CN113933325A - Method for preparing transmission electron microscope sample from rubber in stretching state and performing transmission electron microscope characterization - Google Patents
Method for preparing transmission electron microscope sample from rubber in stretching state and performing transmission electron microscope characterization Download PDFInfo
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- CN113933325A CN113933325A CN202111199419.0A CN202111199419A CN113933325A CN 113933325 A CN113933325 A CN 113933325A CN 202111199419 A CN202111199419 A CN 202111199419A CN 113933325 A CN113933325 A CN 113933325A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 42
- 239000005060 rubber Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000005540 biological transmission Effects 0.000 title claims abstract description 14
- 238000012512 characterization method Methods 0.000 title abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000003825 pressing Methods 0.000 claims abstract description 23
- 239000002390 adhesive tape Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 10
- 238000007710 freezing Methods 0.000 claims abstract description 6
- 230000008014 freezing Effects 0.000 claims abstract description 6
- 239000004636 vulcanized rubber Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 27
- 229910052802 copper Inorganic materials 0.000 claims description 27
- 239000010949 copper Substances 0.000 claims description 27
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims description 5
- 201000009310 astigmatism Diseases 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000005464 sample preparation method Methods 0.000 abstract description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 9
- 238000005086 pumping Methods 0.000 description 8
- 229910003460 diamond Inorganic materials 0.000 description 6
- 239000010432 diamond Substances 0.000 description 6
- 239000006229 carbon black Substances 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- 229920002857 polybutadiene Polymers 0.000 description 2
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010959 steel 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
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the technical field of rubber detection. Aiming at the problem that the TEM microstructure characterization of rubber in a tensile state is difficult at present, the transmission electron microscope characterization method is provided for preparing a transmission electron microscope sample from the rubber in the tensile state. The method comprises the following steps: cutting the vulcanized rubber sheet into rubber strips, stretching the rubber strips by using a stretching device, fixing the end parts of the rubber strips, and then quickly placing the rubber strips in liquid nitrogen for cooling so that the rubber strips do not shrink any more; rapidly transferring the adhesive tape which is in a stretching state and is frozen and fixed into a slicing chamber of a freezing slicer which is cooled in advance to be sliced into ultrathin slices; transferring the ultrathin section to a carrying net, and covering the other carrying net on the ultrathin section to form a sandwich structure; pressing the sandwich structure with a pressing block, and transferring to normal temperature until the sandwich structure is recovered to normal temperature. The sample preparation method is simple and wide in application range, and the microstructure characterization of the rubber in a stretching state at normal temperature is realized.
Description
Technical Field
The invention belongs to the technical field of rubber detection, and particularly relates to a method for preparing a transmission electron microscope sample from rubber in a stretched state and performing transmission electron microscope characterization.
Background
Transmission Electron Microscopy (TEM) samples of rubber in the free state (without any deformation) are currently well established and characterized, but are limited to rubber in the free state. The rubber is in a dynamic stretching (application) state during the running process of the tire, and the mechanical property of the rubber is generally expressed in continuous stretching deformation, so that the representation of the microstructure of the rubber in the stretching state is very important, but the representation of the microstructure of the rubber in the stretching state by using a TEM is blank all the time, the bottleneck of the representation is mainly difficult to prepare, so that a method for preparing and representing a TEM sample by using the rubber in the stretching state is necessary.
Disclosure of Invention
Aiming at the problem that the rubber in a stretched state is difficult to be subjected to TEM microstructure characterization at present, the invention provides a method for preparing a transmission electron microscope sample from the rubber in the stretched state and performing transmission electron microscope characterization, which has a wide application range and can truly reflect the microstructure of the rubber in the stretched state.
