CN105714257B - A kind of single magnetostriction micro-pipe preparation method - Google Patents
A kind of single magnetostriction micro-pipe preparation method Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 38
- 238000004544 sputter deposition Methods 0.000 claims abstract description 21
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 16
- 238000004090 dissolution Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000013077 target material Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 10
- 239000007787 solid Substances 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 239000011162 core material Substances 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 2
- 239000011257 shell material Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000004607 Chlorophora excelsa Nutrition 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- 241000595436 Milicia excelsa Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0005—Separation of the coating from the substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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Abstract
Description
技术领域technical field
本发明属于传感器装置技术领域，特别涉及一种单根磁致伸缩微管的制备方法。The invention belongs to the technical field of sensor devices, in particular to a method for preparing a single magnetostrictive microtube.
背景技术Background technique
微纳米磁致伸缩材料在传感器领域具有广泛的应用，可以检测各种物理参数包括：应力，压力，温度，湿度，粘度，pH值等。这是因为磁致伸缩材料具有磁致伸缩效应，所谓磁致伸缩是指磁性材料在外磁场作用下，其内部磁畴结构发生变化，从而宏观表现为尺寸伸长或缩短的一种现象。在时变磁场下，磁致伸缩材料会发生受迫振动，当其固有频率与外界磁场频率相同时会发生谐振，其谐振频率可作为传感器的检测信号。外界的干扰如：质量载荷，会影响传感器的谐振频率。因此，磁致伸缩传感器也是一种质量传感器。质量灵敏度是表征其性能的一个重要参数，其定义为：单位载荷质量所引起的谐振频率的变化。显然，对于相同载荷质量，谐振频率变化越大，传感器灵敏度越高。由磁致伸缩传感器灵敏度公式可知，其灵敏度大小与其尺寸有关，相同长度的磁致伸缩传感器，体积越小其灵敏度越高。因此，与磁致伸缩线相比，磁致伸缩管体积更小，灵敏度更高。Micro-nano magnetostrictive materials have a wide range of applications in the field of sensors, which can detect various physical parameters including: stress, pressure, temperature, humidity, viscosity, pH value, etc. This is because the magnetostrictive material has a magnetostrictive effect. The so-called magnetostriction refers to a phenomenon in which the internal magnetic domain structure of a magnetic material changes under the action of an external magnetic field, so that the size of the magnetic material is elongated or shortened macroscopically. Under the time-varying magnetic field, the magnetostrictive material will be forced to vibrate, and when its natural frequency is the same as the frequency of the external magnetic field, it will resonate, and its resonant frequency can be used as the detection signal of the sensor. External disturbances such as mass loads will affect the resonant frequency of the sensor. Therefore, the magnetostrictive sensor is also a quality sensor. Mass sensitivity is an important parameter to characterize its performance, which is defined as the change of resonance frequency caused by unit load mass. Obviously, for the same load mass, the greater the change in resonance frequency, the higher the sensitivity of the sensor. It can be seen from the sensitivity formula of the magnetostrictive sensor that its sensitivity is related to its size. For a magnetostrictive sensor of the same length, the smaller the volume, the higher the sensitivity. Therefore, magnetostrictive tubes are smaller and more sensitive than magnetostrictive wires.
磁致伸缩传感器可以是带状或棒状，通过甩带/丝法可制备出宽度5~10mm，厚度20~30µm磁致伸缩带（如: Metglas2826 MB）或者直径为10~300µm磁致伸缩丝。通过电化学沉积-模板法可以制备出尺寸更小的磁致伸缩微纳米线/管阵列，但却无法制备单根磁致伸缩微纳米线/管，限制了其在传感器领域的应用。The magnetostrictive sensor can be in the shape of a ribbon or a rod, and a magnetostrictive ribbon with a width of 5~10mm and a thickness of 20~30µm (eg: Metglas2826 MB) or a magnetostrictive wire with a diameter of 10~300µm can be prepared by the strip/wire method. Smaller magnetostrictive micronanowire/tube arrays can be prepared by electrochemical deposition-template method, but a single magnetostrictive micronanowire/tube cannot be prepared, which limits its application in the field of sensors.
