CN110182755B - Low temperature device for nanometer pressing-in instrument - Google Patents
Low temperature device for nanometer pressing-in instrument Download PDFInfo
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- CN110182755B CN110182755B CN201910414288.XA CN201910414288A CN110182755B CN 110182755 B CN110182755 B CN 110182755B CN 201910414288 A CN201910414288 A CN 201910414288A CN 110182755 B CN110182755 B CN 110182755B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/0046—Surface micromachining, i.e. structuring layers on the substrate using stamping, e.g. imprinting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0075—Strain-stress relations or elastic constants
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0222—Temperature
- G01N2203/0228—Low temperature; Cooling means
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Abstract
The invention discloses a low-temperature device for a nanometer indentation instrument, and belongs to the field of nanometer mechanical testing. The device comprises a sample table (3) and a base (1), wherein a sample (12) is arranged at the end part of the left side of the sample table, an embedded rubber ring (4) is arranged on the inner wall of the right side of an outer protection cover (5), the inner side of the rubber ring (4) is arranged on the outer side of the sample table (3), and a columnar hole is arranged at the lower side of the outer protection cover (5) and is used as an inert gas inlet (13); a rubber ring (4) is arranged inside the right side of the inner protection cover (9), a heating blanket (7) is arranged on the outer wall of the inner protection cover (9), a sealing plate (10) is arranged on the left side of the outer protection cover (5), and a pressure head inlet (11) is arranged in the middle of the sealing plate and at the end part of the left side of the inner protection cover; the upper sides of the outer layer protective cover (5) and the inner layer protective cover (9) are provided with column-shaped holes for installing and sealing the visual cameras (8). The device can simultaneously meet the requirements of a nano indenter loaded transversely or longitudinally, expands the nano mechanical test range and has important application value.
Description
Technical Field
The invention relates to the field of nano mechanical testing, in particular to a low-temperature device applied to a nano indenter and a using method thereof.
Background
With the rapid development of science and technology, more and more advanced precision systems are applied to the low temperature field. The change of the working environment generally causes the change of the material performance and reliability, so it is of great practical significance to explore the change of the mechanical performance of the material in the low-temperature service environment.
The instrumented nanoimprint technology is widely applied as a means for mainly obtaining mechanical performance parameters of materials. The technology measures related parameters such as hardness, elastic modulus and the like by recording the load and the depth of continuous pressing through an instrument, has high measurement precision and wide test range, and does not damage materials.
But the technology is still lacked in the field of low-temperature environment testing. In the field of low-temperature environment, the testing temperature of the international most advanced low-temperature nanoindenter is-100 ℃, and the requirement of the low-temperature application field, such as the storage temperature of liquid and gas, can not be met. And in a low-temperature environment, water vapor in the environment can be condensed and frozen on a low-temperature surface, so that the measured performance is ice performance. The water vapor needs to be removed by regulation in the experiment.
Therefore, a novel low-temperature nano indentation test platform is developed and constructed, the mechanical properties of the material under the nano-micro scale are accurately evaluated, and the method has extremely important scientific significance and engineering value on the research, design and development of advanced surface composite films, functional nano materials and micro-electromechanical products.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a low-temperature device for a nanometer indentation instrument. The device adopts a throttling micro refrigerator, and the low-temperature environment can reach-150 ℃. The accessible changes and lets in gas, satisfies humidity environment and atmosphere environment's test demand, and work efficiency is high, convenient to use.
The technical scheme is as follows: the invention relates to a low-temperature device for a nanometer indentation instrument, which is realized by the following technical scheme.