The technical scheme adopted by the invention is as follows:
in one aspect, the present invention provides a method for preparing a Transmission Electron Microscope (TEM) sample from rubber in a stretched state, comprising the steps of:
(1) cutting the vulcanized rubber sheet into an adhesive tape, fixing one end of the adhesive tape on a stretching device, and stretching the adhesive tape to a certain elongation;
(2) rapidly placing the stretched adhesive tape together with the stretching device in liquid nitrogen for cooling so that the adhesive tape does not shrink any more;
(3) rapidly transferring the adhesive tape which is in a stretching state and is frozen and fixed with a stretching device from liquid nitrogen to a freezing and slicing machine which is cooled in advance and manufacturing ultrathin slices;
(4) transferring the ultrathin section to a carrying net, and covering the other carrying net on the ultrathin section to form a sandwich structure;
(5) pressing the sandwich structure with a pressing block, and transferring to normal temperature until the sandwich structure is recovered to normal temperature.
The purpose of the pressing block is to fix the ultrathin section between two carrying nets, and the ultrathin section can be firmly adsorbed on the carrying nets, and after the ultrathin section is recovered to normal temperature, the pressing block is taken away, and the section can not shrink, so that the microstructure of the rubber in a stretching state can be shot by using a TEM.
Further, the thickness of the vulcanized rubber sheet in the step (1) is 50 um-2 mm; the width of the cut adhesive tape is 1 mm-4 mm.
Furthermore, the stretching device in the step (1) is a rigid straight plate with good dimensional stability, length scales or elongation scales are arranged on the straight plate for reading convenience, a pressing sheet for fixing an adhesive tape is arranged at one end of the straight plate, and the pressing sheet and the straight plate are fixed through bolts. The stretching device can be made of steel plates or iron plates.
Further, the elongation of the rubber strip in the step (1) may be adjusted according to circumstances, and is generally in the range of 100% to 500%.
Further, the stretched adhesive tape in the step (2) is cooled for 10-60 seconds in liquid nitrogen with a stretching device.
Further, the slicing method in the step (3) is as follows: in the microtome, a small strip with a width of 1mm to 2mm is first cut perpendicularly to the drawing direction using scissors which have been cooled beforehand in a slicing chamber, and then the small strip is clamped on a sample holder of the microtome to be sliced, with a slice thickness of 100nm to 300nm and a length of 1mm to 2 mm.
Further, the net in the step (4) is a copper net, a nickel net, a gold net or a molybdenum net with 100-400 meshes.
On the other hand, the invention provides a rubber TEM characterization method in a stretching state, a transmission electron microscope sample is prepared according to the method, then a sandwich structure carrying ultrathin sections is placed at the front end of a sample rod and is fixed, the sample rod is inserted into a TEM pre-pumping chamber, after vacuum pumping is carried out, the sample rod is sent into a lens barrel, an electron gun is opened, the sample is found at a low power, then axis combination, astigmatism adjustment and focusing are carried out, in order to improve the image contrast, a 20-micrometer objective diaphragm is selected, the magnification is adjusted, and a series of images are shot under the Scherflies under the condition of lack of focus.
Compared with the prior art, the invention has the following beneficial effects:
the TEM sample preparation and characterization of the rubber in a stretching state are realized, and the microstructure of the rubber in a normal-temperature stretching state can be truly represented; the sample preparation method is simple and easy to operate; the method is suitable for performing TEM microstructure characterization on all rubber materials.
Drawings
FIG. 1 is a schematic view of the drawing apparatus of examples 1 to 3, 1-bar, 2-plate, 3-bolt, 4-strip
FIG. 2 is a flow chart of the sandwich structure of examples 1-3;
FIG. 3 is a TEM image of a stretched rubber of example 1.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments and the accompanying drawings.
Example 1
A rubber sheet (gum seed is natural rubber, and filler is carbon black N134) with a thickness of 200 microns is prepared.
The adhesive tape was cut into 2mm wide tapes with a blade, one end of the tape was fixed to a stretching device at room temperature, and then the tape was stretched to 300% elongation, and then rapidly cooled in liquid nitrogen for 1 minute. The stretching device is structurally shown in figure 1 and comprises a rigid straight plate 1, wherein the straight plate 1 is provided with elongation rate scales, one end of the straight plate is provided with a pressing sheet 2 at one end of a fixing rubber strip 4, and the pressing sheet 2 and the straight plate are fixed through a bolt 3. In use, the other end of the strip can be pulled by hand to the desired elongation and held.