发明内容Contents of the invention
为了提高传感器的灵敏度，提高磁致伸缩材料在传感器领域的广泛适用性，制备体积小、质量轻的单根磁致伸缩管，本发明提供一种单根磁致伸缩微管制备方法。In order to improve the sensitivity of sensors, improve the wide applicability of magnetostrictive materials in the field of sensors, and prepare single magnetostrictive tubes with small volume and light weight, the invention provides a method for preparing single magnetostrictive microtubes.
本发明通过以下技术方案予以实现。The present invention is achieved through the following technical solutions.
一种单根磁致伸缩微管制备方法，其特征是：由以下步骤依次进行：A method for preparing a single magnetostrictive microtube, characterized in that: the following steps are carried out sequentially:
（一）、快速溶解镁合金芯上磁控溅射磁致伸缩层(1) Rapid dissolution of the magnetron sputtering magnetostrictive layer on the magnesium alloy core
1）、将快速溶解镁合金制成5~30mm长、直径为0.1~10µm的丝；1) Making fast-dissolving magnesium alloy into wires with a length of 5-30 mm and a diameter of 0.1-10 µm;
2）、将镁合金丝放置于磁控溅射仪腔体内的基座上，采用磁控溅射法，对镁合金丝表面溅射磁致伸缩薄膜，得到镁合金丝表面溅射有厚度为1~10µm厚的磁致伸缩薄膜2) Place the magnesium alloy wire on the base in the cavity of the magnetron sputtering apparatus, and use the magnetron sputtering method to sputter a magnetostrictive film on the surface of the magnesium alloy wire to obtain a sputtered surface of the magnesium alloy wire with a thickness of 1~10µm thick magnetostrictive film
（二）、单根磁致伸缩管制备 将前步（一）制得的表面溅射有磁致伸缩层的镁合金丝放入97℃、质量分数为4%的KCl溶液中，待快速溶解镁合金丝完全溶解，得到内径为0.1~10µm，壁厚为1~10µm单根磁致伸缩管。(2) Preparation of a single magnetostrictive tube Put the magnesium alloy wire sputtered with a magnetostrictive layer on the surface prepared in the previous step (1) into a 97°C KCl solution with a mass fraction of 4%, and wait for rapid dissolution The magnesium alloy wire is completely dissolved to obtain a single magnetostrictive tube with an inner diameter of 0.1-10µm and a wall thickness of 1-10µm.
所述磁致伸缩薄膜为Fe-B磁致伸缩薄膜或者Tb-Fe磁致伸缩薄膜。The magnetostrictive film is Fe-B magnetostrictive film or Tb-Fe magnetostrictive film.
所述的磁控溅射所用靶材为磁性金属。The target material used in the magnetron sputtering is magnetic metal.
所述溅射仪腔体内初始真空度为0.08mbar。The initial vacuum degree in the chamber of the sputtering instrument is 0.08mbar.
本发明与现有技术相比具有以下有益效果。Compared with the prior art, the present invention has the following beneficial effects.
1、可以制备1~10µm壁厚、5~30mm长度的磁致伸缩管，灵敏度较同长度和同直径的实心线材高5 .7倍，能更好地满足传感器灵敏度的使用要求。1. Magnetostrictive tubes with a wall thickness of 1-10µm and a length of 5-30mm can be prepared, and the sensitivity is 5.7 times higher than that of solid wires of the same length and diameter, which can better meet the requirements of sensor sensitivity.
2、直接成形微小的单根管，避免对微小的磁致伸缩切割造成管腔堵塞。2. Directly form a tiny single tube to avoid tube lumen blockage caused by tiny magnetostrictive cutting.
