CN102175894A - Method for preparing miniature thermocouple probe of scanning thermal microscopy - Google Patents
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- CN102175894A CN102175894A CN 201010606034 CN201010606034A CN102175894A CN 102175894 A CN102175894 A CN 102175894A CN 201010606034 CN201010606034 CN 201010606034 CN 201010606034 A CN201010606034 A CN 201010606034A CN 102175894 A CN102175894 A CN 102175894A
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Abstract
The invention discloses a method for preparing a miniature thermocouple probe of a scanning thermal microscopy, which belongs to the technical fields of nano machining, nanoscale performance measurement and electronic science. The method for preparing the miniature thermocouple probe of the scanning thermal microscopy comprises the following steps of: a) manufacturing a first metal layer on the front of a cantilever pinpoint of an atomic force microscopy; b) manufacturing an insulating layer on the first metal layer; c) removing the insulating layer in a set area on the tip of the pinpoint; and d) manufacturing a second metal layer on the insulating layer, wherein the second metal layer is in contact with the first metal layer in the set area, and is made from a material different from that of the first metal layer. The method can be used for the technical fields of nano machining, nanoscale performance measurement and the like.
Description
Technical field
The present invention relates to nano-sensor and nano measurement instrument, relate in particular to a kind of method of on commercial AFM cantilever tip, making the nanoscale thermal sensor, belong to nanoprocessing, nanoscale performance measurement and electronic science and technology field.
Background technology
Up to now, the existing low-dimensional materials of many characteristic dimensions below 100 nanometers are manufactured to come out, as carbon nano-tube, various metal or semi-conductive nano wire, Graphene etc.Simultaneously, along with the continuous improvement of large scale integrated circuit manufacture craft, the characteristic dimension of traditional devices has also narrowed down to the magnitude of tens nanometers.Electronics, phonon transmission and the energy dissipation of studying these nano materials and nano-device are significant and very challenging problems, and heat distribution and the dissipation problem of for example studying large scale integrated circuit have very actual purposes.Traditional method is difficult to the sensing point of hygrosensor is accomplished below 1 micron.
Scanning thermal microscope SThM (scanning thermal microscopy) provides the strong instrument of a research submicron-scale heat dissipation.SThM is based on atomic force microscope (AFM:atomic forcemicroscopy) technology.That has reported has two kinds of methods, and the one, utilize on the AFM cantilever micro thermocouple of special processing to realize temperature survey, another kind is an integrated thermal resistance on needle point.Because the AFM technology can clearly be seen the sample surfaces of nano-scale clearly, so theoretically, SThM can survey temperature on the nanoscale and heat conducting.
There are two kinds of methods to can be used to prepare thermocouple type SThM needle point at present.
A kind of is to utilize MEMS (micro electro mechanical system) (MEMS) technology, in the process of preparation in quantity AFM cantilever tip, also prepare most advanced and sophisticated miniature nanometer thermoelectric idol structure [Y.X.Zhang, Y.W.Zhang, J.Blaser, T.S.Sriram, A.Enver and R.B.Marcus, Review of Scientific Instruments 69 (5), 2081 (1998); L.Shi, O.Kwon, A.C.Miner, and A. Majumdar, Journal ofMicroelectromechanical Systems 10 (3), 370 (2001); G.Mills, H.Zhou, A.Midha, L.Donaldson, and J.M.R.Weaver, Appl.Phys.Lett.72 (22), 2900 (1998)].These class methods are all used a series of semiconductor technologies such as chemical vapor deposition, electron beam exposure, vacuum evaporation in preparation process, complex process needs and improves complete semiconductor manufacturing equipment, and preparation cost is very high; But these class methods are fit to large-scale production.
Second kind of method for preparing thermocouple type SThM needle point is to produce micro thermocouple [K.Luo by some procedure of processings at the needle point tip on existing commercialization afm tip, Z.Shi, J.Varesi, and A.Majumdar, J.Vac.Sci.Technol.B 15 (2), and 349 (1997)].The advantage of this method is more flexible, can do some special constructions.But the concrete grammar of only one piece of bibliographical information has also been employed semiconductor technologies such as reactive ion etching, does not still break away from process complexity and the disadvantage that needs expensive instrument.
