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CN102305256B - Metal micrometer/nanometer spring as well as preparation method and application thereof - Google Patents

Metal micrometer/nanometer spring as well as preparation method and application thereof Download PDF

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CN102305256B
CN102305256B CN 201110262186 CN201110262186A CN102305256B CN 102305256 B CN102305256 B CN 102305256B CN 201110262186 CN201110262186 CN 201110262186 CN 201110262186 A CN201110262186 A CN 201110262186A CN 102305256 B CN102305256 B CN 102305256B
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李伟明
黄高山
吴晓京
梅永丰
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Fudan University
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Abstract

本发明属于微纳器件技术领域,具体为一种金属微米/纳米弹簧及其制备方法和应用。制备方法包括:准备一个衬底,在衬底上面存在牺牲层;在牺牲层上面沉积具有内应力以及各向异性的杨氏模量的金属条;选择性地除去在金属条以及衬底之间的部分牺牲层,释放金属条,从而金属条卷曲成为金属纳米/微米弹簧。该金属纳米/微米弹簧可用于流量传感器的测量,具体是将带有金属微米/纳米弹簧的衬底固定在流体通道内部;当流体流过通道时,弹簧达到平衡状态,通过测量弹簧的伸长量来测量流体流速。

The invention belongs to the technical field of micro-nano devices, in particular to a metal micro/nano spring and its preparation method and application. The preparation method includes: preparing a substrate, and there is a sacrificial layer on the substrate; depositing a metal strip with internal stress and anisotropic Young's modulus on the sacrificial layer; selectively removing the metal strip between the metal strip and the substrate. part of the sacrificial layer, the metal strip is released, so that the metal strip curls into a metal nano/micro spring. The metal nano/micro spring can be used for the measurement of the flow sensor, specifically, the substrate with the metal micro/nano spring is fixed inside the fluid channel; when the fluid flows through the channel, the spring reaches an equilibrium state, and the elongation of the spring is measured volume to measure fluid velocity.

Description

一种金属微米/纳米弹簧及其制备方法和应用A kind of metal micro/nano spring and its preparation method and application

技术领域 technical field

本发明属于微纳器件技术领域,具体涉及一种金属微米/纳米弹簧及其制备方法和应用。 The invention belongs to the technical field of micro-nano devices, and in particular relates to a metal micro/nano spring and its preparation method and application.

背景技术 Background technique

近年来,微纳器件,比如微纳尺度的管、线以及弹簧等由于在药物输运、传感器、光学以及储氢等领域存在潜在应用前景,从而受到广泛的关注。在所有的三维微纳器件中,弹簧由于其特殊的形貌而受到更为广泛的研究。由于微米/纳米弹簧具备的独特的螺线型结构以及材料本身具备的压电性能、力学性能以及电学性能,这种微米/纳米弹簧在微纳米机电系统(N/MEMS)、药物输运以及细胞操纵等领域存在潜在应用价值。由于纳米薄膜具有高的比表面积以及可容易改性的表面,利用纳米薄膜卷曲得到的微米/纳米弹簧在生物以及化学传感器方面也具有一定的应用前景。 In recent years, micro-nano devices, such as micro-nano-scale tubes, wires, and springs, have attracted extensive attention due to their potential applications in drug delivery, sensors, optics, and hydrogen storage. Among all three-dimensional micro-nano devices, springs have been more extensively studied due to their special morphology. Due to the unique helical structure of the micro/nano spring and the piezoelectric, mechanical and electrical properties of the material itself, this micro/nano spring is widely used in micro-nano electromechanical systems (N/MEMS), drug delivery and cell There are potential applications in areas such as manipulation. Due to the high specific surface area and easily modifiable surface of nanofilms, the micro/nanosprings obtained by curling nanofilms also have certain application prospects in biological and chemical sensors.

Pu XianGao等人在2006年利用固体-气体过程成功地制备得到了具有超弹性的ZnO纳米弹簧,Cao Chuanbao等人在2007年利用气相化学沉积方法制备了具有超弹性的Si3N4微米弹簧,Li Zhang等人利用卷曲具有内应力的半导体双层膜的方法成功地制备了微米弹簧。在Li Zhang等人所采用的方法中,双层膜的内应力是由不同层之间的晶格失配造成的,卷曲的方向则是由杨氏模量决定的,而在半导体薄膜中的杨氏模量具有显著的各向异性。他们的结果表明弹簧的直径由薄膜的厚度以及晶格失配程度决定,而卷曲方向是沿着杨氏模量最小的方向。 In 2006, Pu XianGao et al. used a solid-gas process to successfully prepare a superelastic ZnO nanospring. Cao Chuanbao et al. prepared a superelastic Si 3 N 4 micron spring by vapor phase chemical deposition in 2007. Li Zhang et al. successfully prepared micro-springs by curling a semiconductor double-layer film with internal stress. In the method adopted by Li Zhang et al., the internal stress of the bilayer film is caused by the lattice mismatch between the different layers, and the direction of curling is determined by the Young's modulus, while in the semiconducting film the Young's modulus has significant anisotropy. Their results show that the diameter of the spring is determined by the thickness of the film and the degree of lattice mismatch, while the curling direction is along the direction of the smallest Young's modulus.