3、直接成形微小的单根管，提高了磁致伸缩微管的尺寸精度。3. Directly form a tiny single tube, which improves the dimensional accuracy of the magnetostrictive microtube.
附图说明Description of drawings
图1为本发明整体结构示意图。Figure 1 is a schematic diagram of the overall structure of the present invention.
具体实施方式detailed description
实施例一Embodiment one
一种单根磁致伸缩微管制备方法，其特征是：由以下步骤依次进行：A method for preparing a single magnetostrictive microtube, characterized in that: the following steps are carried out sequentially:
一、快速溶解镁合金芯上磁控溅射磁致伸缩层1. Rapid dissolution of magnetron sputtering magnetostrictive layer on magnesium alloy core
1）、将快速溶解镁合金制成5mm长、直径为10µm的丝；所述的快速溶解镁合金主要应用于石油钻井用憋压球材料，如魏辽等人于《多级滑套可溶解憋压球材料研究》（《石油机械》2015年第43卷第11期102-106页）所述，将熔融态快速溶解镁合金通过单孔直径为10µm的筛子，镁合金丝每伸出筛子5mm，对筛子表面进行一次剪切，即获得长度为5mm、直径为10μm的快速溶解镁合金丝。1) Make a fast dissolving magnesium alloy into a wire with a length of 5 mm and a diameter of 10 μm; the fast dissolving magnesium alloy is mainly used as a pressure-suppressing ball material for oil drilling, such as Wei Liao et al. As described in "Research on Pressure Ball Materials" ("Petroleum Machinery", Vol. 43, No. 11, pp. 102-106, 2015), the rapidly dissolving magnesium alloy in the molten state is passed through a sieve with a single hole diameter of 10 µm. 5mm, the surface of the sieve is sheared once to obtain a rapidly dissolving magnesium alloy wire with a length of 5mm and a diameter of 10μm.
2）、将镁合金丝放置于磁控溅射仪腔体内的基座上，采用参考文献“ Michael L.Johnson , Odum LeVar , Sang H . Yoon , Jung-Hyun Park , Shichu Huang , Dong-Joo Kim , Zhongyang Cheng , Bryan A . Chin，Dual-cathode method for sputteringmagnetoelastic iron-boron films Vacuum，83 (2009) 958–964 .”中记载的磁控溅射法，2) Place the magnesium alloy wire on the pedestal in the magnetron sputtering chamber, using the reference "Michael L.Johnson, Odum LeVar, Sang H. Yoon, Jung-Hyun Park, Shichu Huang, Dong-Joo Kim , Zhongyang Cheng , Bryan A . Chin, Dual-cathode method for sputtering magnetoelastic iron-boron films Vacuum, 83 (2009) 958–964 .” The magnetron sputtering method recorded in,
对镁合金丝表面溅射Fe-B磁致伸缩薄膜，具体步骤如下：Sputtering Fe-B magnetostrictive film on the surface of magnesium alloy wire, the specific steps are as follows:
① 、系统溅射室共有两个靶材，分别为纯Fe（铁）靶材（纯度99 .9%）和纯B（硼）靶材（99.5%），把Fe靶材和B靶材分别固定在直流负极和射频负极；① There are two targets in the sputtering chamber of the system, which are pure Fe (iron) target (purity 99.9%) and pure B (boron) target (99.5%). The Fe target and B target are respectively Fixed on DC negative pole and RF negative pole;
② 、把镁合金丝放置在基座上，并使镁合金丝与基座垂直，基座的转速设置为20rpm（Revolutions Per minute，转/分钟），调节基座距离使镁合金丝与靶材之间距离为2cm；② Put the magnesium alloy wire on the base, and make the magnesium alloy wire perpendicular to the base, set the speed of the base to 20rpm (Revolutions Per minute, revolutions per minute), adjust the distance between the base and the magnesium alloy wire to the target The distance between them is 2cm;
