CN110455657B - Hydrogel nanoindentation area fine adjustment device - Google Patents
Hydrogel nanoindentation area fine adjustment device Download PDFInfo
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- CN110455657B CN110455657B CN201910804118.2A CN201910804118A CN110455657B CN 110455657 B CN110455657 B CN 110455657B CN 201910804118 A CN201910804118 A CN 201910804118A CN 110455657 B CN110455657 B CN 110455657B
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005350 fused silica glass Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002474 experimental method Methods 0.000 claims description 41
- 230000008569 process Effects 0.000 claims description 14
- 238000007373 indentation Methods 0.000 claims description 13
- 230000005540 biological transmission Effects 0.000 claims description 9
- 230000007246 mechanism Effects 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 8
- 238000009434 installation Methods 0.000 abstract description 6
- 230000008859 change Effects 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract 1
- 238000011160 research Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 230000003028 elevating effect Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011900 installation process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- G01N3/02—Details
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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
- G01N3/02—Details
- G01N3/04—Chucks
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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
- G01N3/02—Details
- G01N3/06—Special adaptations of indicating or recording means
- G01N3/068—Special adaptations of indicating or recording means with optical indicating or recording means
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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
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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
- G01N3/62—Manufacturing, calibrating, or repairing devices used in investigations covered by the preceding subgroups
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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
- G01N2203/04—Chucks, fixtures, jaws, holders or anvils
- G01N2203/0423—Chucks, fixtures, jaws, holders or anvils using screws
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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
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
- G01N2203/0647—Image analysis
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Abstract
The invention discloses a micro-adjusting device for a hydrogel nanoindentation area, which is characterized in that a main body of the device is a table body, a clamping groove capable of being installed on a nanoindentation instrument is formed in the lower portion of the table body, a fixing table and an accommodating hole are respectively formed in the surface of the table body, a standard fused quartz sample for checking is installed on the fixing table, the sample in the accommodating hole can be tightly fixed through screws in two directions, a circular table-shaped bearing table is arranged in the accommodating hole, the bearing table and a gear, a rack, a sliding groove, a worm gear and a bearing in the table body form a lifting table, and adjusting nuts on two sides of the table body are rotated to enable the bearing table to move up and down. The method can realize direct bearing of the hydrogel material in nanoindentation measurement, can adjust the height of the measured microscale area according to the deformation of the hydrogel along with water loss, reduces the installation time of the sample, and solves the problem of experimental error caused by the change of the microscale area due to the bearing and height adjustment of the hydrogel sample.
Description
Technical Field
The invention relates to a micro-adjusting device for a hydrogel nanoindentation area, in particular to a bearing adjusting device used in an in-place mechanical property test experiment of hydrogel by matching with a nanoindentor, and belongs to the technical field of micro-scale mechanical property tests.
Background
In the process of wide application of hydrogel due to good biocompatibility, the change and improvement of mechanical properties of hydrogel attract attention. The traditional hydrogel mechanical property research method adopts a uniaxial tension or compression experiment, but the method mainly researches the macroscopic mechanical property of the hydrogel with larger volume, and cannot complete the mechanical property research of the partial or microstructure of the hydrogel. As a non-destructive research method, the nano indentation experimental method can realize experimental research on the in-situ mechanical property of the hydrogel under the micro-nano scale in a mode of applying load to the diamond indenter to press the indenter into the material, and has the advantages of simple sample preparation, nearly nondestructive experiment, high positioning precision, wide application range and the like. But the bearing device that present nanoindentor used can't realize bearing the weight of directly to the aquogel, and because the shortcoming such as bearing platform height can not be adjusted, bearing area is little, greatly increased the experiment degree of difficulty. Therefore, the research on the hydrogel nanoindentation area micro-regulation device has high practical value.
In the current nanoindentation experimental process, sample load-bearing device can fix metallographic specimen or the sample that bonds on the fixed station, but still have some problems in the direct bearing and the sample altitude mixture control of aquogel sample:
(1) at present, the bottom of a sample bearing part in a nano indentation experiment is supported by a screw, so that the hydrogel material cannot be directly supported, and the hydrogel material must be fixed and supported by means of metallographic phase embedding or bonding on other samples and then placed on the screw of the nano indentation experiment bearing device. The bearing fixing method is complex and low in efficiency, and increases experiment difficulty.
(2) In the process of fixing the sample, the fixing method of the existing nanoindentation bearing device to the sample is in the form of bottom screw support and unidirectional lateral nailing. And the geometric center of the sample is often not coincident with the center of the screw in the sample placing process, and the surface of the sample can be inclined after the sample is laterally nailed. In a nano indentation experiment, a pressure head obtains relevant mechanical properties by adopting a mode of vertically pressing materials, and the inclination of the surface of a sample can cause the pressing area of the pressure head calculated by an experiment system to be inconsistent with the actual pressing area, thereby causing experiment errors.