Summary of the invention
The objective of the invention is to overcome problems of the prior art, propose a kind of simple method, can on the AFM cantilever tip, make micro thermocouple by this method and make it to become the SThM needle point.The inventive method is simple to operate, lower to the hardware device requirement, and the end of probe of thermopair can be made in the front of needle point, thereby has higher sensitivity.The SThM needle point of producing with this method can be on the yardstick of tens nanometers the heat distribution of exosyndrome material.
The inventive method is on the basis of the AFM cantilever tip (as Fig. 1) that can conveniently buy on the market, utilize simple procedure of processing, on needle point, plate the metal level of the different materials of two-layer mutual insulating, and make double layer of metal only connect (remainder insulation) formation micro thermocouple at the place, tip of afm tip.This micro thermocouple is connected the temperature and the thermal measurement that can carry out nanoscale with the measurement of correlation circuit.
Specifically, the inventive method may further comprise the steps:
A) make the first metal layer in the front of AFM cantilever tip (one side that needle point is promptly arranged);
B) on described the first metal layer, make insulation course;
C) remove the insulation course of setting regions on the needle point tip;
D) make second metal level on described insulation course, described second metal level contacts with described the first metal layer in described setting regions, and the material of described second metal level and described the first metal layer is formed different.Cover owing to all be insulated layer the described setting regions of the first metal layer on the needle point tip, so the first metal layer only contacts in described setting regions with second metal level, thereby constituted thermopair.
Described AFM cantilever tip can be common silicon nitride contact afm tip, also can be the AFM cantilever tip (it is conductive material that other needle point has the part main body, needs in advance insulation course to be done on the type afm tip surface and handles) of other form and material.
Preferably, described method also comprises: at described step a) and b) between, one or more lead-in wire on described the first metal layer, made.The design of reserving extension line on the first metal layer step that can simplify the operation, extension line can adopt and reserve 2 or more Redundancy Design simultaneously, improves yield rate.Because the first metal layer substantially all is insulated layer parcel, the method for the extraction electrode contact point that other is commonly used is difficult for the first metal layer is connected with external circuit.In addition, the also easily better original cantilever seat of more adaptive commercial apparatuss of this design just can be realized drawing and measurement function of 2 leads of thermopair through the simple cantilever mount pad of transforming.
Preferably, described method also comprises: after described step d), go up to make the 3rd metal level at the back side of described AFM cantilever tip (one side that does not promptly have needle point), the stress of the cantilever that the technology that described the 3rd metal level can the balance front causes, and can improve reflectivity.Described the 3rd metal is preferably gold.
Preferably, described step a) can be implemented by following method: shown in accompanying drawing 2b, place first baffle plate on the front of described AFM cantilever tip, described first baffle plate covers the selected part in described front; By vacuum coater plated film on the unmasked portion in described front, form described the first metal layer with setting shape and thickness.
Because the first metal layer of the inventive method can be done greatlyyer, therefore baffle plate (comprising herein first plate washer and following second baffle) can be finished by simply making by hand, for example can simply shear flake aluminum and make (being not limited to this method certainly), simplify the condition of processing, made things convenient for the processing and fabricating of needle point.
Described coating process can adopt various vacuum coaters, for example thermal evaporation plated film instrument, the mechanical, electrical sub-beam evaporation plated film instrument of sputter coating etc.
Preferably, described step b) can be implemented by following method: make insulation course by Atomic layer deposition method on described the first metal layer.In fact, the way of growth insulation course can be used a lot of ways, the reason of the preferred Atomic layer deposition method of the present invention is: the insulation course of Atomic layer deposition method deposition to the parcel of needle point very evenly and can cover the surface of all exposures, be not subjected to the influence of AFM cantilever tip surface undulation, may cause the inhomogeneous leaky that produces of film thickness because of surface undulation unlike other film plating process, this is very meaningful for the violent sample of the most advanced and sophisticated this fluctuations of afm tip; In addition, Atomic layer deposition method can accurately be controlled the thickness of deposited film.
Preferably, described step c) can be implemented by following several different methods, such as realize electrostatic breakdown with narishige in the scanning electron microscope of nano-controller (SEM) is housed; Punch with focused ion beam (FIB) technology; The mode of utilization making alive and mating surface friction between AFM cantilever tip and sample removes insulation course.
