阅读说明：本技术 一种大长径比探针的组装方法 (A kind of assemble method of big L/D ratio probe ) 是由 杨树明 程碧瑶 李少博 杨晓凯 王飞 于 2019-08-30 设计创作，主要内容包括：本发明公开了一种大长径比探针的组装方法,该探针包括原子力显微镜探针以及位于针尖的纳米结构,该探针的组装方法为：首先将原子力显微镜探针进行亲水处理,然后将亲水处理后的原子力显微镜探针放置于分散有一维纳米材料的混合溶液中进行组装,得到大长径比探针,并且通过调整一维纳米材料混合溶液的浓度,能够得到不同大长径比的探针。本发明提供的大长径比探针的组装方法,简单易行,不需要复杂昂贵的设备,节约成本。对高深宽比复杂微细结构的测量具有高精度的测量能力。本发明克服了当前使用原子力普通硅探针对高深宽比微细结构成像易产生成像假象的问题。(The invention discloses a kind of assemble methods of big L/D ratio probe, the probe includes atomic force microscope probe and the nanostructure positioned at needle point, the assemble method of the probe are as follows: atomic force microscope probe is subjected to hydrophilic treated first, then the atomic force microscope probe after hydrophilic treated is placed in the mixed solution for be dispersed with monodimension nanometer material and is assembled, obtain big L/D ratio probe, and by adjusting the concentration of monodimension nanometer material mixed solution, the probe of different big L/D ratios can be obtained.The assemble method of big L/D ratio probe provided by the invention, simple and easy, the equipment for not needing complex and expensive, save the cost.There is high-precision measurement capability to the measurement of high-aspect-ratio complexity fine structure.The problem of image artifacts are also easy to produce to suitable to fine structure with high depth-width ratio imaging the present invention overcomes currently used atomic force common silicon probe.)

1. a kind of assemble method of big L/D ratio probe, which is characterized in that the probe includes atomic force microscope probe and position In the nanostructure of needle point, the assemble method of the probe are as follows:

Atomic force microscope probe is subjected to hydrophilic treated first, then places the atomic force microscope probe after hydrophilic treated It is assembled in the mixed solution for be dispersed with monodimension nanometer material, obtains big L/D ratio probe, and by adjusting a wiener The concentration of rice material mixed solution, can obtain the probe of different big L/D ratios.

2. a kind of assemble method of big L/D ratio probe according to claim 1, which is characterized in that this method specifically includes Following implemented step:

1) hydrophilic treated of needle point

The needle point of atomic force microscope probe is eluted with ethyl alcohol or acetone first；Then hydrophilic solution is configured, by needle point It is taken out after immersing hydrophilic solution processing, needle point is enabled to adsorb monodimension nanometer material；

2) configuration of monodimension nanometer material mixed solution

It is measured respectively by 3- aminopropyl triethoxysilane and isopropanol alcoholic solution, according to volume ratio 3- aminopropyl-triethoxy silicon Alkane: isopropanol alcoholic solution=1:8-1:10 proportional arrangement mixed solution A；By monodimension nanometer material according to 0.00004- The dispersion concentration of 0.0005mg/mL is dispersed in isopropanol alcoholic solution, adds above-mentioned mixed solution A sufficiently ultrasound point It dissipates, obtains monodimension nanometer material mixed solution；

3) assembling of big L/D ratio probe

Atomic force microscope probe after hydrophilic treated in step 1) is placed in configured monodimension nanometer material in step 2) Mixed solution in, sufficient standing and precipitating, the monodimension nanometer material Spontaneous adsorption of single big L/D ratio is in atomic force microscope The assembling of probe is completed on probe tip surface.

3. a kind of assemble method of big L/D ratio probe according to claim 2, which is characterized in that in step 1), use The time that ethyl alcohol or acetone elute probe is 5-10min.

4. a kind of assemble method of big L/D ratio probe according to claim 2, which is characterized in that in step 1), configuration Hydrophilic solution according to volume ratio be ammonium hydroxide: hydrogen peroxide: deionized water=1:1:5 solution is configured, wherein ammonium hydroxide select NH₃ The ammonium hydroxide of=25wt%, hydrogen peroxide select H₂O₂The hydrogen peroxide of=30wt%；After needle point is immersed hydrophilic solution, when holding, is a length of 0.5-2h。

5. a kind of assemble method of big L/D ratio probe according to claim 2, which is characterized in that in step 2), 3- ammonia Propyl-triethoxysilicane and aqueous isopropanol are 3- aminopropyl triethoxysilane according to volume ratio: isopropanol alcoholic solution≤ The proportional arrangement of 1:10.

6. a kind of assemble method of big L/D ratio probe according to claim 2, which is characterized in that one-dimensional in step 2) Nano material includes nano wire, nanometer rods and nanotube.

7. a kind of assemble method of big L/D ratio probe according to claim 2, which is characterized in that in step 2), configuration 1-dimention nano mixed solution needs to carry out abundant ultrasonic disperse, ultrasonic time 5-10h using cell crushing instrument.

