CN112986324A - Analysis method of atomic force microscope combined with ultra-fast scanning calorimeter - Google Patents
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/08—Means for establishing or regulating a desired environmental condition within a sample chamber
- G01Q30/10—Thermal environment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/18—Means for protecting or isolating the interior of a sample chamber from external environmental conditions or influences, e.g. vibrations or electromagnetic fields
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
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Abstract
The invention discloses an analysis method of an atomic force microscope combined with an ultrafast scanning calorimeter, which comprises the following steps: (1) a sample is arranged on a sample sensor, and the sample sensor is fixed above an atomic force microscope scanner, so that the scanning of the atomic force microscope is not influenced; (2) connecting a circuit, adjusting the position of a probe of the sample sensor, selecting a sample area needing to be scanned, opening a temperature control device, adjusting to a specified temperature, and introducing dry nitrogen; (3) and starting an FSC experiment after the ambient temperature is stable, and performing structural scanning on the sample by using an AFM after the heat treatment is finished, thereby realizing the tracking and characterization of the nucleation and crystallization process of the sample. The analysis method enables in-situ FSC-AFM characterization to be possible, sample structures in different states can be obtained through ultra-fast temperature rise and fall scanning and isothermal heat treatment of the FSC, the formation and growth processes of single spherulites can be tracked and characterized, and the method has important theoretical research and experimental application values.
Description
Technical Field
The invention belongs to the material analysis technology, and particularly relates to an analysis method of an atomic force microscope combined ultra-fast scanning calorimeter.
Background
With the development of the ultra-high-speed heating and cooling heat treatment technology, the FSC becomes one of the indispensable technologies in the material field. Up to 107The temperature rise and fall rate of K/s can more accurately research the dynamic processes of rapid crystallization kinetics, crystallization recombination, melting, glass transition and the like of various materials (including metal alloys, macromolecules, biological medicines and the like) and obtain important nucleation and crystal growth kinetic data. However, calorimetric data do not provide the most intuitive structural characterization analysis in theoretical research of crystal nucleation and growth, and need to be combined with other structural characterization techniques, such as optical microscopy (including POM, SEM, TEM) and spectral characterization (including infrared and X-ray), to obtain more structural information.
The AFM can provide three-dimensional surface images, high-resolution representation of molecular single chains can be achieved in the structural research of high polymer materials, the sample is simple to prepare, the sample does not need to be subjected to any special treatment (such as copper plating or carbon), the damage to the sample is extremely low, and the AFM is one of the best techniques for analyzing the crystal structure and researching the crystal growth dynamics. The ultra-fast scanning calorimetry technology and the AFM are combined, so that the bottleneck of the prior art can be broken, the technical advantages of the ultra-fast scanning calorimetry technology and the AFM are integrated, and the tip technology of more efficient and more accurate crystal growth dynamics and crystal morphology characterization is developed.
At present, no analysis system and method combining an atomic force microscope with an ultra-fast scanning calorimeter are available in the market.
Disclosure of Invention
The purpose of the invention is as follows: in view of the above prior art, the present application provides an analysis method combining an atomic force microscope and an ultrafast scanning calorimeter.
The technical scheme is as follows: the analysis method of the atomic force microscope combined ultra-fast scanning calorimeter comprises the following steps:
(1) a sample is arranged on a sample sensor, and the sample sensor is fixed above an atomic force microscope scanner, so that the scanning of the atomic force microscope is not influenced;
(2) connecting a circuit, adjusting the position of a probe of the sample sensor, selecting a sample area needing to be scanned, opening a temperature control device, adjusting to a specified temperature, and introducing dry nitrogen;
(3) and starting an FSC experiment after the ambient temperature is stable, and performing structural scanning on the sample by using an AFM after the heat treatment is finished, thereby realizing the tracking and characterization of the nucleation and crystallization process of the sample.