(3) The nano indentation test height is within a certain range, and the experiment fails when the nano indentation test height is too much higher or lower than the standard sample. In the sample installation, whether sample and standard sample can only rely on the naked eye respectively at a horizontal plane, go back highly fixed and be difficult to the regulation after the installation, if the sample installation is too high or low excessively, can only pull down the sample and install again, this process can waste a large amount of time. And the surface of the hydrogel sample can be reduced due to dehydration shrinkage after a certain period of experiment, and the mechanical properties of the microstructure region can not be continuously measured due to the difficulty in finding the microstructure region during the reinstallation of the sample in the experiment process.
In order to overcome the problems, the invention provides a micro-adjusting device for a hydrogel nanoindentation area, which can directly bear soft substances such as hydrogel and the like on the basis of the function of the original nanoindentation bearing device, can realize the free height lifting of a bearing platform through nut adjustment, greatly saves the experiment time, ensures the continuous operation of a hydrogel nanoindentation experiment, and simultaneously ensures that a sample has no any micro disturbance in the test process, thereby reducing the data error caused by the repeated installation of the sample in the nanoindentation experiment process and more accurately obtaining the in-situ mechanical property of the material.
Disclosure of Invention
The invention aims to design a micro-adjusting device for a hydrogel nanoindentation area, which can directly bear a hydrogel nanoindentation sample, can freely adjust the height of a bearing platform, ensures that the material is not influenced by the preparation process, reduces the installation time of the sample and optimizes the whole experimental process.
In order to achieve the purpose, the technical scheme adopted by the invention is a hydrogel nanoindentation area micro-adjustment device, a table body (1) is a main body of the adjustment device, sliding grooves (2) are arranged at two ends of the bottom of the table body (1), and the table body (1) is arranged on a clamping seat of a nanoindentation instrument through the sliding grooves (2); the upper part of the table body (1) is provided with a fixed table (3) and an accommodating hole (5), a fused quartz standard sample (4) which can be used for calibrating a nano-indenter microscope and a pressure head is installed on the fixed table (3), experimental data on the fused quartz standard sample (4) can be used for correcting the shape parameters of the pressure head, the accommodating hole (5) is hollow, the top of the accommodating hole contains two screws (7) which are respectively adjusted in two directions, and the screws are used for screwing the nano-indenter sample in two freedom directions; a bearing table (6) for directly placing a hydrogel sample is arranged in the accommodating hole (5), and the bearing table (6) moves in the vertical direction under the rotation of adjusting nuts (8) on the two sides of the table body; the height adjusting mechanism is arranged in the table body (1), a rack (16) is used for supporting the height adjustment of the bearing table (6), the rack (16) is fixedly arranged on the sliding chute (15), and the rack (16) can move up and down in the sliding chute (15) under the driving of the helical gear (14); the helical gear (14) is installed on the transmission shaft (13), the other end of the transmission shaft (13) is provided with the worm wheel (12), the worm wheel (12) is meshed with the worm (11), the two ends of the worm (11) are provided with the adjusting nuts (8) for rotating the worm (11), and the bearing platform (6) is prevented from moving up and down under the condition of external force due to the self-locking property of the transmission of the worm wheel (12) and the worm (11); the transmission shaft (13) penetrates through the second bearing (10), the worm (11) penetrates through the first bearing, and the worm (11) and the transmission shaft (13) can freely rotate in the table body due to the existence of the first bearing and the second bearing (10) and play a role in supporting and fixing.
The experimental method of the hydrogel nanoindentation area fine adjustment device in nanoindentation comprises the following operation steps: placing the prepared hydrogel sample on a bearing table (6), rotating an adjusting nut (8) and observing the surface height of the hydrogel to enable the hydrogel sample to be slightly lower than the surface of a fused quartz standard sample (4) by about 2mm, and then installing the device on a nanoindentation clamping seat; on a fused quartz standard sample (4), after a microscope and an indenter pressure head of an indenter are checked, an operating instrument moves the device under the microscope, the height of a bearing table (6) is adjusted until a sample surface microstructure can be observed under the microscope, a fixing screw (7) is screwed in to fix a hydrogel sample, and an experimental area is selected for experiment; in the experiment process, the sample measuring area is lower than the nano indentation measuring area due to the water absorption shrinkage of the sample, the surface height of the hydrogel sample is adjusted by rotating the adjusting nut (8) according to the actual situation, and the experiment is continued after the microstructure surface area of the experiment sample is observed again.