8. a kind of assemble method of big L/D ratio probe according to claim 2, which is characterized in that single big in step 3) The monodimension nanometer material of draw ratio by Spontaneous adsorption in needle surface mechanism be Brownian movement.

9. a kind of assemble method of big L/D ratio probe according to claim 2, which is characterized in that be assembled in step 3) The probe of monodimension nanometer material is sufficiently eluted for several times using isopropanol alcoholic solution, drying nitrogen drying.

Technical field

The invention belongs to micro-nano manufacture field of measuring technique, and in particular to a kind of assemble method of big L/D ratio probe.

Background technique

With being constantly progressive for modern micrometer-nanometer processing technology, various novel microcircuits, micro optical element, micromechanics etc. are to it The demand of measuring surface form is very urgent, these structures depend on high-aspect-ratio complexity fine structure extensively.For advanced wide It than the measurement of complicated fine structure, is typically necessary by direct or indirect micro- amplification, it is desirable that have higher laterally resolution Rate and longitudinal resolution.Compared with the measurement of smooth surface, to measure high-aspect-ratio complexity fine structure real topography and Position deviation is relatively difficult.

Measurement method mainly has eyes with non-contact method and contact method two major classes at present.Typical noncontact optical measurement technology has three Horn cupping and interferometry.The former is radiated in object under test plane, by anti-by scattering principle by the beam of laser that light source issues It penetrates and is finally imaged on the detector.When the position of body surface changes, phase also occurs on the detector for imaging The displacement answered.By the way that as the relational expression between shifting and actual displacement, true ohject displacement can be by the detection moved to picture and meter It obtains.But this method is suitble to measure large-sized structure, and the body surface that cannot be irradiated to for laser is unable to measure.Interference Method is that the light beam projected by light source is divided into measurement light and reference light by spectroscope, respectively directive reference planes and objective plane, Two-beam after reflection is overlapped and is interfered at spectroscope.When objective plane is mobile, the light and shade striped meeting of interference pattern Change corresponding number and its change frequency is write down by photoelectric counter, it is possible thereby to the mobile distance of objective plane is calculated, But measurement range is limited by optical wavelength, is not suitable for measurement bumps and is changed greatly complex-curved.

It is the common instrument of contact type measurement, depth measurement by the high-precision probe-type contourgraph of representative of Stylus method Precision depends on matched displacement sensor, generally there is the magnitude of 0.1nm up to 0.1-0.2mm, longitudinal resolution, laterally Resolution ratio is related with needle type radius.Since probe will contact measured surface, such measured surface unit area under a certain pressure The contact pressure of upper receiving is very big, if measured surface hardness is lower, probe often scratches measured surface, therefore this method is not The micro nano surface processed suitable for soft metals such as copper, aluminium.In addition, presently used probe is largely tungsten material or gold Made of hard rock, the draw ratio that there is no reliable process to make probe is sufficiently large, helpless to the measurement of suitable to fine structure with high depth-width ratio.

Summary of the invention

The purpose of the present invention is overcoming defect and deficiency existing in the prior art, a kind of group of big L/D ratio probe is provided Dress method, with meet suitable to fine structure with high depth-width ratio measurement it is reliable and stable, precision is high etc. requires.

The present invention adopts the following technical scheme that realize:

A kind of assemble method of big L/D ratio probe, the probe include atomic force microscope probe and receiving positioned at needle point Rice structure, the assemble method of the probe are as follows:

Atomic force microscope probe is subjected to hydrophilic treated first, then by the atomic force microscope probe after hydrophilic treated It is placed in the mixed solution for be dispersed with monodimension nanometer material and is assembled, obtain big L/D ratio probe, and by adjusting one The concentration of dimension nano material mixed solution can obtain the probe of different big L/D ratios.

A further improvement of the present invention lies in that this method specifically includes following implemented step:

1) hydrophilic treated of needle point

The needle point of atomic force microscope probe is eluted with ethyl alcohol or acetone first；Then hydrophilic solution is configured, it will Needle point takes out after immersing hydrophilic solution processing, and needle point is enabled to adsorb monodimension nanometer material；

2) configuration of monodimension nanometer material mixed solution

It is measured respectively by 3- aminopropyl triethoxysilane and isopropanol alcoholic solution, according to three ethoxy of volume ratio 3- aminopropyl Base silane: isopropanol alcoholic solution=1:8-1:10 proportional arrangement mixed solution A；By monodimension nanometer material according to 0.00004- The dispersion concentration of 0.0005mg/mL is dispersed in isopropanol alcoholic solution, adds above-mentioned mixed solution A sufficiently ultrasound point It dissipates, obtains monodimension nanometer material mixed solution；

3) assembling of big L/D ratio probe

Atomic force microscope probe after hydrophilic treated in step 1) is placed in configured 1-dimention nano in step 2) In the mixed solution of material, the monodimension nanometer material Spontaneous adsorption of sufficient standing and precipitating, single big L/D ratio is aobvious in atomic force Micro mirror probe tip surface, completes the assembling of probe.