③ 、启动真空泵使溅射仪腔体内背底真空度达到9.33x10-5Pa，然后在溅射仪腔体通入体积流量为30sccm（standard-state cubic centimeter per minute）氩气直到溅射仪腔体内真空度稳定在0.8Pa；③ Start the vacuum pump to make the back vacuum in the sputtering chamber reach 9.33x10 -5 Pa, and then inject argon gas with a volume flow rate of 30 sccm (standard-state cubic centimeter per minute) into the sputtering chamber until the sputtering chamber The vacuum in the body is stable at 0.8Pa;
④ 、Fe靶材和B靶材溅射功率分别为41W和100W；④ The sputtering power of Fe target and B target is 41W and 100W respectively;
⑤ 、每次溅射时间设置为2小时，每次溅射后休息20分钟，溅射次数为4次，得到镁合金丝表面溅射有厚度为5μm厚的Fe-B磁致伸缩层；⑤. Each sputtering time is set to 2 hours, rest for 20 minutes after each sputtering, and the number of sputterings is 4 times, and the surface of the magnesium alloy wire is sputtered with a thickness of 5 μm Fe-B magnetostrictive layer;
二、磁致伸缩管制备2. Preparation of magnetostrictive tube
通过研究得知，优选Mg、Al和Zn等材料或合金为核体材料，并在基体金属晶粒包覆一层与核体具有一定氧化电位差的壳体材料，使得核体和壳体材料在含有Cl－的电解质溶液中形成微电池而产生强烈的电化学反应，从而实现材料可溶解以Mg为例，其标准电极电位为-2 .37V，腐蚀电位一般在+0 .5～-1 .65V之间，腐蚀主要以单价的Mg离子与水反应生成更加稳定的二价Mg产物，并放出氢气，其溶解反应过程如式(1)和式(2)所示。总反应：Through research, it is known that materials or alloys such as Mg, Al, and Zn are preferred as the core material, and a layer of shell material with a certain oxidation potential difference from the core is coated on the matrix metal grains, so that the core and shell materials A micro-battery is formed in an electrolyte solution containing Cl- to generate a strong electrochemical reaction, so that the material can be dissolved. Taking Mg as an example, its standard electrode potential is -2.37V, and its corrosion potential is generally +0.5~-1 Between .65V, the corrosion mainly reacts with monovalent Mg ions and water to form more stable divalent Mg products, and releases hydrogen gas. The dissolution reaction process is shown in formula (1) and formula (2). Overall response:
Mg+H++H2O→ Mg2++OH-+H2↑(1)；Mg+H + +H 2 O → Mg 2+ +OH - +H 2 ↑(1);
当碱性溶液中存在氯离子时，还会进一步发生以下反应生成MgCl2，从而导致金属表面迅速发生点腐蚀，从而加快Mg金属的腐蚀：When there are chloride ions in the alkaline solution, the following reactions will further occur to generate MgCl 2 , which will lead to rapid pitting corrosion on the metal surface, thereby accelerating the corrosion of Mg metal:
Mg(OH)2+2Cl-→ MgCl2+2OH－(2)。Mg(OH) 2 +2Cl - → MgCl 2 +2OH - (2).
将前步制得的表面溅射有Fe-B磁致伸缩层的镁合金丝放入97℃、质量分数为4%的KCl溶液中，待快速溶解镁合金丝完全溶解，得到内径为10µm，壁厚为5µm单根Fe-B磁致伸缩管。Put the magnesium alloy wire sputtered with Fe-B magnetostrictive layer on the surface prepared in the previous step into the KCl solution with a mass fraction of 4% at 97°C, and wait until the fast-dissolving magnesium alloy wire is completely dissolved to obtain an inner diameter of 10 μm. A single Fe-B magnetostrictive tube with a wall thickness of 5µm.