目前,利用卷曲纳米薄膜制备的微米/纳米弹簧一般都是半导体外延材料,比如InGaAs/GaAs双层膜以及SiGe/Si双层膜,由于受限与外延技术,目前为止还没有关于纯金属的微米/纳米弹簧制备的研究报道。而与半导体材料相比,金属材料具有更好的力学以及电学性能,因此金属微米/纳米弹簧更适于在微纳器件中的应用。 At present, micron/nanosprings prepared by curling nanofilms are generally semiconductor epitaxial materials, such as InGaAs/GaAs double-layer films and SiGe/Si double-layer films. / Research report on the preparation of nano springs. Compared with semiconductor materials, metal materials have better mechanical and electrical properties, so metal micro/nano springs are more suitable for application in micro-nano devices.

发明内容 Contents of the invention

本发明的目的在于提供一种力学和电学性能优良的金属微米/纳米弹簧及其制备方法和应用。 The object of the present invention is to provide a metal micro/nano spring with excellent mechanical and electrical properties and its preparation method and application.

本发明提供的金属微米/纳米弹簧的制备方法,包括以下几个步骤: The preparation method of the metal micro/nanospring provided by the invention comprises the following steps:

(1)准备一个衬底,在衬底上面存在牺牲层; (1) Prepare a substrate on which a sacrificial layer exists;

(2)在牺牲层上面沉积具有内应力以及各向异性的杨氏模量的金属条; (2) Depositing metal strips with internal stress and anisotropic Young's modulus on the sacrificial layer;

(3)选择性地除去在金属条和衬底之间的部分牺牲层,释放金属条,从而金属条卷曲成为金属纳米/微米弹簧。  (3) Selectively remove part of the sacrificial layer between the metal strip and the substrate to release the metal strip, so that the metal strip curls into a metal nano/micro spring. the

本发明中,步骤(2)在牺牲层上面沉积具有内应力以及各向异性的杨氏模量的金属条,包括以下两个步骤,首先利用物理或化学气相沉积法在牺牲层上沉积一层金属薄膜,然后利用光刻的方法将薄膜图形化,称为金属条。其中,物理气相沉积的方法包括溅射,热蒸发以及电子束蒸发等。 In the present invention, step (2) deposits a metal strip with internal stress and anisotropic Young's modulus on the sacrificial layer, including the following two steps, first depositing a layer on the sacrificial layer by physical or chemical vapor deposition The metal film is then patterned by photolithography, called metal strips. Among them, physical vapor deposition methods include sputtering, thermal evaporation, and electron beam evaporation.

本发明中,所述利用物理气相沉积法在牺牲层上沉积一层金属薄膜,可通过控制沉积参数,比如沉积速率、衬底温度、衬底倾斜角度以及沉积压强等,得到具有在生长方向内应力梯度差和各向异性杨氏模量的金属薄膜。 In the present invention, the physical vapor deposition method is used to deposit a layer of metal thin film on the sacrificial layer, by controlling deposition parameters, such as deposition rate, substrate temperature, substrate tilt angle and deposition pressure, etc., to obtain Stress Gradient Difference and Anisotropic Young's Modulus of Metal Thin Films.

本发明中,所述金属微米/纳米弹簧的几何参数,如直径,螺旋角以及螺间距等,根据设计要求确定。 In the present invention, the geometric parameters of the metal micro/nano spring, such as diameter, helix angle and pitch, are determined according to design requirements.

本发明中,金属微米/纳米弹簧的材料(沉积的金属簿膜)可以金、钛、铬、或铝等单一组分金属(金属簿膜),也可以是这些金属的合金(合金簿膜),也可以是这些金属的多层金属(多层金属簿膜)。 In the present invention, the material of the metal micro/nanospring (deposited metal thin film) can be a single component metal (metal thin film) such as gold, titanium, chromium, or aluminum, or an alloy of these metals (alloy thin film) , It can also be a multilayer metal (multilayer metal film) of these metals.

本发明中,所述的牺牲层可以是SiO2层。 In the present invention, the sacrificial layer may be a SiO2 layer.

