜厚度以不低于所述钛合金基片的表面粗糙度的两倍为宜。It needs to be further explained: 1. When polishing the surface of the titanium alloy substrate in step 1, choose to use a polishing machine for polishing, or use sandpaper and polishing paste for polishing; after polishing, the surface of the titanium alloy substrate should be cleaned. ; 2. The cleaning process uses acetone, alcohol, and deionized water to clean the surface of the titanium alloy substrate, and then dry it for use; 3. The target material used in the magnetron reactive sputtering described in step 2 and step 3 It is an aluminum target, the working gas is argon, and the reaction gas is nitrogen; 4. The surface roughness of the titanium alloy substrate is measured by the average surface roughness or the root mean square surface roughness; the pre-sputtered deposition in step 2 The thickness of the aluminum nitride film is preferably not less than twice the surface roughness of the titanium alloy substrate.
本发明的有益效果是：The beneficial effects of the present invention are:
本发明在钛合金基片表面成功制备出C轴取向的氮化铝薄膜，所制备的氮化铝薄膜具有高度的C轴取向、较低的表面粗糙度和良好的压电效应，从而为氮化铝薄膜型声表面波器件直接做在钛合金材料表面提供了材料基础，并为氮化铝薄膜型声表面波传感器在航空、航天领域的高可靠性应用提供了一种可能。The present invention successfully prepares a C-axis-oriented aluminum nitride film on the surface of a titanium alloy substrate, and the prepared aluminum nitride film has a high degree of C-axis orientation, low surface roughness and good piezoelectric effect, thereby being nitrogen AlN film-type surface acoustic wave devices directly made on the surface of titanium alloy materials provide a material basis, and provide a possibility for high-reliability applications of aluminum nitride film-type surface acoustic wave sensors in the fields of aviation and aerospace.
附图说明Description of drawings
图1待沉积氮化铝薄膜的钛合金基板的XRD测试图。Figure 1 is an XRD test pattern of a titanium alloy substrate to be deposited with an aluminum nitride film.
图2400℃下预溅射30分钟所生长氮化铝薄膜的XRD测试图。Fig. 2 XRD test pattern of aluminum nitride film grown by pre-sputtering at 30 minutes at 400°C.
图3400℃自降温溅射6小时后所制最终样品的XRD测试图。Figure 3 is the XRD test pattern of the final sample prepared after sputtering at 400°C for 6 hours.
图4最终样品表面的SEM测试图。Figure 4 SEM test image of the final sample surface.
图5最终样品表面的AFM测试图。Figure 5 AFM test image of the final sample surface.
具体实施方式Detailed ways
下面结合附图对本发明做进一步说明：The present invention will be further described below in conjunction with accompanying drawing:
一种在钛合金基片表面制备C轴取向氮化铝薄膜的方法，包括以下步骤：A method for preparing a C-axis orientation aluminum nitride film on the surface of a titanium alloy substrate, comprising the following steps:
a.首先对经过抛光膏粗抛光的TC4钛合金基片用超声波清洗，依次采用丙酮，酒精，去离子水清洗基片，并用氮气吹干，将清洗干净的基板放入充入纯氮气的烘干箱中加热到120℃烘干1小时以除去基片表面的水分。防止污渍与水汽影响生长薄膜的质量。a. First, clean the TC4 titanium alloy substrate roughly polished by polishing paste with ultrasonic waves, then use acetone, alcohol, and deionized water to clean the substrate in turn, and blow it dry with nitrogen gas. Put the cleaned substrate into a drying oven filled with pure nitrogen gas. Heat to 120°C in a dry box and dry for 1 hour to remove moisture on the surface of the substrate. Prevent stains and moisture from affecting the quality of the grown film.
b.将清洗与烘干好的基片利用夹具将其放置于中频磁控溅射仪的承片台上，然后关闭腔体。正常启动磁控溅射仪器，对腔体抽真空到5.0×10-4Pa以下，并开启样品加热电源，将样品台加热至400°C并维持，然后再次将真空抽到5.0×10-4pa以下即可。b. Place the cleaned and dried substrate on the substrate stage of the intermediate frequency magnetron sputtering apparatus with a fixture, and then close the cavity. Start the magnetron sputtering instrument normally, evacuate the cavity to below 5.0×10 -4 Pa, turn on the sample heating power, heat the sample stage to 400°C and maintain it, and then evacuate the chamber to 5.0×10 -4 again below pa.