A further improvement of the present invention lies in that in step 1), time for using ethyl alcohol or acetone to elute probe for 5-10min。

A further improvement of the present invention lies in that the hydrophilic solution of configuration is ammonium hydroxide: dioxygen according to volume ratio in step 1) Water: deionized water=1:1:5 solution is configured, and wherein ammonium hydroxide selects NH₃The ammonium hydroxide of=25wt%, hydrogen peroxide select H₂O₂= The hydrogen peroxide of 30wt%；After needle point is immersed hydrophilic solution, when holding a length of 0.5-2h.

A further improvement of the present invention lies in that in step 2), 3- aminopropyl triethoxysilane and aqueous isopropanol, according to Volume ratio is 3- aminopropyl triethoxysilane: isopropanol alcoholic solution≤1:10 proportional arrangement.

A further improvement of the present invention lies in that monodimension nanometer material includes nano wire, nanometer rods and nanometer in step 2) Pipe.

A further improvement of the present invention lies in that configuration 1-dimention nano mixed solution is needed using clasmatosis in step 2) Instrument carries out abundant ultrasonic disperse, ultrasonic time 5-10h.

A further improvement of the present invention lies in that in step 3) single big L/D ratio monodimension nanometer material by Spontaneous adsorption in The mechanism of needle surface is Brownian movement.

A further improvement of the present invention lies in that the probe for being assembled with monodimension nanometer material in step 3) is molten using isopropanol alcohol Liquid sufficiently elutes for several times, drying nitrogen drying.

The present invention has following beneficial technical effect:

The assemble method of big L/D ratio probe provided by the invention, simple and easy, the equipment for not needing complex and expensive are saved Cost.There is high-precision measurement capability to the measurement of high-aspect-ratio complexity fine structure.The present invention overcomes currently used originals The problem of sub- common silicon probe of power is also easy to produce image artifacts to suitable to fine structure with high depth-width ratio imaging.The assemble method may be implemented to criticize Amount, which is produced to have, is less than 50nm needle point radius of curvature, and draw ratio is greater than 40:1's and has excellent mechanical property, not easy to wear (average probe material is that silicon belongs to hard brittle material, and monodimension nanometer material has great tensile strength and elasticity modulus, theoretical The axial tensile-strength maximum of upper carbon nanotube is visited up to 100GPa or more, elasticity modulus up to the big L/D ratio of 1TPa or more) Needle.

Detailed description of the invention

Fig. 1 is atomic force microscope probe scanning electron microscope diagram piece used in the specific embodiment of the invention.

Fig. 2 is the fixture schematic diagram that atomic force microscope probe is clamped in the specific embodiment of the invention.

Fig. 3 is the big L/D ratio probe that carbon nanotube is assembled in the specific embodiment of the invention.

Specific embodiment

The present invention is further explained below in conjunction with drawings and examples.

A kind of method of big L/D ratio probe for the measurement of high-aspect-ratio complexity fine structure provided by the invention, the spy Needle includes the nanostructure at atomic force microscope probe and tip, the assemble method of the probe are as follows: first by atomic force microscopy Mirror probe carries out hydrophilic treated, is then placed into the mixed solution for be dispersed with monodimension nanometer material and is assembled, and adjusts one-dimensional The concentration of nano material mixed solution obtains the probe of different big L/D ratios.

Specific step is as follows:

1) hydrophilic treated of needle point

Needle point is eluted with ethyl alcohol first, the elution time is 5-10min；It is ammonium hydroxide according to volume ratio: hydrogen peroxide: goes Ionized water=1:1:5 carries out the configuration of hydrophilic solution, total volume 50-500mL.Needle point clamping is put into beaker on fixture, It takes 25-250mL hydrophilic solution to pour into beaker to close the lid, beaker is put into oil bath fireless cooker and is kept for 75-85 DEG C of heating temperature, It is taken out after constant heating 0.5-2h.

2) configuration of monodimension nanometer material mixed solution

It is measured respectively using graduated cylinder by 3- aminopropyl triethoxysilane and aqueous isopropanol, according to the ratio of 1:8-1:10 Configure the mixed solution A of 50-500mL；Monodimension nanometer material is dispersed in isopropanol solvent, dispersion concentration is 0.00004-0.0005mg/mL, adds the abundant ultrasonic disperse of above-mentioned mixed solution A, and ultrasonic time 5-10h is obtained uniform Monodimension nanometer material mixed solution.The monodimension nanometer material of probe tip assembling includes nano wire, nanometer rods and nanotube etc..

3) assembling of big L/D ratio probe

The mixed of configured monodimension nanometer material in step 2) will be placed in using the probe after ethanol rinse in step 1) It closes in solution, the monodimension nanometer material of sufficient standing and precipitating, single big L/D ratio will be by Brownian movement Spontaneous adsorption in needle Complete the assembling of probe in sharp surface；The probe for being assembled with monodimension nanometer material is needed sufficiently to be eluted using isopropanol for several times, dry It is dried with nitrogen.