本发明提供的金属微米/纳米弹簧可用于流量传感器中进行流速流量测定,具体如下: The metal micron/nanospring provided by the present invention can be used in the flow sensor to measure the flow rate and flow rate, as follows:

流量传感器包括一个流体通道,将带有金属微米/纳米弹簧的衬底固定在流体通道内部。当流体通过该通道时,弹簧受到液体流动的粘滞力以及衬底对弹簧的拉力,处于平衡状态。此时,粘滞力与衬底对弹簧的拉力数值上相等。粘滞力与流体自身的粘滞系数以及流速有关,而衬底对弹簧的拉力可以通过弹簧伸长量来表示。一般来说,对于同一种流体,其粘滞系数固定不变,弹簧的伸长量随着流体的流速的上升而增大,因此,我们可以通过测量弹簧的伸长量来测量流体的流速。而弹簧的伸长量通过光学显微镜测量获得。 The flow sensor consists of a fluid channel inside which a substrate with metallic micro/nanosprings is held. When the fluid passes through the channel, the spring is in a balanced state due to the viscous force of the fluid flow and the tension of the substrate to the spring. At this time, the viscous force is numerically equal to the tension force of the substrate on the spring. The viscous force is related to the viscosity coefficient of the fluid itself and the flow velocity, while the tension of the substrate on the spring can be expressed by the elongation of the spring. Generally speaking, for the same fluid, its viscosity coefficient is fixed, and the elongation of the spring increases with the flow rate of the fluid. Therefore, we can measure the flow rate of the fluid by measuring the elongation of the spring. The elongation of the spring is measured by optical microscopy.

附图说明 Description of drawings

图1为本发明制备金属微米/纳米弹簧的流程图。其中,(a)为Si衬底上有一层SiO2作为牺牲层;(b)表示采用电子束蒸发的方法在SiO2牺牲层上沉积一层厚度为40 nm的Au薄膜;(c)表示利用氢氟酸将SiO2牺牲层去除;(d)最后形成Au微米/纳米弹簧。 Fig. 1 is a flowchart of the preparation of metal micro/nano springs in the present invention. Among them, (a) means that there is a layer of SiO 2 on the Si substrate as a sacrificial layer; (b) means that a layer of Au film with a thickness of 40 nm is deposited on the SiO 2 sacrificial layer by electron beam evaporation; (c) means that using Hydrofluoric acid removes the SiO2 sacrificial layer; (d) finally forms Au micro/nano springs.

图2为通过倾斜衬底角度沉积薄膜,得到Au薄膜具有各向异性的杨氏模量图示。 Fig. 2 is a graph showing the anisotropic Young's modulus of the Au film obtained by depositing the film at an inclined substrate angle.

图3为采用金属微米/纳米弹簧测试流体流速的示意图。其中,(a)为流体静止时,弹簧处于初始状态,(b)为流体以一定的速度从左向右流过时,弹簧受到粘滞力作用而伸长的状态。 Fig. 3 is a schematic diagram of testing fluid flow rate using metal micro/nano springs. Among them, (a) is the initial state of the spring when the fluid is still, and (b) is the state of the spring being elongated by the viscous force when the fluid flows from left to right at a certain speed.

图中标号:1. 衬底;2. 牺牲层;3. 金属层;4. 金属微米/纳米弹簧;5. 衬底的法线方向与蒸发原子气的入射方向成的角度;6. 蒸发源;7. 衬底;8.流体通道。 Labels in the figure: 1. Substrate; 2. Sacrificial layer; 3. Metal layer; 4. Metal micro/nano spring; 5. The angle between the normal direction of the substrate and the incident direction of the evaporated atomic gas; 6. Evaporation source ; 7. Substrate; 8. Fluidic channel.

具体实施方式 Detailed ways

以下通过实例进一步对本发明进行描述。 The present invention is further described by examples below.

下面结合附图及具体实例,对发明制备金属微米/纳米弹簧作进一步说明。 In the following, the preparation of metal micro/nano springs by the invention will be further described in conjunction with the accompanying drawings and specific examples.