The device comprises a sample table and a base, wherein a cylindrical hole is formed in the center of the right part of the sample table, a throttling micro refrigerator is arranged in the cylindrical hole, the cylindrical hole is connected with an external exhaust port, a high-pressure atmosphere inlet and a switch valve, and the right end of the sample table is connected with the solid base; a sample is arranged at the left end of the sample table, and a columnar hole is formed beside the sample to facilitate installation of a humidity sensor; an embedded rubber ring is arranged on the inner wall of the right side of the outer-layer protective cover, the inner side of the rubber ring is arranged on the outer side of the sample table, and a columnar hole is arranged on the lower side of the outer-layer protective cover and serves as an inert gas inlet; a rubber ring is arranged inside the right side of the inner layer protective cover, a heating blanket is arranged on the outer wall of the inner layer protective cover, a columnar hole is arranged at the top of the left side of the inner layer protective cover and serves as a pressure head inlet, and a columnar hole is arranged on the lower wall of the inner layer protective cover and communicated with the inert gas inlet; a sealing plate is arranged on the left side of the outer layer protective cover, and a pressure head inlet is arranged in the middle of the sealing plate; the upper sides of the outer layer protective cover and the inner layer protective cover are provided with column-shaped holes for installing and sealing the visual cameras.
The throttling micro refrigerator adopts the Joule-Thomson effect of isenthalpic expansion to rapidly refrigerate.
The humidity sensor is embedded in the sample table.
The heating blanket is wrapped outside the inner protective cover, and water vapor in the device is removed in a mode of heating by the heating blanket and introducing inert gas flow through the inert gas inlet.
The sample platform adopts outer safety cover, inlayer safety cover and closing plate to guarantee the leakproofness of device.
The sealing plate is a sealing plate structure with a multilayer design, and through holes in the sealing plates are different in size and shape in the sealing plates with the multilayer design.
The through holes in the sealing plates are circular or oval, the axes of the oval through holes are overlapped, and the long axes of the oval through holes are not overlapped.
Has the advantages that: the invention provides a low-temperature device for a nanometer indentation instrument, which has the advantages that compared with the prior art:
1. the device adopts a throttling micro refrigerator, and the low-temperature environment can reach-150 ℃.
2. According to the device, the humidity sensor is installed in the sample table by adopting an embedded method, so that the space utilization rate is improved.
3. The device adopts an internal and external protection method to ensure the sealing property of the device and remove water vapor in the device.
4. The device can meet the test requirements of a humidity environment and an atmosphere environment by changing the introduced gas, and has high working efficiency and convenient use.
Drawings
FIG. 1 is a schematic diagram of the internal structure of a low-temperature apparatus for a nanoindenter in an embodiment of the present invention;
FIG. 2 is a schematic overall view of the external shape of a low-temperature apparatus for a nanoimprinting apparatus according to an embodiment of the present invention;
FIG. 3 is an exploded view of a sealing plate of a cryodevice for a nanoindenter in an embodiment of the present invention;
labeled as: the device comprises a base 1, a throttling micro refrigerator 2, a sample table 3, a rubber ring 4, an outer protective cover 5, a humidity sensor 6, a heating blanket 7, a visual camera 8, an inner protective cover 9, a sealing plate 10, a pressure head inlet 11, a sample 12, an inert gas inlet 13, a throttling micro refrigerator exhaust port 14, a switch valve 15 and a high-pressure atmosphere inlet 16.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments and drawings, but the present invention is not limited to the specific embodiments.