c.关闭溅射挡板，开启样品台旋转电源，开启中频频电源进行预热5min中，腔体内通入氩气90SCCM左右进行，调节真空度到0.94Pa左右并调节电源电压使其产生辉光，并调节溅射功率为400瓦以对铝靶材进行预溅射15min中，清除靶材表面可能含有的杂质，然后通入氮气，控制氮气与氩气的总流量为130SCCM，氮气比例为40％等参数，并维持真空度在0.94Pa下进行预反应溅射。c. Close the sputtering baffle, turn on the rotating power supply of the sample stage, turn on the intermediate frequency power supply to preheat for 5 minutes, and put about 90 SCCM of argon gas into the cavity, adjust the vacuum degree to about 0.94Pa and adjust the power supply voltage to make it produce glow , and adjust the sputtering power to 400 watts to pre-sputter the aluminum target for 15 minutes, remove the impurities that may be contained on the target surface, and then pass in nitrogen, control the total flow of nitrogen and argon to 130SCCM, and the ratio of nitrogen to 40 % and other parameters, and maintain the vacuum at 0.94Pa for pre-reaction sputtering.
d.待腔体内气氛稳定后打开挡板，调节溅射功率为2000瓦进行30分钟的400℃恒温薄膜生长过程。d. After the atmosphere in the chamber is stable, open the baffle, adjust the sputtering power to 2000 watts, and perform a film growth process at a constant temperature of 400° C. for 30 minutes.
e.同时，因为TC4钛合金相对于单晶块材来说近乎于非晶材料，材料表面晶格表面能与界面能的不同，薄膜能在任何位置成核，不能像单晶块材表面一样形核受到周期性晶格的约束。因此为了提高薄膜的生长质量，我们在保证薄膜表面不开裂、粗糙度满足制作声表面波传感器要求的情况下延长生长时间至6小时。e. At the same time, because the TC4 titanium alloy is almost an amorphous material compared to the single crystal bulk material, the lattice surface energy of the material surface is different from the interface energy, and the film can nucleate at any position, which cannot be the same as the surface of the single crystal bulk material Nucleation is constrained by a periodic lattice. Therefore, in order to improve the growth quality of the film, we extended the growth time to 6 hours while ensuring that the surface of the film does not crack and the roughness meets the requirements for making a surface acoustic wave sensor.
图1展示了TC4钛合金基板的XRD测试图，显示出TC4钛合金中含有少量(002)与(101)晶向的Ti。Figure 1 shows the XRD test pattern of the TC4 titanium alloy substrate, showing that the TC4 titanium alloy contains a small amount of Ti in the (002) and (101) crystal orientations.
图2展示了400℃恒温溅射30分钟所生长氮化铝薄膜的XRD测试图，图中显示出经历30分钟恒温生长后，钛合金表面开始形成少量的(002)取向的氮化铝薄膜。Figure 2 shows the XRD test pattern of the aluminum nitride film grown by constant temperature sputtering at 400°C for 30 minutes. The figure shows that after 30 minutes of constant temperature growth, a small amount of (002)-oriented aluminum nitride film begins to form on the surface of the titanium alloy.
图3展示了400℃自降温溅射6小时后所制最终样品的XRD测试图，图中显示了我们成功在TC4钛合金基板上生长出了高(002)晶向的氮化铝薄膜，其Omega摇摆曲线半高宽Figure 3 shows the XRD test pattern of the final sample prepared after sputtering at 400°C for 6 hours. The figure shows that we have successfully grown an aluminum nitride film with a high (002) crystal orientation on the TC4 titanium alloy substrate. Omega Rocking Curve FWHM
FWHM＝4.1°，基本上达到了制作高性能薄膜型声表面波器件所需要的高(002)取向氮化铝薄膜要求。FWHM=4.1°, which basically meets the requirement of high (002) oriented aluminum nitride thin film required for making high-performance thin-film surface acoustic wave devices.
图4由SEM测试图可知，薄膜表面晶粒大小较为均匀，晶粒排列紧密。虽然晶粒形状与理想的正六边形有差距，但是薄膜表面晶粒排列致密，没有明显的空隙，这样就很适合我们自作薄膜型SAW器件。It can be seen from the SEM test picture in Fig. 4 that the grain size on the surface of the film is relatively uniform and the grains are closely arranged. Although there is a gap between the grain shape and the ideal regular hexagon, the grains on the surface of the film are densely arranged without obvious gaps, which is very suitable for our self-made thin film SAW devices.
图5由AFM测试图可知，最终样品薄膜表面的均方根粗糙度RMS＝8.943nm，达到了制作薄膜型声表面波器件小于30nm的一般要求。因此我们在现有工艺条件下在TC4钛合金基片上生长的薄膜的表面粗糙度达到了制作薄膜型SAW器件的要求。It can be seen from the AFM test chart in Fig. 5 that the root mean square roughness of the surface of the final sample film is RMS=8.943nm, which meets the general requirement of less than 30nm for the production of thin-film surface acoustic wave devices. Therefore, under the existing process conditions, the surface roughness of the film grown on the TC4 titanium alloy substrate meets the requirements for making thin film SAW devices.
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