图1为利用本发明中的方法制备金微米/纳米弹簧的示意图。其中,(a)为Si衬底1上有一层SiO2作为牺牲层2。(b)表示,采用电子束蒸发的方法在SiO2牺牲层上沉积一层厚度为40 nm的Au金属层3。其中在沉积过程中,通过改变沉积参数,如沉积速率、衬底温度以及沉积压强等,可以制备得到具有内应力的Au薄膜;将衬底的法线方向与蒸发源6蒸发原子气的入射方向成一定角度5,如图2所示,由于倾斜衬底角度沉积薄膜存在阴影效应,通过这种方法沉积得到的Au薄膜具有各向异性的杨氏模量。然后利用光刻的方法,将Au薄膜进行图形化,得到金属条,如(c)所示。最后,利用氢氟酸将SiO2牺牲层去除,从而将Au金属条从衬底上脱离开来,形成Au金属微米/纳米弹簧4,如(d)所示。 Fig. 1 is a schematic diagram of preparing gold micro/nanosprings using the method of the present invention. Among them, (a) is a layer of SiO 2 on the Si substrate 1 as the sacrificial layer 2 . (b) shows that an Au metal layer 3 with a thickness of 40 nm was deposited on the SiO 2 sacrificial layer by electron beam evaporation. Wherein, in the deposition process, by changing the deposition parameters, such as deposition rate, substrate temperature and deposition pressure, etc., an Au film with internal stress can be prepared; At a certain angle 5 , as shown in Figure 2, due to the shadow effect of the deposited film at an inclined substrate angle, the Au film deposited by this method has anisotropic Young's modulus. Then use photolithography to pattern the Au thin film to obtain metal strips, as shown in (c). Finally, the SiO 2 sacrificial layer was removed by hydrofluoric acid, so that the Au metal strips were separated from the substrate to form Au metal micro/nano springs 4, as shown in (d).

图3为基于金属微米/纳米弹簧测试流体流速的示意图,具有金属微米/纳米弹簧的衬底7固定在流体通道8内部,其中金属微米/纳米弹簧4的一端固定在衬底7上。其中,(a)表示,当流体静止时,弹簧处于初始状态,没有受到拉伸,此时长度为l 0。(b)表示,当流体以一定的速度流过时,弹簧收到粘滞力作用而伸长,此时的长度为l。弹簧的伸长量x等于l-l 0,该数值由流体的粘滞系数以及流速决定。而采用同一种流体时,粘滞系数保持不变,因此x值仅与流速成正比。从而根据以上分析,即可以通过测量弹簧的伸长量来测量流体的流速。 3 is a schematic diagram of testing fluid flow rate based on metal micro/nano springs. The substrate 7 with metal micro/nano springs is fixed inside the fluid channel 8, and one end of the metal micro/nano springs 4 is fixed on the substrate 7. Among them, (a) means that when the fluid is still, the spring is in the initial state without being stretched, and the length at this time is l 0 . (b) means that when the fluid flows through at a certain speed, the spring receives the action of viscous force and elongates, and the length at this time is l . The elongation x of the spring is equal to l - l 0 , which is determined by the viscosity coefficient of the fluid and the flow rate. When using the same fluid, the viscosity coefficient remains unchanged, so the x value is only proportional to the flow rate. Therefore, according to the above analysis, the flow rate of the fluid can be measured by measuring the elongation of the spring.

Claims (6)

1. the preparation method of a metal micrometer/nanometer spring is characterized in that concrete steps are:
(1) prepare a substrate, have sacrifice layer on substrate;
(2) metal bar that deposition has internal stress and anisotropic Young's modulus on sacrifice layer;
(3) optionally remove partial sacrifice layer between metal bar and substrate, discharge metal bar, thus the curling metal nano/micron spring that becomes of metal bar;
Step (2) deposits the metal bar with internal stress and anisotropic Young's modulus on sacrifice layer, comprise following two steps, at first utilize physics or Low Pressure Chemical Vapor Deposition to deposit the layer of metal film on sacrifice layer, then utilize the method for photoetching with metal thin-film pattern, obtain metal bar.
2. preparation method according to claim 1, it is characterized in that the described physical vaporous deposition that utilizes deposits the layer of metal film on sacrifice layer, by controlling deposition parameter, comprise deposition rate, underlayer temperature, substrate tilting angle or deposition pressure, obtain having poor in direction of growth internal stress gradient and the metallic thin film anisotropy Young's modulus.
3. preparation method according to claim 1 and 2 is characterized in that the material of described metal is gold, titanium, chromium or aluminium one-component metal, or several alloy in these metals, or several multiple layer metal in these metals.
4. preparation method according to claim 1 and 2, is characterized in that described sacrifice layer is SiO 2Layer.
5. the metal micrometer/nanometer spring for preparing of preparation method as described in one of claim 1-4.
6. metal micrometer/nanometer spring as claimed in claim 5 is measured the application of rate of flow of fluid and flow in flow transducer.
CN 201110262186 2011-09-06 2011-09-06 Metal micrometer/nanometer spring as well as preparation method and application thereof Expired - Fee Related CN102305256B (en)

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