In the step (3), selecting isothermal temperature Tc to perform isothermal crystallization in the temperature interval of glass transition temperature Tg and melting point Tm, then cooling to below Tg at high speed, and performing AFM structural scanning; and then raising the temperature to Tc at a high speed for isothermal, lowering the temperature for AFM scanning, repeating a series of experiments to track the structure transformation process of the sample in Tc isothermal crystallization, and realizing the tracking characterization of the sample nucleation and crystallization process.
Further, the high-speed temperature reduction and high-speed temperature rise rate is 10K/s-1000,000K/s.
In the step (2), the specified temperature is above 260K.
In the step (1), the sample sensor is XI393 and XI394 series with TO5 as a support.
In the step (1), the atomic force microscope is provided with an open sample bin, and a piezoelectric ceramic tube is used as a scanner.
The application also discloses an analysis system of the atomic force microscope and ultrafast scanning calorimeter adopted by the analysis method, which comprises an atomic force microscope, a sample sensor, a reference sensor, an FSC electronic element and a computer control end, wherein the sample sensor is arranged above the piezoelectric scanner of the atomic force microscope and is connected with the FSC electronic element, the FSC electronic element is also connected with the reference sensor, and the atomic force microscope and the FSC electronic element are respectively connected to the computer control end; the device also comprises an environment control device for adjusting the environment of the atomic force microscope.
The atomic force microscope described above has an open sample chamber, and a piezoelectric ceramic tube is used as a scanner. The examples used are Level AFM from Anfatec, Germany. The sample sensor is the XI393, XI394 series with TO5 as support.
The sample sensor is fixed above the piezoelectric scanner of the atomic force microscope through a sample sensor support, the sample sensor support is a cylindrical groove and is sleeved on the piezoelectric scanner, and the sensor is arranged in the groove and is fixed; the sensor uses a TO5 copper substrate, and bendable copper pins are distributed at the bottom and are connected with an FSC circuit through the pins. Further, the pins may be connected to the FSC lines using pin circuit connectors.
Preferably, the sensor and the sample sensor support are fixed through screws or fixed by bonding.
Preferably, the device further comprises an environment control module for adjusting the environment of the atomic force microscope. The environment control module is composed of an insulation isolation box, a temperature control device and a fan.
The insulating isolation box comprises 3 layers, wherein the innermost layer is an aluminum foil, the middle layer is acrylic glass, and the outermost layer is a polystyrene insulating foam board. Preferably, the middle layer is 5mm thick acrylic glass, and the outermost layer is a 30mm thick polystyrene insulating foam sheet. In use, the insulating isolation box covers the AFM and other temperature control devices, and the electronic component part of the FSC is disposed outside the insulating box.
The temperature control device and the fan are arranged in the insulating isolation box, the temperature control device comprises a cold finger and a thermometer, the cold finger is connected with a mechanical refrigeration pump (taking FT 100, Jumbo as an example) to carry out constant temperature control on the inside of the insulating isolation box, and the constant temperature (which can be as high as about 260K at the lowest) can be kept in the insulating isolation box; the thermometer is close to AFM equipment and connected with a numerical control thermometer outside the box; the fan is used for blowing dry nitrogen, keeps the inside of the insulation box dry, and is beneficial to signal scanning of the FSC.
Because the sensor is arranged in an open environment, in order to reduce the influence of the change of air flow and environment temperature on the FSC signal, an insulating isolation box is additionally arranged around AFM equipment, and a temperature control device and a fan are arranged in the box, so that the temperature range which can be scanned when the FSC and AFM are used together can be further widened, and more sample structure information can be obtained.
The FSC comprises an SRS amplifier and an NI data acquisition board.
All circuit connections in this application all avoid contact probe cantilever and scanner, and the connecting wire is fixed after gathering, and all AFM functions all are the same before the antithetical couplet is used. Parts which are not recorded in the application can be of conventional models in the market, and the connection relation can also be set universally.