The cooled adhesive tape is quickly transferred from liquid nitrogen to a freezing microtome which is cooled in advance (below minus 50 ℃) together with a stretching device, a pair of scissors which are frozen in advance in a slicing chamber are used for cutting a strip with the width of 1mm in a direction perpendicular to the stretching direction, the strip is clamped on a sample clamp of the microtome for fixing, then a glass cutter is used for flattening the section, and finally an ultrathin section with the thickness of 200nm and the length of 1mm is cut by a diamond cutter for standby.
Sucking up a 200-mesh pure copper net by using a suction head, placing the pure copper net at the position close to a cutting edge of a diamond knife, transferring the cut regular slices to the copper net by using a lash brush, transferring 3 slices, transferring the copper net to one side of a knife rest by using the suction head, and finally covering another 200-mesh copper net on the copper net.
Pressing a cubic metal pressing block with the side length of about 1cm above the copper mesh, taking out the copper mesh and the pressing block together, placing on a table top, and placing for 10min at normal temperature for later use.
And placing the copper mesh loaded with the sample at the front end of the sample rod for fixing, inserting the sample rod into the TEM pre-pumping chamber, and sending the sample rod into the lens cone after vacuum pumping. Opening an electron gun, finding a sample at a low power, then performing operations such as axis combination, astigmatism adjustment, focusing and the like, selecting a 20-micrometer objective lens diaphragm to improve the image contrast, adjusting the magnification and shooting a series of images under the Sherzel under-focus condition.
Example 2
A rubber sheet (seed rubber is butadiene rubber, and filler is carbon black N234) with a thickness of 300 microns was prepared.
The film was first cut into a 2mm wide strip with a knife, stretched to 300% elongation after fixing one end of the strip on a stretching device at room temperature, and then rapidly cooled in liquid nitrogen for 1 minute.
And quickly transferring the cooled adhesive tape together with a stretching device into a freezing microtome which is cooled in advance to below (-50 ℃), cutting small strips with the width of 2mm by using scissors which are frozen in advance and perpendicular to the stretching direction, clamping the small strips on a sample holder of the microtome for fixing, flattening the cross section by using a glass cutter, and finally, cutting ultrathin sections with the thickness of 100nm and the length of 2mm by using a diamond cutter for standby.
Sucking up a 300-mesh pure copper net by using a suction head, placing the suction head at the position of a diamond knife close to a knife edge, transferring the cut regular slices to the copper net by using a lash brush, transferring 4 slices, transferring the copper net to one side of a knife rest by using the suction head, and finally covering another 300-mesh copper net on the suction head.
Pressing a cubic metal pressing block with the side length of about 1cm above the copper mesh, taking out the copper mesh and the pressing block together, placing on a table top, and placing for 10min at normal temperature for later use.
And placing the copper mesh loaded with the sample at the front end of the sample rod for fixing, inserting the sample rod into the TEM pre-pumping chamber, and sending the sample rod into the lens cone after vacuum pumping. Opening an electron gun, finding a sample at a low power, then performing operations such as axis combination, astigmatism adjustment, focusing and the like, selecting a 20-micrometer objective lens diaphragm to improve the image contrast, adjusting the magnification and shooting a series of images under the Sherzel under-focus condition.
Example 3
A rubber sheet (seed rubber is butadiene rubber, and filler is carbon black N330) with a thickness of 400 microns is prepared.
The film was first cut into strips of 3mm in width with a blade, one end of the strip was fixed to a stretching device at room temperature and then stretched to an elongation of 200%, and then it was rapidly cooled in liquid nitrogen for 2 minutes.
