CN118067482A - Preparation method of rare earth nickelate film section transmission sample - Google Patents
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 52
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 44
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000010432 diamond Substances 0.000 claims abstract description 171
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 171
- 238000000227 grinding Methods 0.000 claims abstract description 148
- 238000005498 polishing Methods 0.000 claims abstract description 95
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 79
- 238000005520 cutting process Methods 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 39
- 230000005484 gravity Effects 0.000 claims abstract description 16
- 239000010408 film Substances 0.000 claims description 69
- 238000010884 ion-beam technique Methods 0.000 claims description 25
- 229910002244 LaAlO3 Inorganic materials 0.000 claims description 21
- 239000010409 thin film Substances 0.000 claims description 16
- 230000003287 optical effect Effects 0.000 claims description 14
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- 239000002245 particle Substances 0.000 claims description 11
- 238000007517 polishing process Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
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- 238000004627 transmission electron microscopy Methods 0.000 description 1
Classifications
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- 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
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- 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
- G01N1/32—Polishing; Etching
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- 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
- G01N2001/2873—Cutting or cleaving
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Abstract
The invention discloses a preparation method of a rare earth nickelate film section transmission sample, and belongs to the technical field of material electron microscope testing. The method comprises the following steps: cutting the rare earth nickelate film to obtain an initial cutting sample; bonding and cutting the two initial cutting samples to obtain two sections to be sampled; two sections to be sampled are respectively fixed on a sample table, and the section samples are obtained by grinding and polishing by means of the self gravity of the sample table, wherein the first section and the second section are respectively and sequentially coated with diamond sand paper of 30 mu m, 15 mu m, 6 mu m, 3 mu m, 1 mu m and 0.1 mu m; and finally, carrying out low-temperature thinning by adopting an ion thinning instrument to obtain a rare earth nickelate film section transmission sample. The invention adopts a mode of combining manual and mechanical grinding to pre-thin the rare earth nickelate film opposite-sticking sample, eliminates the pit process, simplifies the sample preparation process, and solves the problems of difficult sample preparation and low success rate of the rare earth nickelate film section transmission sample.
Description
Technical Field
The invention relates to the technical field of material electron microscope testing, in particular to a preparation method of a rare earth nickelate film section transmission sample.
Background
Perovskite rare earth nickelates are one type of perovskite oxide and have received considerable attention because of their metal-insulator transition properties. Isothermal induction of perovskite rare earth nickelate metal-insulator transition can be achieved by hydrogen doping, which does not require temperature modulation, and can produce a higher band gap than the original insulating phase at low temperatures, which opens up more possibilities for its application. In order to study the changes in perovskite rare earth nickelate microstructure during this process, it was analyzed by means of transmission electron microscopy.
The preparation of the transmission electron microscope sample is a crucial step in the microscopic research of the transmission electron microscope. The transmission electron microscope requires that the electron beam can pass through the sample, and the thickness of the sample for transmission electron microscope analysis is preferably controlled within 100 nm due to the weak penetration of the electron beam. There are many preparation methods of the transmission electron microscope sample, and the transmission electron microscope sample is prepared by three main steps of pre-thinning, pit and final thinning by using a traditional sample preparation method which is widely applied. The main factors influencing the efficiency and the success rate of the method are the pre-thinning and pit process, wherein the pre-thinning usually adopts two thinning modes of manual grinding and mechanical grinding, the manual grinding has small applied external force, the thinning speed is low, the efficiency is low, and the mechanical grinding has large applied external force, the thinning speed is high and the efficiency is high. At present, a manual grinding mode is often adopted for brittle materials and adhesion samples, but for LaAlO 3, such a substrate with brittle quality and larger hardness, manual grinding is difficult to pre-thin, takes longer time, pit treatment is carried out on the samples after pre-thinning, so that the samples are extremely easy to crack, in addition, for the materials with larger hardness, ion thinning takes more time, long-time sputtering can cause the surface temperature of the samples to rise, and the samples are damaged.