Has the advantages that: the analysis method of the atomic force microscope combined ultra-fast scanning calorimeter can simultaneously carry out FSC and AFM scanning experiments on nano-micron samples, so that in-situ FSC-AFM characterization becomes possible, sample structures (nucleation or crystallization) in different states can be obtained through ultra-fast temperature rise and fall scanning and isothermal heat treatment of the FSC, AFM real-time scanning is carried out at the same sample position, tracking characterization of sample nucleation and crystallization processes can be realized, the formation and growth processes of single spherulites can be tracked and characterized, the nucleation process of the sample can be further intuitively researched, and the method has important theoretical research and experimental application values.
Drawings
FIG. 1 is a schematic diagram of a sensor configuration;
FIG. 2 is a schematic view of the connection of the sensor mount and the piezoelectric scanner;
FIG. 3 is a top view and a cross-sectional view of FIG. 2;
FIG. 4 is a schematic diagram of an apparatus incorporating an atomic force microscope and an ultrafast scanning calorimeter;
FIG. 5 is a schematic diagram of the atomic force microscope coupled with the analysis system of the ultrafast scanning calorimeter;
FIG. 6 is a design drawing of an FSC-AFM experiment;
FIG. 7 is a scan of the PEEK sample by AFM after 0.01s,0.1s,1s,2s,4s and 10s isothermal at 564K.
Detailed Description
The present application will be described in detail with reference to specific examples.
Example 1
The device integrating the atomic force microscope and the ultrafast scanning calorimeter comprises an Atomic Force Microscope (AFM) (Level AFM of Anfatec company, germany), an FSC electronic component, a sample sensor and a reference sensor, wherein the sample sensor is a series of 393 and XI394 using TO5 as a support, the structure of the sample sensor is shown in fig. 1, the sample sensor comprises a TO5 copper substrate 4, a chip 6 and a bendable copper pin 5, the sample sensor is fixed above an atomic force microscope piezoelectric scanner through a sample sensor support, the structure of the sample sensor support 1 is shown in fig. 2, the sample sensor support is a cylindrical groove which is sleeved on the piezoelectric scanner 3, and the sample sensor is arranged in the groove and fixed through a screw 2. The breakable copper pins 5 of the sample sensor are connected with an FSC electronic component by using a pin type circuit connector, the FSC electronic component is also connected with a reference sensor, and the FSC electronic component is the prior art and can be an SRS amplifier and an NI data acquisition board.
As shown in fig. 4, the apparatus integrating the AFM and the ultrafast scanning calorimeter further includes an insulating isolation box for environmental control of the AFM, the insulating isolation box covers the AFM and the temperature control device, and the electronic component of the FSC is disposed outside the insulating box; the composite insulation board comprises 3 layers, wherein the innermost layer is an aluminum foil, the middle layer is acrylic glass with the thickness of 5mm, and the outermost layer is a polystyrene insulation foam board with the thickness of 30 mm. The insulating isolation box is also internally provided with a temperature control device and a fan, the temperature control device comprises a cold finger and a thermometer, the cold finger is connected with a mechanical refrigeration pump (taking FT 100, Jumbo as an example) to carry out constant temperature control on the inside of the insulating isolation box, and the constant temperature (which can be as high as about 260K at the lowest) can be kept in the insulating isolation box; the thermometer is close to AFM equipment and is connected with a numerical control thermometer outside the box; the fan is used to blow dry nitrogen gas to keep the inside of the insulation box dry, and simultaneously, the signal scanning of the FSC is facilitated.
The sample support of the atomic force microscope is replaced by a special sensor support, the sample is placed on a sensor (XI393, XI394 series, TO5 copper substrate) and placed in the special sensor support, the sensor is fixed by using a side screw, four metal pins of the sensor are placed outside the support and connected with an electric wire by using a pin type circuit connector, and the reference sensor is also connected with the electric wire by using the pin type circuit connector and fixed together with the electric wire. And a connecting wire is connected with electronic elements (SRS amplifier and NI data acquisition board) of the ultra-fast scanning calorimeter from a circuit outlet of the isolation box, and the FSC and AFM experiments are simultaneously controlled by a computer control terminal.