Described first method can be implemented by following method: the operation nano-controller is with the tip of tungsten tip (or other conductive pinpoint) near described AFM cantilever tip in the visual field of scanning electron microscope, between described tungsten tip and described AFM cantilever tip, apply voltage, with the insulation course puncture at described most advanced and sophisticated place.
Described second method can be implemented by following method: adopt the part of the described insulation course at the described most advanced and sophisticated place of focused-ion-beam lithography, etching depth is greater than the thickness of described insulation course and less than the thickness sum of described insulation course and described the first metal layer.
Described the third method can be implemented by following method: apply voltage between described AFM cantilever tip and a conducting sample, make the mantle friction of the tip of AFM cantilever tip at described conducting sample simultaneously, until the described insulation course of removing on the described tip.Owing to added voltage, the electric current when insulation course is removed between needle point and conducting sample can change, and insulation course on the tip is removed and the first metal layer is retained with this may command.
Preferably, described step d) can be implemented by following method: shown in accompanying drawing 2h, place second baffle on described insulation course, described second baffle covers the selected part of described insulation course; By vacuum coater plated film on the unmasked portion of described surface of insulating layer, form described second metal level with setting shape and thickness.
In the methods of the invention, described first metal and second metal (the first metal layer and second metal level in other words) can be selected from various metals, unique requirement is that two kinds of thermoelectricity capability diversity ratios between the metal are more remarkable, the Seebeck coefficient difference that is them is bigger, surpass preset threshold, thereby the thermopair that these two kinds of metals are constituted can obtain big as far as possible pyroelectric signal.A lot of materials such as titanium, palladium, gold, silver, aluminium can be as metal level.
In the methods of the invention, described insulation course can be selected from various insulating material.The inventive method has 2 points to the requirement of insulation course, and the one, insulating property will be got well, and really insulate in discontiguous place to guarantee two metal levels; The 2nd, can remove with methods such as electric breakdown or etchings, so that can open insulation course at the most advanced and sophisticated place of needle point.Preferably, the material of described insulation course is selected from hafnia, aluminium oxide or zirconia.
With the thermopair needle point that the inventive method is made, can characterize the heat distribution state of the material of tens nanoscales.Key property of the present invention is convenience and the simplification that needle point is made.After thermocouple signal extracted and write down, through and existing data analysis contrast, just can obtain the Temperature Distribution on the nanoscale of the sample that will measure.In addition, simple procedure of processing of the present invention is equally applicable to the thermocouple sensor of integration of compactization on other existing micro devices, is used to study the thermal effect of local.Has technology simply with to the interdependent low advantage of equipment than the way that on silicon chip, prepares thermopair with semiconductor technologies such as traditional photoetching, plated films.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) figure of commercialization AFM cantilever tip, and wherein Fig. 1 is the top view of this cantilever tip a), has 4 semi-girders on the cantilever, and respectively there is a needle point at the place, tip of each semi-girder, and (tip portion that shows among the figure is represented semi-girder.Needle point of the present invention is positioned at the place, tip of semi-girder.The yardstick of needle point is less, does not show in this figure); Fig. 1 b) is the side view of cantilever tip one end under certain viewing angle, can sees 2 semi-girders (yardstick of needle point is less, does not show) in this figure; Fig. 1 c) be Fig. 1 b) enlarged drawing of circular portion, shown the details of needle point on semi-girder;
Fig. 2 is a schematic flow sheet of making thermopair according to the inventive method, expresses for simplifying, and only shows 1 in 4 needle points among the figure; Wherein, 1-AFM cantilever tip; The 2-the first metal layer; The 3-insulation course; 4-second metal level; The 10-semi-girder; 11-cantilever main body; The 12-needle point; 13-needle point tip; 15-first baffle plate; The 16-second baffle; The 21-lead-in wire;
Fig. 3 is the schematic side view according to the cantilever tip top of the flow process of the inventive method making thermopair; Each layer is needle point from top to bottom successively among Fig. 3 f, the first metal layer, the insulation course and second metal level;
Fig. 4 is the scanning electron microscope diagram that utilizes (4a) back (4b) before the voltage breakdown insulation course in the SEM of nano-controller is housed;
Fig. 5 is to use the scanning electron microscope diagram after the FIB mode is removed insulation course;
Fig. 6 is the photo in kind that is assemblied in the scanning calorimeter needle point on a kind of afm tip cantilever seat.