Therefore, the invention provides a preparation method of a rare earth nickelate film section transmission sample, which aims to solve the problems of difficult sample preparation and low success rate in the preparation of the rare earth nickelate film section transmission sample.
Disclosure of Invention
Aiming at the problems of difficult sample preparation and low success rate in the existing rare earth nickelate film section transmission sample preparation, the invention provides a preparation method of the rare earth nickelate film section transmission sample, which comprises the steps of carrying out grinding, polishing and pre-thinning on the rare earth nickelate film sample by combining manual grinding and mechanical grinding, then carrying out final thinning to prepare the rare earth nickelate film section transmission sample, fixing the sample by a manual grinding table, facilitating the observation of the thickness of the sample at any time in the grinding process, simultaneously ensuring that the pressure applied to the sample is smaller and only the gravity of the sample table is higher, and avoiding sample fragmentation caused by larger applied pressure in the mechanical grinding process; the grinding speed is changed by adjusting the rotating speed of the grinding and polishing disc, so that the grinding time is shortened, and the phenomenon of uneven sample surface caused by applying pressure to the sample for accelerating the grinding speed in the manual grinding process is avoided; meanwhile, the thickness of the sample is smaller after mechanical grinding, a pit instrument is not required to be used for thinning, and the phenomenon that the opposite-sticking sample is cracked in the pit process is avoided; in the mechanical grinding process, the first surface is used for polishing as a main purpose, and the sample is still kept to be thick when turned over, so that cracking of the opposite-sticking sample in the turning over process is avoided; ion thinning is performed in a low-temperature environment, so that the sample is prevented from being damaged due to the fact that the temperature of the sample is increased under long-time energy concentrated sputtering.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
The invention aims to provide a preparation method of a rare earth nickelate film section transmission sample, which comprises the following steps:
cutting the rare earth nickelate film, and cleaning to obtain an initial cutting sample; bonding the surfaces of the two initial cutting samples to be stuck, curing, cutting along the length direction of the initial cutting samples after curing is finished to obtain to-be-sampled sections, and marking the to-be-sampled sections as a first section and a second section;
Fixing the first cutting surface on a sample stage, sequentially adopting 30 mu m diamond sand paper, 15 mu m diamond sand paper, 6 mu m diamond sand paper, 3 mu m diamond sand paper, 1 mu m diamond sand paper and 0.1 mu m diamond sand paper, and grinding and polishing after the first cutting surface contacts with the diamond sand paper by means of self gravity of the sample stage to obtain a primary grinding sample;
Fixing the second section on a sample stage, sequentially adopting 30 mu m diamond sand paper, 15 mu m diamond sand paper, 6 mu m diamond sand paper, 3 mu m diamond sand paper, 1 mu m diamond sand paper and 0.1 mu m diamond sand paper, and grinding and polishing after the second section contacts with the diamond sand paper by means of self gravity of the sample stage to obtain a section sample;
and simultaneously adopting an ion thinning instrument to thin the first section and the second section of the section sample to form a hole, enlarging a thin area of the section of the sample, and finally cleaning an amorphous layer to obtain the rare earth nickelate thin film section transmission sample.
Further, in the process of grinding and polishing the first section to be sampled, when the first section is contacted with the diamond abrasive paper and then ground and polished, the grinding and polishing rotating speed of the diamond abrasive paper is 15-30 rpm/min, and the thickness of a primary grinding sample after the grinding and polishing of the first section is 700 mu m; in the first section grinding and polishing process, the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches on diamond film particles on the first section are observed to be consistent, and the diamond abrasive paper of the next specification is replaced.
Further, in the second section grinding and polishing process, when the second section to be sampled is contacted with the diamond sand paper for grinding and polishing, the grinding and polishing rotating speed is 15-20 rpm/min when the diamond sand paper with the thickness of 30 mu m is adopted for grinding and polishing, and the grinding and polishing rotating speeds are 10-15 rpm/min when the diamond sand paper with the thickness of 15 mu m, the diamond sand paper with the thickness of 6 mu m and the diamond sand paper with the thickness of 3 mu m are adopted for grinding and polishing; when the 1 mu m diamond sand paper and the 0.1 mu m diamond sand paper are adopted for grinding and polishing, the grinding and polishing are 5-10 rpm/min; in the grinding and polishing process of the second section, the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the direction of scratches on diamond film particles on the first section is observed to be consistent, and the diamond abrasive paper of the next specification is replaced.