The hydrogel nanoindentation area fine adjustment device provided by the invention has the functions of the original bearing device, can also realize direct bearing of a hydrogel sample, can adjust the height of the sample at any time according to the experimental requirements, solves the problems that the hydrogel sample cannot be directly supported and cannot be adjusted by the original sample table, can save the long time cost caused by preparation of the nanoindentation sample and repeated height adjustment due to the requirement of hydrogel bearing, and can reduce the water content of the hydrogel sample in long initial period of the experiment to influence the accuracy of the experimental result.
Compared with the traditional nano indentation experiment bearing device, the invention has the following advantages:
1. the bearing device can realize direct bearing of materials such as hydrogel and the like, can nail the sample from two freedom directions in the fixing process, reduces the time cost for preparing the nano indentation experiment sample due to the fact that the sample cannot be directly fixed, and avoids experiment errors caused by experiment surface inclination due to unidirectional screw nail tightening and bottom screw bearing.
2. The bearing device can realize free adjustment of the surface height of the sample, and the turbine worm in the lifting platform ensures that the surface height of the bearing platform has good stability, optimizes the installation process of the sample, and meets the requirement of adjusting the height of the sample at any time according to the surface height change of hydrogel.
3. The prior nanoindentor in China basically depends on import, an original sample table of the nanoindentor does not have the functions of size adjustment and direct fixation, and related matched components are expensive.
Drawings
Figure 1 is a schematic view of a hydrogel nanoindentation area micro-modulation device.
FIG. 2 is a view of an exemplary structure of an elevating platform inside a platform body of a hydrogel nanoindentation area fine adjustment device.
Detailed Description
The hydrogel nanoindentation area fine adjustment device and the method for performing nanoindentation experiments using the device according to the present invention will be described in further detail with reference to fig. 1 and 2.
An example view of a hydrogel nanoindentation region micro-adjustment device is shown in fig. 1, and is characterized in that: the device is externally composed of a table body (1), a clamping groove (2), a fixing table (3), a fused quartz standard sample (4), an accommodating hole (5), a bearing table (6), a fixing screw (7) and an adjusting screw (8). The structure of the lifting platform in the micro-adjusting device for the hydrogel nanoindentation areas is shown in fig. 2, and the lifting mechanism of the bearing platform (6) consists of a first bearing, a second bearing (10), a worm (11), a turbine (12), a transmission shaft (13), a helical gear (14), a sliding groove (15) and a rack (16) in the platform body (1). The clamping groove (2) is positioned at the bottom of the table body (1) and can be installed on the nano-indenter clamping groove in a sliding-in mode; the diameter of the bearing platform (6) is 3mm smaller than that of the accommodating hole (5), and the bearing platform can slide up and down in the accommodating hole (5); the bearing platform (6) is fixed with the rack (16), the rack (16) can move up and down in the chute (15) under the driving of the helical gear (14), and when the rack (16) is positioned at the top end of the chute (15), the maximum height adjustment of the bearing platform (6) in the accommodating hole (5) is realized; adjusting nut (8) and worm (11) are in same epaxial, and worm wheel (12) worm (11) mesh together, rotate adjusting nut (8), can realize reciprocating of plummer (6) through whole adjustment mechanism, and the meshing of worm wheel (12) worm (11) has the auto-lock nature, can only drive worm wheel (11) through worm (8) and rotate, and this to a great extent has guaranteed the stability of plummer (6).
The experimental method comprises the following specific steps: the prepared hydrogel sample is placed on a bearing table (6), an adjusting nut (8) is rotated to enable the surface of the hydrogel sample to be slightly lower than the fused quartz standard sample (4) by about 3mm, and then a clamping groove (15) of the device is slid into a clamping seat of the nano indentation. The accuracy of the correlation between the microscope and the indenter was checked on a fused silica standard (4) before the experiment was started.
After the checking is finished, the adjusting nut (8) is rotated until a clear hydrogel microstructure is observed under a microscope, the fixing screw (7) is rotated to fix the hydrogel sample table on the bearing table, and an experiment area is selected for an experiment; in the experiment process, the sample measuring area is lower than the nano indentation measuring area due to the water absorption shrinkage of the sample, the height of the bearing platform (6) is adjusted in a fine adjustment mode, and the experiment is continued after the microstructure surface area of the experiment sample is observed again.