实施例二Embodiment two
一种单根磁致伸缩微管制备方法，其特征是：由以下步骤依次进行：A method for preparing a single magnetostrictive microtube, characterized in that: the following steps are carried out sequentially:
一、快速溶解镁合金芯上磁控溅射磁致伸缩层1. Rapid dissolution of magnetron sputtering magnetostrictive layer on magnesium alloy core
1）、将快速溶解镁合金制成30mm长、直径为0.1µm的丝；1) A wire with a length of 30 mm and a diameter of 0.1 µm was made from a rapidly dissolving magnesium alloy;
2）、将镁合金丝放置于磁控溅射仪腔体内的基座上 ， 采用参考文献“ HimalayBasumatary, J. Arout Chelvane, D.V. Sridhara Rao, S.V. Kamat, Rajeev Ranjan，Effect of sputtering parameters on the structure, microstructure and magneticproperties of Tb-Fe films Thin Solid Films 583 (2015) 1–6”中记载的磁控溅射法，2) Place the magnesium alloy wire on the pedestal in the magnetron sputtering chamber, using the reference "HimalayBasumatary, J. Arout Chelvane, D.V. Sridhara Rao, S.V. Kamat, Rajeev Ranjan, Effect of sputtering parameters on the structure, The magnetron sputtering method described in microstructure and magneticproperties of Tb-Fe films Thin Solid Films 583 (2015) 1–6",
对镁合金丝表面溅射Tb-Fe磁致伸缩薄膜，具体步骤如下：Sputtering Tb-Fe magnetostrictive film on the surface of magnesium alloy wire, the specific steps are as follows:
① 、把合金靶材（50%Tb，50%Fe）固定在直流负极；①. Fix the alloy target (50%Tb, 50%Fe) on the DC negative electrode;
② 、把镁合金丝放置在基座上，并与基座垂直，基座的转速设置为20 rpm，靶材与基座间的距离为15cm；②. Place the magnesium alloy wire on the base and make it perpendicular to the base. The speed of the base is set to 20 rpm, and the distance between the target and the base is 15cm;
③ 、启动真空泵使溅射仪腔体内背景真空度达到1.33× 10-4Pa，然后在溅射仪腔体通入氩气直到腔体内真空度稳定在2Pa；③ Start the vacuum pump to make the background vacuum in the sputtering chamber reach 1.33×10-4Pa, and then inject argon into the sputtering chamber until the vacuum in the chamber is stable at 2Pa;
④ 、把溅射功率设置为150W，同时使腔体内真空度保持在2.0Pa④. Set the sputtering power to 150W and keep the vacuum in the chamber at 2.0Pa
⑤ 、每次溅射时间设置为1小时，每次溅射后休息20分钟，溅射次数为6次，得到镁合金丝表面溅射有厚度为2µm厚的Tb-Fe磁致伸缩薄膜。⑤. Each sputtering time is set to 1 hour, rest for 20 minutes after each sputtering, and the number of sputtering is 6 times to obtain a Tb-Fe magnetostrictive film with a thickness of 2 μm sputtered on the surface of the magnesium alloy wire.
二、磁致伸缩管制备2. Preparation of magnetostrictive tube
将前步制得的表面溅射有Tb-Fe磁致伸缩层的镁合金丝放入97℃、质量分数为4%的KCl溶液中，待快速溶解镁合金丝完全溶解，得到内径为0.1µm，壁厚为2µm单根Tb-Fe磁致伸缩管。Put the magnesium alloy wire sputtered with a Tb-Fe magnetostrictive layer on the surface prepared in the previous step into a KCl solution with a mass fraction of 4% at 97°C, and wait until the rapidly dissolving magnesium alloy wire is completely dissolved to obtain an inner diameter of 0.1 µm. , a single Tb-Fe magnetostrictive tube with a wall thickness of 2µm.
上面结合附图对本发明的实施例作了详细说明，但是本发明并不限于上述实施例，在本领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下作出各种变化。The embodiments of the present invention have been described in detail above in conjunction with the accompanying drawings, but the present invention is not limited to the above embodiments. Within the scope of knowledge of those of ordinary skill in the art, various modifications can be made without departing from the gist of the present invention. kind of change.
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