The cooled gel strip is rapidly transferred from liquid nitrogen together with a stretching device to a freezing microtome which is cooled in advance to below-50 DEG C
Cutting a small strip with the width of 1mm by using scissors which are frozen in a slicing chamber in advance and are perpendicular to the stretching direction, clamping the small strip on a sample clamp of a slicer for fixing, flattening the section by using a glass cutter, and finally, cutting an ultrathin slice with the thickness of 100nm and the length of 1mm by using a diamond cutter for standby.
Sucking up a 200-mesh pure copper net by using a suction head, placing the pure copper net at the position close to a cutting edge of a diamond knife, transferring the cut regular slices to the copper net by using a lash brush, transferring 3 slices, transferring the copper net to one side of a knife rest by using the suction head, and finally covering another 200-mesh copper net on the copper net.
Pressing a cubic metal pressing block with the side length of about 1cm above the copper mesh, taking out the copper mesh and the pressing block together, placing on a table top, and placing for 10min at normal temperature for later use.
And placing the copper mesh loaded with the sample at the front end of the sample rod for fixing, inserting the sample rod into the TEM pre-pumping chamber, and sending the sample rod into the lens cone after vacuum pumping. Opening an electron gun, finding a sample at a low power, then performing operations such as axis combination, astigmatism adjustment, focusing and the like, selecting a 20-micrometer objective lens diaphragm to improve the image contrast, adjusting the magnification and shooting a series of images under the Sherzel under-focus condition.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (8)
1. A method for manufacturing a transmission electron microscope sample from rubber in a stretching state is characterized by comprising the following steps:
(1) cutting the vulcanized rubber sheet into an adhesive tape, fixing one end of the adhesive tape on a stretching device, and stretching the adhesive tape to a certain elongation;
(2) placing the stretched adhesive tape together with the stretching device in liquid nitrogen for cooling so that the adhesive tape does not shrink any more;
(3) rapidly transferring the adhesive tape which is in a stretching state and is frozen and fixed with a stretching device from liquid nitrogen to a freezing and slicing machine which is cooled in advance and manufacturing ultrathin slices;
(4) transferring the ultrathin section to a carrying net, and covering the other carrying net on the ultrathin section to form a sandwich structure;
(5) pressing the sandwich structure with a pressing block, and transferring to normal temperature until the sandwich structure is recovered to normal temperature.
2. The method of claim 1, wherein the vulcanized rubber sheet of step (1) has a thickness of 50um to 2 mm; the width of the cut adhesive tape is 1 mm-4 mm.
3. The method according to claim 1, wherein the stretching device in step (1) is a rigid straight plate with length scale or elongation scale, and a pressing piece with a fixing rubber strip at one end, and the pressing piece and the straight plate are fixed by bolts.
4. The method according to claim 1, wherein the elongation of the rubber strip of step (1) is 100% to 500%.
5. The method according to claim 1, wherein the stretched rubber strip in step (2) is cooled in liquid nitrogen for 10-60 seconds.
6. The method of claim 1, wherein the slicing method of step (3) is: in the microtome, a small strip with a width of 1mm to 2mm is first cut perpendicularly to the drawing direction using scissors which have been cooled beforehand in a slicing chamber, and then the small strip is clamped on a sample holder of the microtome to be sliced, with a slice thickness of 100nm to 300nm and a length of 1mm to 2 mm.
7. The method according to claim 1, wherein the mesh in the step (4) is a copper mesh, a nickel mesh, a gold mesh or a molybdenum mesh with a mesh size of 100-400.
8. A rubber TEM representation method in a stretching state is characterized in that a transmission electron microscope sample is prepared according to the method of claims 1-7, then a sandwich structure carrying ultrathin sections is placed at the front end of a sample rod to be fixed, the sample rod is inserted into a TEM pre-drawing chamber, after vacuum drawing is completed, the sample rod is sent into a lens barrel, an electron gun is opened, the sample is found out under low power, then axis combination, astigmatism adjustment and focusing are carried out, in order to improve image contrast, a 20-micron objective diaphragm is selected, the magnification is adjusted, and a series of images are shot under the Scherrer under-focus condition.
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