Embodiment
In conjunction with the accompanying drawings the present invention is further described below by specific embodiment, but does not limit the present invention in any way.
Present embodiment utilizes commercial AFM contact mode silicon nitride needle point, selects titanium and palladium 2 kinds of metal layer material as thermopair, makes the micro thermocouple probe that is applicable to that VEECO D-3100 type AFM instrument cantilever mount pad uses, and concrete steps are as follows.
(a) the AFM cantilever tip of selecting conveniently to have bought on the market (model DNP-20, VEECO, USA) (Fig. 1), and prepare micro thermocouple on the tip of a V-shape cantilever tip therein.Fig. 2 is a schematic flow sheet of making thermopair, expresses for simplifying, and actual 4 needle points are only drawn one (shown in Fig. 2 a).In step a and c, the metal of employing has been selected Titanium and the palladium metal as step a and c evaporation through selecting relatively and testing and determine.The starting point of selecting these two kinds of metals is that the thermoelectricity capability diversity ratio between them is more remarkable, the gap of Seebeck coefficient that shows as them is bigger, be respectively 9.1 (μ V/K) and-10.0 (μ V/K), such two kinds of Metal Contact can obtain very big pyroelectric signal.Because titanium is oxidized easily, so in evaporation, with the metal of titanium as the ground floor evaporation; insulation course and second layer metal that it will be plated subsequently protect; with this system film combination, can effectively prevent the destruction of oxidation to thermopair, keep the long-term effectiveness of thermopair.
Shown in Fig. 2 b, needle point 1 and first baffle plate, the 15 usefulness conducting resinls of tailoring with flake aluminum are sticked on the substrate back simply just can put into the plated film instrument and carry out evaporation, on the nitride silicon based end, plate the titanium of 60 nanometers earlier.In the coating process, baffle plate 15 serves as mask plate.After plated film finishes,, form the first metal layer 2, i.e. a titanium electrode on overhanging beam 10 and the needle point 12 in cantilever main body 11.After this step process finished, the side at needle point 12 places was shown in Fig. 3 b.Because the yardstick of cantilever main body 11 is several millimeters magnitude, so flake aluminum (first plate washer 15) can directly be determined the shape of wanting by hand.
(b) utilize the method for spot welding on the first metal layer 2, to burn-on a lead, the results are shown in Figure 2b as contact conductor 21 (, can draw 2 or more with as redundant) in order to insure.
(c) for isolated two kinds of thermo-electric metal materials, with grow in the afm tip substrate hafnia of tens nanometers of Atomic layer deposition method, this layer hafnia will be as two kinds of intermetallic separation layers.The AFM cantilever tip of abovementioned steps being made of conducting resinl is fixed on the substrate (material is not limit) earlier, then the AFM cantilever tip on substrate and its is put into the sample chamber of ald instrument, after vacuumizing, the hafnia of about 40 nanometer thickness of growth is a presoma with water and Tetrakis (Dimethylamido) Hafnium in 90-250 ℃ temperature range.After this flow process finished, needle surface was all covered by the uniform insulation course 3 of a layer thickness, the results are shown in synoptic diagram 2c, and the side of needle point 12 is shown in Fig. 3 c at this moment.
(d) one of committed step of the present invention is exactly with simple way the partial insulative layer on the needle point tip 13 3 to be removed, shown in Fig. 2 d.
The method that can adopt has multiple, as in the SEM of nano-controller is housed, using the method for electrostatic breakdown, perhaps use FIB, perhaps the mode that making alive and mating surface rub on AFM cantilever tip-sample removes the part of insulation course, hafnium oxide layer is got an aperture, expose Titanium, the side schematic view of needle point 12 such as Fig. 3 e.