The low-temperature device for the nanometer indentation instrument in the embodiment has the composition structure shown in figure 1, and comprises a sample table 3 and a base 1, wherein a cylindrical hole is formed in the center of the bottom of the right side of the sample table, a throttling micro refrigerator 2 is arranged in the cylindrical hole and is connected with an external throttling micro refrigerator exhaust port 14, a high-pressure atmosphere inlet 16 and a switch valve 15, the bottom of the sample table is connected with a fixing device of the solid base 1, a sample 12 is arranged at the top of the left side of the sample table, a humidity sensor 6 is convenient to mount due to the fact that the cylindrical hole is formed in the side edge of the sample table, an embedded rubber ring 4 is arranged on the inner wall of the bottom of the right side of an outer protection cover 5, the embedded rubber ring 4 is convenient to mount on the sample table 3, the cylindrical holes are formed in the upper and lower sides of the cylindrical hole and serve as an inert gas inlet 13, the rubber ring 4 is also arranged at the bottom of the right side of the inner protection cover 9, a heating blanket 7 is arranged on the outer layer of the side wall, the cylindrical holes are formed in the upper and the top of the upper and lower sides and the left side walls, and the top of the left side walls, the pressure head inlet 11 and the inert gas inlet 13 are convenient to flow in the inert gas, outer safety cover left side sets up closing plate 10, sets up pressure head entry 11 in the closing plate middle part, sets up sealed visual camera 8 through the upside column hole of inside and outside safety cover. The through holes in each sealing plate are circular or oval, the axes of the oval through holes are overlapped, and the major axes of the oval through holes are not overlapped.
The working principle of the embodiment is as follows: the experimental apparatus was sequentially installed in the low temperature environment according to the above-described embodiment with reference to fig. 1. When the test device starts to work, pressure gas, usually nitrogen or hydrogen, is introduced into a high-pressure atmosphere inlet 16, a switch valve 15 and a throttling micro refrigerator exhaust port 14 are opened, the throttling micro refrigerator 2 starts to work, the inlet 11 of the pressure head of the nano indenter is observed to be in pre-contact with the surface of a sample through a visual camera 8, then inert gas is continuously and slowly introduced into an inert gas inlet 13, a heating blanket 7 is opened to start heating, water vapor on the surface of the material starts to be removed, a humidity sensor 6 is observed, and when the required humidity range is reached, the pressure head formally contacts the surface of the material to start an experiment. When the throttled micro refrigerator 2 is closed, the humidity environment requirement can be met by observing the humidity sensor by changing the incoming gas flow, e.g. the humidity gas flow, to the inert gas inlet 13.
Claims (7)
1. A low temperature device for a nanometer indentation instrument is characterized in that: the device comprises a sample table (3) and a base (1), wherein a cylindrical hole is formed in the center of the right part of the sample table (3), a throttling micro refrigerator (2) is arranged in the cylindrical hole, the cylindrical hole is connected with an external exhaust port (14), a high-pressure atmosphere inlet (16) and a switch valve (15), and the right end of the sample table is connected with the solid base (1); a sample (12) is arranged at the left end of the sample table, and a columnar hole is formed beside the sample (12) to facilitate installation of a humidity sensor (6); an embedded rubber ring (4) is arranged on the inner wall of the right side of the outer-layer protective cover (5), the inner side of the rubber ring (4) is arranged on the outer side of the sample table (3), and a columnar hole is arranged on the lower side of the outer-layer protective cover (5) and serves as an inert gas inlet (13); a rubber ring (4) is arranged inside the right side of the inner layer protective cover (9), a heating blanket (7) is arranged on the outer wall of the inner layer protective cover (9), a columnar hole is arranged at the top of the left side of the inner layer protective cover (9) and serves as a pressure head inlet (11), and a columnar hole is arranged on the lower wall of the inner layer protective cover (9) and communicated with an inert gas inlet (13); a sealing plate (10) is arranged on the left side of the outer layer protective cover (5), and a pressure head inlet (11) is arranged in the middle of the sealing plate; the upper sides of the outer layer protective cover (5) and the inner layer protective cover (9) are provided with column-shaped holes for installing and sealing the visual cameras (8).
2. A cryogenic device for a nanoindenter as defined in claim 1 wherein said throttling micro-refrigerator (2) employs the joule-thomson effect of isenthalpic expansion for rapid refrigeration.
3. The cryodevice for nanoindenters according to claim 1, wherein the humidity sensor (6) is embedded inside the sample stage (3).
4. A cryogenic device for a nanoindenter as defined in claim 1 wherein the heater blanket (7) is wrapped around the inner protective cover (9) and water vapor is removed from the device by heating the heater blanket (7) and passing an inert gas stream through the inert gas inlet (13).
