CN102817006A - Method for gold film modification of atomic force microscope probe by magnetron sputtering - Google Patents
Method for gold film modification of atomic force microscope probe by magnetron sputtering Download PDFInfo
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- CN102817006A CN102817006A CN2012103087084A CN201210308708A CN102817006A CN 102817006 A CN102817006 A CN 102817006A CN 2012103087084 A CN2012103087084 A CN 2012103087084A CN 201210308708 A CN201210308708 A CN 201210308708A CN 102817006 A CN102817006 A CN 102817006A
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Abstract
The invention discloses a method for gold film modification of an atomic force microscope probe by magnetron sputtering. The method consists of: by means of magnetron sputtering, depositing a Cr film and an Au film on a cleaned atomic force microscope probe (silicon or silicon nitride) in order under room temperature; and changing the thickness of the Cr film and the Au film by changing the sputtering time, thus finally obtaining the atomic force microscope probe covered with a Cr film of 3-20nm and an Au film of 30-100nm. And the probe can be used in microcosmic science and other fields. As the magnetron sputtering method has the advantages of simple equipment, film uniformity, fast deposition speed, and applicability for large area film making, etc., the method disclosed in the invention can be widely used in industrial production.
Description
Technical field
The present invention relates to the atomic force microscope probe of microcosmic scientific domain, specifically is with magnetron sputtering method atomic force microscope probe (silicon or silicon nitride) to be carried out the film modified method of gold.
Background technology
AFM is a kind of important analytical instrument of material microcosmic field tests; Can be on Nano grade the physical properties of various materials and sample be comprised that pattern and mechanical property etc. survey, be widely used in fields such as nanotechnology science, Materials science, Surface Science, semi-conductor industry, biomedical science.
The AFM Au probe is mainly used in two aspects, (1) conduction acupuncture needle, and the AFM that can be used for conducting electricity measures, and semiconductor material surface is carried out nanometer processing such as anodic oxidation; (2) Au probe of functionalization biomolecules is mainly used in AFM unit molecule power spectrometry bio-molecular interaction power (gold plating of needle surface make needle point functionalization (as using the mercaptan chemistry) easier) etc.
Current, it mainly is hot vapour deposition method (Wieland J.A., Gewirth A.A that AFM silicon or silicon nitride probe are carried out the film modified method of gold; And Leckband D.E.J.Biol.Chem.2005,280:41037 – 41046) and electron beam evaporation plating (Chen G., Ning X.; Park B.; Et al.Langmuir 2009,25:2860-2864), promptly in high vacuum not under the condition of heated probe; (simple gold-plated probe gold plate in use comes off easily to utilize thermal evaporation plated film or electron beam evaporation deposition method to plate one deck chromium and golden film successively at detecting probe surface; The Cr film can strengthen the bonding force of golden film and probe), but shortcoming such as still there is the poor adhesive force of golden film and probe in the Au probe of these methods preparation, and the roughness of golden film is big; Can produce deviation to the measuring result of AFM, therefore develop and a kind ofly effectively atomic force microscope probe is carried out the film modified method of gold be very important.
The Chinese invention patent publication number is CN102539840A, and this invention provides " a kind of magnetic microscope probe of low magnetic moment high-coercive force and method of manufacture thereof.Said method of manufacture may further comprise the steps: clean the Si probe; Si probe stationary after cleaning in the sample chamber of magnetic control sputtering device, and is vacuumized the sample chamber, after this, feed high purity inert gas, make the gaseous tension of sample chamber maintain the 0.1-0.5 handkerchief; Through the magnetron sputtering mode CoPt magneticalloy is splashed to the Si detecting probe surface, thereby obtains having the Si probe of magnetisable coating; The Si probe with magnetisable coating that obtains is heated to 500 ℃-750 ℃ under vacuum condition, thermal treatment 15-180 minute, makes magneticalloy be converted into the L10-CoPt alloy, thereby obtain the magnetic microscope probe of low magnetic moment high-coercive force." only be applied to the Si probe in this technology and shall not be applied to Si
3N
4Probe is handled, and need carry out high-temperature heat treatment for the post-processed of probe simultaneously.
