Method for preparing cross section transmission electron microscope sample

Abstract

The invention belongs to the technical field of testing, and relates to a method for preparing a cross section transmission electron microscope sample. The method includes the steps as follows: firstly cutting a sample into long strips, cleaning the surfaces of the long strip samples with acetone to remove impurities, then airing the long strip samples naturally, coating the surface of each long strip sample provided with a film with a layer of curable adhesive, correspondingly bonding the adhesive surfaces of two long strip samples, heating and solidifying the long strip samples after mutualbonding at the temperature of 130 DEG, and then cooling the heated and solidified samples to the room temperature; and secondly cutting a through groove at one end of a molybdenum rod along the center, coating the outer surface of a to-be-tested sample and the inner surface of the groove with a layer of curable adhesive respectively, heating and solidifying the to-be-tested sample after putting and fixing the to-be-tested sample into the groove, coating the inner surface of a copper pipe with a layer of curable adhesive uniformly, plugging the molybdenum rod groove embedded with the to-be-tested sample and provided with one end coated with curable adhesive in the copper pipe, and performing cutting, grinding, dimpling and ion milling to the cross section sample, so as to obtain the electron microscope cross section sample. The method has a simple process, safe and reliable operating procedures, has no pollution and deformation in the sample, and is highly practical.

Description

Technical field: [0001] The invention belongs to the technical field of electron microscope testing of material products, and relates to a new process for preparing a material cross-section test sample for a transmission electron microscope, in particular to a preparation method for a cross-section transmission electron microscope sample. Background technique: [0002] At present, in the field of electron microscope testing technology, due to the limitation of electron penetration ability, in order to obtain good test results of test samples by transmission electron microscope, it is first necessary to prepare a good cross-section of the material to be tested by transmission electron microscope or to be tested. Sample, the standard of a good TEM sample is that the sample has a thin area that can be observed, and the thickness of the thin area is generally about 100nm; if the sample is to be analyzed by high-resolution microscopy, the thickness of the thin area is required to ...

AI Technical Summary

Problems solved by technology

In the current technology, researchers at home and abroad mainly use the method provided by Gatan Company of the United States to prepare cross-sectional samples for transmission electron microscopy. In this preparation method, the sample pretreatment process is relatively cumbersome, and the mechanical damage to the sample is relatively large. , In addition, it relies heavily on the proprietary equipment produced by its company, especially in the process of cutting the bonded sample into a cylinder (about 2.3mm in diameter) using an ultrasonic cutting machine (Gatan 601 Ultrasonic Cutter), Due to the effect of mechanical external force, the sample is easily broken under stress, which brings certain difficulties to the successful preparation of cross-section samples and causes waste of materials; The preparation method of the sample has been improved in many aspects. The specific operation is to mechanically grind and polish the bonded sample first, then stick a copper ring, and then carry out ion thinning. The copper in these technical solutions The ring introduction increases the extra thickness of the sample, prolongs the time of ion thinning, and causes greater damage to the sample

To sum up, the preparation process of the prior art is complicated, the preparation cost is high, the mechanical grinding and polishing are difficult, the effect is poor, and the sample is seriously damaged

Images