Method with electrostatic breakdown in SEM is specially: earlier needle point is put in the SEM sample chamber that nano-controller is housed, be evacuated down to the specified vacuum degree, open electron beam and carry out scanning electron microscopic observation, find behind the needle point with nano-controller tungsten tip mounted thereto tip, between tungsten tip and AFM cantilever tip titanium coating, add suitable voltage the insulation course at tip is punctured (Fig. 3 d) near afm tip.Be determined by experiment, be added in when voltage on tungsten tip and the AFM cantilever tip titanium coating surpasses a threshold value (35V-40V) and puncture and can take place, the diameter of breakdown area is in hundred nanometer scale.The size of breakdown area is little with an alive magnitude relationship, and is not the just generation of alive moment punch-through sometimes.Tungsten tip not necessarily will contact with the afm tip tip, under the very near situation of distance, punctures and also can take place, and Fig. 4 is the SEM photo before and after puncturing.
Utilize FIB to prepare the most advanced and sophisticated method that goes up aperture specifically: earlier needle point to be put into the FIB sample chamber, be evacuated down to and open electron beam behind the setting or ion beam finds needle point and defines etched area, adopt focused ion beam that the needle point tip is etched away a part, the thickness that etches away is thicker slightly than insulation course, but do not penetrate the ground floor metal, remove the effect that insulation course keeps metal level again to reach.Can etch the aperture of diameter tens nanometers even tens nanometers and the regular shape in hole with FIB; Shortcoming is to the equipment requirements height.Fig. 5 be with FIB at the needle point tip photo after insulation course punching.
The third method of removing the most advanced and sophisticated place of AFM cantilever tip insulation course is to utilize commercial AFM system.Make the AFM system works in conduction AFM (C-AFM) pattern, between needle point and conducting sample, add voltage and apply suitable power, allow needle point on the conducting sample surface, scan among a small circle, simultaneously real-time monitoring current with contact mode.Under the acting in conjunction of mantle friction and voltage, the insulation course at the most advanced and sophisticated place of needle point can be removed.The conduction afm tip (the inboard evaporation of needle point has metal) that tens nano oxidized hafnium layers are arranged for a surface coverage, if conducting sample uses high directed cracking graphite (HOPG), the voltage that adds about 10-20 volt between needle point and sample scans among a small circle and keeps the some time (tens seconds to several minutes scopes) just can realize that the tip locates the removal of insulation course with contact mode.Monitoring shows that saltus step can take place the electric current of flowing through between needle point and the sample, shows that the insulation course at most advanced and sophisticated place is removed.The hole of Xing Chenging can observed with SEM afterwards in this way.
What above-mentioned way had can obtain meticulousr hole, and the nano-controller that does not need scanning electron microscope and complexity that has respectively has superiority, and has shown that from a side the inventive method has wide in range applicability.
(e) on insulation course 3, plate the Metal Palladium of 60 nanometers another electrode as thermopair.At first preparing what a flake aluminum baffle plate 16 (can make of simple manual method, also used baffle plate 15 in the available step (a) equally.Barrier material also can be other material.)。Shown in Fig. 2 e, place baffle plate 16 and evaporation metal.Front schematic view such as Fig. 2 f after this step finishes, Fig. 3 f is the side schematic view of needle point 12.
(f) in order to solve the crooked and normal problem of using of reflectivity decline influence of afm tip stress that a series of process may cause, plate the gold of tens nanometer thickness at the back side of AFM cantilever tip 1.This step also can use a simple baffle plate to block the needle point back side in coating process does not need gold-plated part.
Installation situation and the contact conductor of AFM cantilever thermopair needle point on the cantilever seat of finally making seen Fig. 6.Thermocouple signal one end is drawn by the lead of reserving, and an other end is drawn by the conduction making leaf spring on the cantilever tip pedestal.The physical dimension and the position of this conduction making leaf spring considered in design during baffle plate in the aforementioned preparation thermopair needle point process, and the position of baffle plate placement also is according to the position of the conduction making leaf spring on the pedestal and definite when reserving the position of lead and plated film.The position of the design of baffle plate and placement location and reservation lead can be readjusted according to the design size of different types of AFM cantilever tip pedestal, and this also shows that from a side the inventive method has wide in range applicability.