5. The cryodevice for nanoindenters according to claim 1, wherein the sample stage (3) ensures the sealing of the device by using an outer protective cover (5), an inner protective cover (9), and a sealing plate (10).
6. The low-temperature apparatus for a nanoindenter of claim 1, wherein the sealing plate (10) has a multi-layer sealing plate structure in which through holes in the sealing plates are not uniform in size and shape.
7. The cryodevice for nanoindenter of claim 6, wherein the through holes of the sealing plates (10) are circular or elliptical, the axes of the elliptical through holes coincide, and the major axes of the elliptical through holes do not overlap.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910414288.XA CN110182755B (en) | 2019-05-17 | 2019-05-17 | Low temperature device for nanometer pressing-in instrument |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910414288.XA CN110182755B (en) | 2019-05-17 | 2019-05-17 | Low temperature device for nanometer pressing-in instrument |
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| Publication Number | Publication Date |
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| CN110182755A CN110182755A (en) | 2019-08-30 |
| CN110182755B true CN110182755B (en) | 2021-10-29 |
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| CN201910414288.XA Active CN110182755B (en) | 2019-05-17 | 2019-05-17 | Low temperature device for nanometer pressing-in instrument |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110822098A (en) * | 2019-12-13 | 2020-02-21 | 马鞍山钢铁股份有限公司 | Shaft seal failure protection structure and application method thereof |
| CN113607584B (en) * | 2021-10-08 | 2021-12-07 | 太原科技大学 | Nano-indentator test sample high-temperature heating device |
Citations (6)
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| JP2010181191A (en) * | 2009-02-03 | 2010-08-19 | Shimadzu Corp | Internal pressure test device |
| CN104614935A (en) * | 2015-02-06 | 2015-05-13 | 浙江大学 | Universal high-precision micro-structure preparation system and application method of universal high-precision micro-structure |
| CN105021469A (en) * | 2015-07-10 | 2015-11-04 | 中山大学 | In-situ mechanical property testing device of nuclear material in high temperature irradiation simulation environment |
| CN204944965U (en) * | 2015-07-29 | 2016-01-06 | 吉林大学 | Miniature precision in-situ nano impression and scratch test device |
| CN106501109A (en) * | 2016-09-13 | 2017-03-15 | 北京理工大学 | The in-situ nano impression test platform of energy storage material under a kind of electrochemical hot atmosphere |
| CN208297278U (en) * | 2018-04-16 | 2018-12-28 | 吉林大学 | Micro-nano impression/the cut test device of two-pass combination drive |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3031345A1 (en) * | 2015-01-05 | 2016-07-08 | Ecole Polytech | PROCESS FOR THE SYNTHESIS OF CARBON MATERIALS FROM CARBONIC AGGLOMERATES CONTAINING CARBYN / CARBYNOID CHAINS |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010181191A (en) * | 2009-02-03 | 2010-08-19 | Shimadzu Corp | Internal pressure test device |
| CN104614935A (en) * | 2015-02-06 | 2015-05-13 | 浙江大学 | Universal high-precision micro-structure preparation system and application method of universal high-precision micro-structure |
| CN105021469A (en) * | 2015-07-10 | 2015-11-04 | 中山大学 | In-situ mechanical property testing device of nuclear material in high temperature irradiation simulation environment |
| CN204944965U (en) * | 2015-07-29 | 2016-01-06 | 吉林大学 | Miniature precision in-situ nano impression and scratch test device |
| CN106501109A (en) * | 2016-09-13 | 2017-03-15 | 北京理工大学 | The in-situ nano impression test platform of energy storage material under a kind of electrochemical hot atmosphere |
| CN208297278U (en) * | 2018-04-16 | 2018-12-28 | 吉林大学 | Micro-nano impression/the cut test device of two-pass combination drive |
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