Claims (2)
1. A hydrogel nanoindentation area fine adjustment device is characterized in that: the device comprises a table body (1), wherein the table body (1) is a main body of an adjusting device, clamping grooves (2) are formed in two ends of the bottom of the table body (1), a fixing table (3) and a containing hole (5) are formed in the upper portion of the table body, a fused quartz standard sample (4) is installed on the fixing table (3), the containing hole (5) is hollow, a bearing table (6) for directly placing a hydrogel sample is arranged in the containing hole (5), the bearing table (6) is fixed on the device through a rack (16), a height adjusting mechanism is installed in the table body (1), and the rack (16) is installed on a sliding groove (15); a helical gear (14) is meshed on the rack (16), the helical gear (14) is installed on a transmission shaft (13), a worm wheel (12) is arranged at the other end of the transmission shaft (13), and the worm wheel (12) is meshed with the worm (11); adjusting nuts (8) for rotating the worm (11) are arranged at two ends of the worm (11), the transmission shaft (13) penetrates through the second bearing (10), and the worm (11) penetrates through the first bearing (9);
the clamping groove (2) at the lower part of the table body (1) is fixedly arranged on a nano-indenter clamping table in a sliding manner; the fused quartz standard sample (4) at the upper part of the table body (1) is used for adjusting the contact ratio of a nano indenter microscope and a pressure head; two screws (7) are arranged on the side wall of the accommodating hole (5), and the bearing table (6) is fixed by the screws (7) in two freedom directions;
the surface of the bearing table (6) is a circular plane and directly bears a hydrogel sample; the adjusting nut (8) is rotated to realize the free movement of the bearing table (6) in the vertical direction; when the rack (16) is positioned at the top end of the sliding chute (15), the bearing platform (6) reaches the maximum height;
the worm wheel (12) and worm (11) structure has a self-locking characteristic, the worm (11) drives the worm wheel (12) to rotate, the bearing platform (6) is prevented from moving up and down under the condition of external force, and the stability of the lifting platform in the up-and-down adjusting process is ensured.
2. A method for performing nanoindentation experiments using the hydrogel nanoindentation area micro-regulating apparatus as defined in claim 1, characterized in that: placing the prepared hydrogel sample on a bearing table (6), rotating an adjusting nut (8) to enable the surface of the hydrogel sample to be 3mm lower than that of a fused quartz standard sample (4), and then sliding a clamping groove (2) into a clamping seat with nano indentations; before the experiment begins, firstly, checking the contact ratio between a microscope and a indenter of an indenter on a fused quartz standard sample (4); after the checking is finished, the adjusting nut (8) is rotated until a clear hydrogel microstructure is observed under a microscope, the fixing screw (7) is rotated to fix the hydrogel sample on the bearing table (6), and an experimental area is selected for carrying out an experiment; in the experiment process, the sample measuring area is lower than the nano indentation measuring area due to the water absorption shrinkage of the fused quartz standard sample (4), the height of the bearing table (6) is adjusted in a fine adjustment mode, and the experiment is continued after the microstructure surface area of the experiment sample is observed again.
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| CN104297082A (en) * | 2014-09-25 | 2015-01-21 | 吉林大学 | In-situ micro-nano indentation/scratch tester |
| CN108495658A (en) * | 2015-09-01 | 2018-09-04 | 巴克斯特国际公司 | Hemostatic material |
| CN109932262A (en) * | 2019-04-12 | 2019-06-25 | 中国原子能科学研究院 | The measurement method of mechanical property at material different depth |
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| JP2011013033A (en) * | 2009-06-30 | 2011-01-20 | Wd Media Singapore Pte Ltd | Nano indentation test method and apparatus of the same |
| JP2011064476A (en) * | 2009-09-15 | 2011-03-31 | Toppan Printing Co Ltd | Jig for parallel-feeding of samples |
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| CN102252923B (en) * | 2011-04-19 | 2013-01-23 | 赵宏伟 | Miniaturized in-situ nanoindentation testing device |
| CN206756618U (en) * | 2017-05-08 | 2017-12-15 | 吉林大学 | Suspension type rotary fast positioning original position impression/deepen arc cut test device |
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| CN104297082A (en) * | 2014-09-25 | 2015-01-21 | 吉林大学 | In-situ micro-nano indentation/scratch tester |
| CN108495658A (en) * | 2015-09-01 | 2018-09-04 | 巴克斯特国际公司 | Hemostatic material |
| CN109932262A (en) * | 2019-04-12 | 2019-06-25 | 中国原子能科学研究院 | The measurement method of mechanical property at material different depth |
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| Title |
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| 纳米压痕仪使用方法简介Nano-Indenter-G200;匿名;《CSDn https://download.csdn.net/download/yinzi912/9923521》;20170807;第1-9页 * |
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