Claims (10)
1. the preparation method of a scanning thermal microscope micro thermocouple probe comprises:
A) make the first metal layer in the front of AFM cantilever tip;
B) on described the first metal layer, make insulation course;
C) remove the insulation course of setting regions on the tip of needle point;
D) make second metal level on described insulation course, described second metal level contacts with described the first metal layer in described setting regions, and the material of described second metal level and described the first metal layer is formed different.
2. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1 is characterized in that, described method also comprises: at described step a) and b) between, one or more lead-in wire on described the first metal layer, made.
3. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1, it is characterized in that, described method also comprises: after described step d), on the back side of described AFM cantilever tip, make the 3rd metal level, the stress of the described cantilever of described the 3rd metal level balance, and improve reflectivity.
4. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1, it is characterized in that, described step a) is implemented by following method: place first baffle plate in the front of described AFM cantilever tip, described first baffle plate covers the selected part in described front; By vacuum coater plated film on the unmasked portion in described front, form described the first metal layer with setting shape and thickness.
5. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1 is characterized in that, described step b) is implemented by following method: make insulation course by Atomic layer deposition method on described the first metal layer.
6. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1 is characterized in that, described step c) is implemented by following method: utilize narishige to puncture by the insulation course of electric breakdown mode with described most advanced and sophisticated place in scanning electron microscope.
7. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1, it is characterized in that, described step c) is implemented by following method: adopt the part of the described insulation course at the described most advanced and sophisticated place of focused-ion-beam lithography, etching depth is greater than the thickness of described insulation course and less than the thickness sum of described insulation course and described the first metal layer.
8. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1, it is characterized in that, described step c) is implemented by following method: apply voltage between a described AFM cantilever tip and a conducting sample, make of the mantle friction of the tip of AFM cantilever tip simultaneously, until the partial insulative layer of removing on the described tip at described conducting sample.
9. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1, it is characterized in that, described step d) is implemented by following method: place second baffle on described insulation course, described second baffle covers the selected part of described insulation course; By vacuum coater plated film on the unmasked portion of described surface of insulating layer, form described second metal level with setting shape and thickness.
10. the preparation method of scanning thermal microscope micro thermocouple probe as claimed in claim 1 is characterized in that, the Seebeck coefficient difference of described first metal and second metal surpasses setting threshold.
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| CN104764905A (en) * | 2015-03-24 | 2015-07-08 | 清华大学深圳研究生院 | Atomic force microscope scanning thermal probe and preparation method thereof |
| CN105510639A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Probe for scanning probe microscope, preparation method of the probe, and detection method of the probe |
| CN105510638A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Probe for scanning probe microscope, preparation method of the probe, and detection method of the probe |
| CN107656097A (en) * | 2017-10-31 | 2018-02-02 | 中国石油大学(华东) | A kind of sample preparation methods for being easy to AFM testing coating growth kinetics models |
| CN110146726A (en) * | 2019-05-22 | 2019-08-20 | 季华实验室 | Method for controlling probe temperature |
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| CN105510638A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Probe for scanning probe microscope, preparation method of the probe, and detection method of the probe |
| CN105510638B (en) * | 2014-09-24 | 2018-10-19 | 中国科学院宁波材料技术与工程研究所 | Probe, preparation method and detection method in a kind of scanning probe microscopy |
| CN105510639B (en) * | 2014-09-24 | 2018-10-19 | 中国科学院宁波材料技术与工程研究所 | Probe, preparation method and detection method in a kind of scanning probe microscopy |
| CN104764905A (en) * | 2015-03-24 | 2015-07-08 | 清华大学深圳研究生院 | Atomic force microscope scanning thermal probe and preparation method thereof |
| CN104764905B (en) * | 2015-03-24 | 2018-04-20 | 清华大学深圳研究生院 | A kind of afm scan thermal probe and preparation method thereof |
| CN107656097A (en) * | 2017-10-31 | 2018-02-02 | 中国石油大学(华东) | A kind of sample preparation methods for being easy to AFM testing coating growth kinetics models |
| CN107656097B (en) * | 2017-10-31 | 2023-09-22 | 中国石油大学(华东) | Sample preparation method for testing coating growth dynamics model by using AFM (atomic force microscope) |
| CN110146726A (en) * | 2019-05-22 | 2019-08-20 | 季华实验室 | Method for controlling probe temperature |
| 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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