Further, in the second section grinding and polishing process, after grinding and polishing by adopting 30 mu m diamond sand paper, the thickness of the section sample is 100 mu m; sequentially adopting 15 mu m diamond sand paper, 6 mu m diamond sand paper and 3 mu m diamond sand paper for grinding and polishing, wherein the thickness of a section sample is 25 mu m; the thickness of the cross-section sample was 25 μm after polishing with 1 μm diamond coated abrasive and 0.1 μm diamond coated abrasive in this order.
Further, when the ion thinning instrument is adopted for thinning to an outlet, the voltage of the ion thinning instrument is 5-6 kV, the angle of the ion beam emitting target is +/-10 degrees, and the time is 60-90 minutes.
Further, the voltage of the ion thinning instrument is 3-4 kV, the angle of the ion beam emitting target is +/-8 degrees, and the time is 20-30 min when the thin area of the section of the sample is enlarged; and then changing the voltage of the ion thinning instrument to be 2-3 kV, wherein the angle of the ion beam emitting target is +/-5 degrees, and the time is 20-30 min.
Further, when the amorphous layer is cleaned, the voltage of the ion thinning instrument is 0.5-1 kV, the angles of the ion beam emitting targets are sequentially + -3 degrees, and the time is 10-20 min.
Further, when the ion thinning instrument is adopted for thinning, the temperature of the section sample is-40 ℃ to-70 ℃.
Further, the rare earth nickelate film is RNiO 3/LaAlO3 film or RNiO 3/Si film, and R is rare earth metal.
Further, two pieces of the surface of the initial cutting sample are adhered by adopting an adhesive, wherein the adhesive is formed by bonding G1 adhesive resin and a hardening agent according to the weight ratio of 10:1, and curing at 120 ℃ for 30min.
Compared with the prior art, the invention has the following beneficial effects:
The invention combines manual grinding and mechanical grinding to grind, polish and pre-thin the rare earth nickelate film sample, and finally thin the prepared rare earth nickelate film section transmission sample. The manual grinding table is used for fixing the sample, so that the thickness of the sample can be conveniently observed in the grinding process, meanwhile, the pressure applied to the sample is small, and only the gravity of the sample table is used, so that the sample is prevented from being broken due to the fact that the pressure applied in the mechanical grinding process is large; the grinding speed is changed by adjusting the rotating speed of the grinding and polishing disc, so that the grinding time is shortened, the phenomenon that the surface of the sample is uneven due to the fact that pressure is applied to the sample for accelerating the grinding speed in the manual grinding process is avoided, meanwhile, the thickness of the sample after mechanical grinding is smaller, a pit instrument is not required to be used for thinning, and the phenomenon that the opposite-sticking sample is broken in the pit process is avoided; in the mechanical grinding process, the first surface is used for polishing as a main purpose, and the sample is still kept to be thick when turned over, so that cracking of the opposite-sticking sample in the turning over process is avoided; ion thinning is performed in a low-temperature environment, so that the sample is prevented from being damaged due to the fact that the temperature of the sample is increased under long-time energy concentrated sputtering.
Compared with the traditional sample preparation method, the method has the advantages that the pit process is omitted, the sample preparation process is simplified, the possibility of cracking the sticky sample is reduced, the pre-thinned sample is thinner, the sample preparation process is simplified, the ion thinning is carried out at low temperature, and finally, the preparation of the high-success-rate and high-quality RNiO 3/LaAlO3 film or RNiO 3/Si film opposite sticky sample is realized. And the ion thinning effect can be better without preparing a wedge-shaped sample, the operation is simpler, and the ion thinning process is carried out at low temperature, so that the damage of ion beams to the sample in the sample preparation process is reduced.