Summary of the invention
The technical problem that the present invention will solve provides a kind of magnetron sputtering that utilizes atomic force microscope probe is carried out the film modified method of gold, overcomes the deficiency that prior art exists, and obtains the atomic force microscope probe that the surface is coated with golden film.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The probe that cleans up is placed in the magnetron sputtering chamber; Utilize magnetron sputtering technology at sputter chromium film and golden film successively under the pure argon atmosphere, on atomic force microscope probe (silicon or silicon nitride) under the room temperature, obtain the atomic force microscope probe that the surface is covered with 3 ~ 20nm chromium film and 30 ~ 100nm gold film.
Further, above-mentioned preparation method carries out according to the following steps:
(1) probe cleans: clean with chloroform, ultraviolet ray-ozone, chloroform successively;
(2) sputter chromium film: adopt d.c. sputtering chromium target, sputter gas is a pure argon;
(3) sputter gold film: adopt the d.c. sputtering gold target, sputter gas is a pure argon;
In said (1), chloroform cleans, and each time is 10 ~ 20min.
In said (1), ultraviolet ray-ozone clean time is 10 ~ 30min, through ultraviolet ray-ozone the impurity such as organism that substrate surface retains is carried out exhaustive oxidation, thereby plays the effect that the degree of depth is cleaned.
In said (2) and (3), the distance of regulating substrate and target is 10～20cm, prevent since substrate and target distance too closely cause from sputter, the while again can not be too far away, thus the assurance quality of forming film.
In said (2) and (3), the magnetron sputtering chamber is vacuumized, make its vacuum tightness less than 1.0 * 10
-4Pa.
In said (2), the chromium target adopts d.c. sputtering, and wherein sputtering power is 100W, and sputtering time is 10～70s.
In said (3), gold target adopts d.c. sputtering, and sputtering power is 70W, and sputtering time is 150～500s.
In said (2) and (3), the purity of pure argon is more than 99.99%, and gas pressure intensity is 0.8～1.6Pa.
In said (2) and (3), atomic force microscope probe does not heat.
Magnetron sputtering method has that equipment is simple, film forming is even, sedimentation velocity is fast, can be used for making in enormous quantities advantages such as film.Compare with evaporation coating; Substrate is cleaned in plasma zone all the time and activates in the magnetron sputtering film process of the present invention, has removed the not strong sputtered atom of sticking power, purifies and activate substrate surface; Strengthened the sticking power of sputtered atom and substrate, thereby the sticking power of sputter coating and substrate is higher.During film, the sputtered atom energy is higher than evaporation atom energy in preparation, and the substrate temperature of sputter is higher, and atom is bigger in the mobility of substrate surface, through atomic rearrangement, can obtain surface-stable, film that roughness is little.CN102539840A compares with Chinese invention patent, and film does not need thermal treatment, thereby has guaranteed the stability of membrane structure and composition, more helps the raising of the stable and repeatability of film performance.
Description of drawings
Fig. 1 is covered with the atomic force microscope probe synoptic diagram of Cr film and Au film for surface among the present invention.Wherein, 1 is AFM silicon or silicon nitride probe, and 2 is the Cr film, and 3 is the Au film.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment is that prerequisite is implemented with technical scheme of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
Atomic force microscope probe is cleaned 10 ~ 20min, ultraviolet ray-ozone clean 10 ~ 30min, chloroform cleaning 10 ~ 20mi with chloroform successively, place magnetron sputtering indoor.Be that (gas pressure intensity is 0.8～1.6Pa), and the maintenance probe temperature is a room temperature, carries out the sputter of Cr and Au film successively, and promptly magnetron sputtering chamber vacuum tightness is less than 1.0 * 10 under the situation of pure argon at film forming gas
-4Pa, the Cr target adopts d.c. sputtering, and sputtering power is 100W, and sputtering time is 10s, processes the Cr film that thickness is about 3nm; The Au target adopts d.c. sputtering, and sputtering power is 70W, and sputtering time is 150s, processes the Au film that thickness is about 30nm, and the total thickness of film is about 33nm, and wherein the thickness of film calculates according to the speed of growth of film.With AFM the roughness of film is measured afterwards.