The specific experiment operation using the device is that the signal connecting end (four pins of signal output of a heater and a thermocouple) of a sensor (TO5 substrate) provided with a sample is bent, the other pins are inserted into a special sample support, the sensor and an AFM scanner are fixed by screwing screws on the side surface of the support, the bent pins of the sensor are inserted by using a contact pin type connecting wire, meanwhile, the reference sensor is connected, the reference sensor and a connecting wire are fixed, and the disturbance of the circuit TO AFM scanning is reduced. Cover the insulating isolation box, start the fan and drum into dry gas (nitrogen gas or argon gas), start temperature control device, set up invariable experimental temperature in the isolation box (can set up any temperature more than 260K), connect sensor connecting line into FSC electronic component, carry out FSC and AFM experimental design at the computer control end, need not to remove the sample.
Example 2
The analysis system of the atomic force microscope combined ultra-fast scanning calorimeter shown in fig. 5 comprises an atomic force microscope, a sample sensor, a reference sensor, an FSC electronic component and a computer control end, wherein the sample sensor is arranged above an atomic force microscope scanner and is connected with the FSC electronic component, the FSC electronic component is also connected with the reference sensor, and the atomic force microscope and the FSC electronic component are respectively connected to the computer control end. The device also comprises a temperature control device which is arranged outside the atomic force microscope and used for controlling the environment. Wherein the atomic force microscope is a Level AFM of Antatec, Germany. The sample sensors were in series XI393, XI394 with TO5 as support. The FSC comprises an SRS amplifier and an NI data acquisition board.
The method for analyzing by adopting the system comprises the following steps:
taking a PEEK sample as an example, the sample was mounted on an XI39395 sensor (TO5 copper base), placed on an AFM sample holder, and fixed with holder side screws TO fix the position of the sensor TO the AFM scanner, so that AFM scanning was not affected. Connecting a circuit, adjusting the position of a probe, selecting a sample scanning area through a microscope image in AFM experimental software, covering an AFM component by an insulating box, opening a temperature control device, keeping the temperature in the insulating box at 300K, introducing dry nitrogen, starting an FSC experiment after the ambient temperature is stable, as shown in figure 6, selecting isothermal temperature Tc to perform isothermal crystallization in a temperature interval of glass transition temperature Tg and melting point Tm, cooling to below Tg at a high speed (for example, 100,000K/s), performing AFM structural scanning, scanning to Tc at a high speed to perform isothermal scanning, cooling to perform AFM scanning, and repeating a series of experiments to track the structural transition process of the sample in Tc isothermal crystallization so as to realize the tracking and characterization of the nucleation and crystallization process of the sample. FIG. 7 is a schematic diagram of AFM scanning after isothermal crystallization in 0.01s (a), 0.1s (b), 1s (c), 2s (d), 4s (e) and 10s (f), and it can be seen from the diagram that when the isothermal time is short (FIG. 7a-b), the surface of the sample is in an unordered glass state, and when the isothermal time is gradually increased, the surface of the sample is nucleated and gradually grows to generate spherulites (FIG. 7c), and then the spherulites gradually increase in size until the surface of the sample is fully paved (FIG. 7 d-f). The example proves that the FSC-AFM combination further improves the theoretical research capability of researching the crystal growth mechanism, can track and characterize the formation and growth process of single spherulite, can even further intuitively research the nucleation process of a sample, and has important theoretical research and experimental application values.