Drawings
FIG. 1 is a schematic diagram of the process flow for preparing a transmissive sample of a rare earth nickelate thin film cross section according to the present invention.
FIG. 2 is an optical view of a NdNiO 3/LaAlO3 thin film cross-section transmission sample prepared in example 1 of the present invention.
FIG. 3 is a high resolution transmission electron microscope image of NdNiO 3/LaAlO3 thin film interfaces prepared in example 1 of the present invention.
FIG. 4 is a high resolution transmission electron microscope image of SmNiO 3/LaAlO3 thin film interfaces prepared in example 2 of the present invention.
FIG. 5 is a transmission electron microscope image of SmNiO 3/Si thin film cross-section sample prepared in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials described are commercially available unless otherwise specified.
According to the invention, in the pre-thinning stage, the transmission sample of the rare earth nickelate film section prepared by combining manual grinding with the grinding and polishing disc is utilized, external force is not applied in the grinding process except for the self gravity of the sample table, the grinding speed is changed by adjusting the rotating speed of the grinding and polishing disc, so that the grinding time is shortened, the phenomenon that the surface of the sample is uneven due to the fact that pressure is applied to the sample for accelerating the grinding speed in the manual grinding process is avoided, meanwhile, the thickness of the sample is smaller after mechanical grinding, the thickness of the sample is kept to be larger when the sample is turned over only by polishing without pre-thinning in the thickness when the first surface is ground, the possibility of cracking of the sticky sample is reduced, and the section thin area is obtained in the thinning stage without using a pit instrument for thinning, so that the sticky sample is prevented from being cracked in the pit process, and the problems that the RNiO 3/Si or RNiO 3/LaAlO3 film is easy to crack and the RNiO 3/LaAlO3 film or RNiO 3/Si film is difficult to grind the sticky sample are solved, and the efficiency is low and time-consuming are solved.
The invention provides a preparation method of a rare earth nickelate film section transmission sample, wherein a process flow diagram is shown in figure 1, and the preparation method comprises the following steps:
cutting the rare earth nickelate film, and cleaning to obtain an initial cutting sample; bonding the surfaces of the two initial cutting samples to be stuck, curing, cutting along the length direction of the initial cutting samples after curing is finished to obtain to-be-sampled sections, and marking the to-be-sampled sections as a first section and a second section;
fixing the first cutting surface on a sample stage, sequentially adopting 30 mu m diamond sand paper, 15 mu m diamond sand paper, 6 mu m diamond sand paper, 3 mu m diamond sand paper, 1 mu m diamond sand paper and 0.1 mu m diamond sand paper, and grinding and polishing after the first cutting surface is contacted with the diamond sand paper by means of self gravity of the sample stage without applying extra pressure to obtain a primary grinding sample;
Fixing the second section on a sample stage, sequentially adopting 30 mu m diamond sand paper, 15 mu m diamond sand paper, 6 mu m diamond sand paper, 3 mu m diamond sand paper, 1 mu m diamond sand paper and 0.1 mu m diamond sand paper, and grinding and polishing after the second section is contacted with the diamond sand paper by means of self gravity of the sample stage without applying additional pressure to obtain a section sample;
and simultaneously adopting an ion thinning instrument to thin the first section and the second section of the section sample to form a hole, enlarging a thin area of the section of the sample, and finally cleaning an amorphous layer to obtain the rare earth nickelate film section transmission sample.
In a specific embodiment, in the first section grinding and polishing process, when the first section to be sampled is ground and polished after being contacted with the diamond abrasive paper, the grinding and polishing rotating speed of the diamond abrasive paper is 15-30 rpm/min, and the thickness of a primary grinding sample after the grinding and polishing of the first section is 700 mu m. Wherein, the sample to be sampled is fixed on a sample stage by adopting hot melt adhesive, the diamond sand paper is fixed on a grinding and polishing disc, the first section to be sampled faces downwards, the sample stage is held by hand, and the first section to be sampled is contacted with the diamond abrasive paper by means of the gravity of the sample stage to carry out grinding and polishing. The condition for replacing the diamond abrasive paper is that the directions of scratches remained on the diamond film particles on the first section are consistent under a 100 times optical microscope, which indicates that the scratches are introduced for grinding the last diamond abrasive paper, and the diamond abrasive paper with the next specification is replaced.