Embodiment 2:
Atomic force microscope probe is cleaned with chloroform, ultraviolet ray-ozone, chloroform successively, place magnetron sputtering indoor.At film forming gas is under the situation of pure argon, and the maintenance probe temperature is a room temperature, carries out the sputter of Cr and Au film successively, and promptly the Cr target adopts d.c. sputtering, and sputtering power is 100W, and sputtering time is 20s, processes the Cr film that thickness is about 6nm; The Au target adopts d.c. sputtering, and sputtering power is 70W, and sputtering time is 200s, processes the Au film that thickness is about 40nm, and the total thickness of film is about 46nm, and wherein the thickness of film calculates according to the speed of growth of film.With AFM the roughness of film is measured afterwards.
Embodiment 3:
Atomic force microscope probe is cleaned with chloroform, ultraviolet ray-ozone, chloroform successively, place magnetron sputtering indoor.At film forming gas is under the situation of pure argon, and the maintenance probe temperature is a room temperature, carries out the sputter of Cr and Au film successively, and promptly the Cr target adopts d.c. sputtering, and sputtering power is 100W, and sputtering time is 35s, processes the Cr film that thickness is about 10nm; The Au target adopts d.c. sputtering, and sputtering power is 70W, and sputtering time is 300s, processes the Au film that thickness is about 60nm, and the total thickness of film is about 70nm, and wherein the thickness of film calculates according to the speed of growth of film.With AFM the roughness of film is measured afterwards.
Embodiment 4:
Atomic force microscope probe is cleaned with chloroform, ultraviolet ray-ozone, chloroform successively, place magnetron sputtering indoor.At film forming gas is under the situation of pure argon, and the maintenance probe temperature is a room temperature, carries out the sputter of Cr and Au film successively, and promptly the Cr target adopts d.c. sputtering, and sputtering power is 100W, and sputtering time is 50s, processes the Cr film that thickness is about 15nm; The Au target adopts d.c. sputtering, and sputtering power is 70W, and sputtering time is 350s, processes the Au film that thickness is about 70nm, and the total thickness of film is about 85nm, and wherein the thickness of film calculates according to the speed of growth of film.With AFM the roughness of film is measured afterwards.
Embodiment 5:
Atomic force microscope probe is cleaned with chloroform, ultraviolet ray-ozone, chloroform successively, place magnetron sputtering indoor.At film forming gas is under the situation of pure argon, and the maintenance probe temperature is a room temperature, carries out the sputter of Cr and Au film successively, and promptly the Cr target adopts d.c. sputtering, and sputtering power is 100W, and sputtering time is 70s, processes the Cr film that thickness is about 20nm; The Au target adopts d.c. sputtering, and sputtering power is 70W, and sputtering time is 450s, processes the Au film that thickness is about 90nm, and the total thickness of film is about 110nm, and wherein the thickness of film calculates according to the speed of growth of film.With AFM the roughness of film is measured afterwards.
More than the detecting probe surface structure that obtains of each embodiment as shown in Figure 1, deposit certain thickness Cr film 2 and Au film 3 on the probe 1 successively, each thicknesses of layers and roughness are as shown in table 1 below.
The thickness of each embodiment middle probe surface C r film of table 1 and Au film
| The embodiment numbering | ?1 | 2 | 3 | 4 | 5 |
| Cr film thickness/ |
3 | 6 | 10 | 15 | 20 |
| Au film thickness/nm | 30 | 40 | 60 | 70 | 90 |
| Roughness RMS/nm | 1.6 | 2.0 | 1.4 | 2.2 | 2.6 |
It is film modified that the present invention utilizes magnetron sputtering that atomic force microscope probe is carried out gold; On the probe that cleans up, deposit Cr film and Au film under the room temperature successively; Through changing the thickness that sputtering time changes Cr film and Au film; Finally can obtain the atomic force microscope probe that the surface is covered with 3～20nm Cr film and 30～100nm Au film successively; The AFM that can be used for conducting electricity measures and semiconductor material surface is carried out nanometer processing such as anodic oxidation, and field such as AFM unit molecule power spectrometry bio-molecular interaction power.Equipment is simple because magnetron sputtering method has, low price, film forming evenly, can be used for advantage such as big area system film, this preparation method can be used widely in suitability for industrialized production.