Claims (6)
1. An analysis method of an atomic force microscope combined with an ultrafast scanning calorimeter is characterized by comprising the following steps:
(1) a sample is arranged on a sample sensor, and the sample sensor is fixed above an atomic force microscope scanner, so that the scanning of the atomic force microscope is not influenced;
(2) connecting a circuit, adjusting the position of a probe of the sample sensor, selecting a sample area needing to be scanned, opening a temperature control device, adjusting to a specified temperature, and introducing dry nitrogen;
(3) and starting an FSC experiment after the ambient temperature is stable, and performing structural scanning on the sample by using an AFM after the heat treatment is finished, thereby realizing the tracking and characterization of the nucleation and crystallization process of the sample.
2. The analysis method of the atomic force microscope combined with the ultrafast scanning calorimeter as claimed in claim 1, wherein in the step (3), in the temperature interval of the glass transition temperature Tg and the melting point Tm, isothermal temperature Tc is selected for isothermal crystallization, and then the temperature is reduced to below Tg at high speed for AFM structural scanning; and then raising the temperature to Tc at a high speed for isothermal, lowering the temperature for AFM scanning, repeating a series of experiments to track the structure transformation process of the sample in Tc isothermal crystallization, and realizing the tracking characterization of the sample nucleation and crystallization process.
3. The method of claim 2, wherein the high temperature decrease and the high temperature increase are at a rate of 10K/s to 1000,000K/s.
4. The method for analyzing by combining an atomic force microscope and an ultrafast scanning calorimeter as set forth in claim 1, wherein the specified temperature is 260K or more in step (2).
5. The method for analyzing an AFM combined with an ultrafast scanning calorimeter as claimed in claim 1, wherein, in the step (1), the sample sensor is XI393 and XI394 series using TO5 as a support.
6. The method for analyzing by combining an atomic force microscope and an ultrafast scanning calorimeter as claimed in claim 1, wherein, in the step (1), the atomic force microscope has an open sample chamber, and a piezoelectric ceramic tube is used as the scanner.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1589398A (en) * | 2001-11-19 | 2005-03-02 | 财团法人理工学振兴会 | Method for thermal analysis and system for thermal analysis |
| CN109142406A (en) * | 2018-09-07 | 2019-01-04 | 上海大学 | A kind of metal phase change research device |
| CN110715956A (en) * | 2019-11-20 | 2020-01-21 | 南京大学射阳高新技术研究院 | Laser heating single-sensor rapid scanning calorimeter |
| CN110823943A (en) * | 2019-11-20 | 2020-02-21 | 南京大学射阳高新技术研究院 | Modular structure ultra-fast scanning calorimeter |
| CN211652636U (en) * | 2019-11-20 | 2020-10-09 | 南京大学射阳高新技术研究院 | Ultra-thin sensor support of ultra-fast scanning calorimeter |
| CN111766264A (en) * | 2020-05-29 | 2020-10-13 | 中国科学院上海硅酸盐研究所 | Device for in-situ characterization of nanoscale thermal conductivity by controlling excitation through thermal wave hopping for atomic force microscope |
-
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- 2021-03-05 CN CN202110244360.6A patent/CN112986324A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1589398A (en) * | 2001-11-19 | 2005-03-02 | 财团法人理工学振兴会 | Method for thermal analysis and system for thermal analysis |
| CN109142406A (en) * | 2018-09-07 | 2019-01-04 | 上海大学 | A kind of metal phase change research device |
| CN110715956A (en) * | 2019-11-20 | 2020-01-21 | 南京大学射阳高新技术研究院 | Laser heating single-sensor rapid scanning calorimeter |
| CN110823943A (en) * | 2019-11-20 | 2020-02-21 | 南京大学射阳高新技术研究院 | Modular structure ultra-fast scanning calorimeter |
| CN211652636U (en) * | 2019-11-20 | 2020-10-09 | 南京大学射阳高新技术研究院 | Ultra-thin sensor support of ultra-fast scanning calorimeter |
| CN111766264A (en) * | 2020-05-29 | 2020-10-13 | 中国科学院上海硅酸盐研究所 | Device for in-situ characterization of nanoscale thermal conductivity by controlling excitation through thermal wave hopping for atomic force microscope |
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Application publication date: 20210618 |