Although content of the present invention has been done detailed introduction through above-mentioned preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (9)
1. one kind is utilized magnetron sputtering that atomic force microscope probe is carried out the film modified method of gold; It is characterized in that: the probe that cleans up is placed in the magnetron sputtering chamber; Utilize magnetron sputtering technology sputter chromium film and golden film successively under pure argon atmosphere under the room temperature; Obtain the atomic force microscope probe that the surface is covered with 3 ~ 20nm chromium film and 30 ~ 100nm gold film, said atomic force microscope probe is silicon probe or silicon nitride probe.
2. method according to claim 1 is characterized in that, this method is carried out according to the following steps:
(1) probe cleans: clean with chloroform, ultraviolet ray-ozone, chloroform successively;
(2) sputter chromium film: adopt d.c. sputtering chromium target, sputter gas is a pure argon;
(3) sputter gold film: adopt the d.c. sputtering gold target, sputter gas is a pure argon.
3. method according to claim 2 is characterized in that, in said (1), the chloroform scavenging period is 10 ~ 20min, and ultraviolet ray-ozone clean time is 10 ~ 30min.
4. method according to claim 2 is characterized in that, in said (2), the base vacuum degree is less than 1.0 * 10
-4Pa, the distance of regulating substrate and target is 10～20cm, selects 99.99% the pure chromium target sputtering target as the Cr thin film deposition for use.
5. method according to claim 2 is characterized in that, in said (3), the base vacuum degree is less than 1.0 * 10
-4Pa, the distance of regulating substrate and target is 10～20cm, selects 99.99% the proof gold target sputtering target as the Au thin film deposition for use.
6. according to each described method of claim 2-5, it is characterized in that in said (2), adopt d.c. sputtering chromium target, wherein sputtering power is 100W, sputtering time is 10～70s.
7. according to each described method of claim 2-5, it is characterized in that in said (3), adopt the d.c. sputtering gold target, sputtering power is 70W, sputtering time is 150～500s.
8. method according to claim 1 and 2 is characterized in that, in said (2) and (3), the purity of pure argon is more than 99.99%, and gas pressure intensity is 0.8～1.6Pa.
9. method according to claim 1 and 2 is characterized in that, in said (2) and (3), atomic force microscope probe does not heat.
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Cited By (5)
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| CN104880579A (en) * | 2015-06-02 | 2015-09-02 | 常州朗道科学仪器有限公司 | Method and device for preparing ultrahigh-vacuum spin-polarized scanning tunneling microscope probe |
| CN106442432A (en) * | 2016-09-13 | 2017-02-22 | 中国科学院理化技术研究所 | Super-localization photoelectric current scanning imaging system based on aperture type conducting probe |
| CN106610439A (en) * | 2015-10-23 | 2017-05-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | An inclined silicon pinpoint and a manufacturing method thereof |
| CN110724920A (en) * | 2018-07-17 | 2020-01-24 | 航天科工惯性技术有限公司 | Preparation method of Au thin film |
| CN111089988A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | High-uniformity magnetic probe and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104880579A (en) * | 2015-06-02 | 2015-09-02 | 常州朗道科学仪器有限公司 | Method and device for preparing ultrahigh-vacuum spin-polarized scanning tunneling microscope probe |
| CN106610439A (en) * | 2015-10-23 | 2017-05-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | An inclined silicon pinpoint and a manufacturing method thereof |
| CN106610439B (en) * | 2015-10-23 | 2019-04-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tilting silicon needle point and preparation method thereof |
| CN106442432A (en) * | 2016-09-13 | 2017-02-22 | 中国科学院理化技术研究所 | Super-localization photoelectric current scanning imaging system based on aperture type conducting probe |
| CN110724920A (en) * | 2018-07-17 | 2020-01-24 | 航天科工惯性技术有限公司 | Preparation method of Au thin film |
| CN110724920B (en) * | 2018-07-17 | 2021-11-12 | 航天科工惯性技术有限公司 | Preparation method of Au thin film |
| CN111089988A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | High-uniformity magnetic probe and preparation method thereof |
| CN111089988B (en) * | 2019-12-27 | 2023-01-31 | 季华实验室 | High-uniformity magnetic probe and preparation method thereof |
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| CN102817006B (en) | 2014-04-16 |
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