In the invention, the rare earth nickelate film can be prepared on brittle substrates such as LaAlO 3 (LAO)、SrTiO3 (STO), glass, quartz and the like, and also can be prepared on a Si substrate.
According to the invention, in the first cutting surface grinding process, external force is not applied except the self gravity of the sample table, the grinding speed is changed by adjusting the rotating speed of the grinding and polishing disc, so that the grinding time is shortened, the phenomenon that the surface of the sample is uneven due to the fact that pressure is applied to the sample for accelerating the grinding speed in the manual grinding process is avoided, meanwhile, the thickness of the sample after mechanical grinding is smaller, only polishing is not performed when the first surface is ground, and the larger thickness is kept when the sample is turned over, so that the possibility of cracking the sticky sample is reduced. In the present invention, the purpose of the hot melt adhesive is to fix the sample to the sample stage, and the hot melt adhesive is a plastic adhesive which is conventionally purchased.
In a specific embodiment, in the process of grinding and polishing the second section, when the second section to be sampled is contacted with the diamond abrasive paper for grinding and polishing, and the grinding and polishing speed is 15 rpm/min when the diamond abrasive paper with the thickness of 30 mu m is adopted for grinding and polishing; when 15 mu m diamond sand paper, 6 mu m diamond sand paper and 3 mu m diamond sand paper are adopted for grinding and polishing, the grinding and polishing rotating speeds are 10-15 rpm/min; when the 1 mu m diamond sand paper and the 0.1 mu m diamond sand paper are adopted for grinding and polishing, the grinding and polishing rotating speeds are 5-10 rpm/min. In the invention, the mode of grinding and polishing the second section is basically the same as the mode of grinding and polishing the first section, after grinding and polishing the first section, the to-be-sampled surface (namely the second section) is turned over, the to-be-sampled surface is fixed on a sample table by adopting hot melt adhesive, diamond abrasive paper is fixed on a grinding and polishing disc, the to-be-sampled second section faces downwards, the sample table is held by a hand, the to-be-sampled second section is contacted with the diamond abrasive paper by means of self gravity of the sample table, grinding and polishing are carried out, firstly, the 30 mu m diamond abrasive paper is used for quickly grinding the sample until a linear cutting trace disappears, then 15 mu m, 6 mu m and 3 mu m diamond abrasive paper are sequentially replaced for grinding, and the condition that the scratch directions of the sample under a 100 times optical microscope are consistent is that scratches introduced by grinding the last diamond abrasive paper are ground, and finally, the sample is polished by 1 mu m abrasive paper and 0.5 mu m abrasive paper.
In a specific embodiment, in the second section grinding and polishing process, after grinding and polishing by adopting 30 μm diamond sand paper, the thickness of a section sample is 100 μm, the excessive thickness subsequent grinding time is prolonged, and the excessive thickness sample is easy to crack; after the 15 mu m diamond sand paper, the 6 mu m diamond sand paper and the 3 mu m diamond sand paper are sequentially adopted for grinding and polishing, the thickness of a section sample is 25 mu m, the subsequent ion thinning of the thickness sample takes shorter time, and the sample is not easy to crack; the thickness of the cross-section sample was 25 μm after polishing with 1 μm diamond coated abrasive and 0.1 μm diamond coated abrasive in this order for the purpose of thoroughly removing scratches on the sample surface.
In a specific embodiment, grinding and polishing are carried out to obtain a section sample, a molybdenum ring is fixed on a second section of the section sample by using a curing agent, then the section sample is separated from a sample table by placing the section sample in a solvent, the solvent adopted for separating the section sample from the sample table is acetone solution, and the soaking time is 30-60 min. In the present invention, the purpose of the curing agent is to fix the molybdenum ring on the polished cross-section sample, and the curing agent is a conventionally purchased curing agent such as AB glue.
In a specific embodiment, when the ion thinning instrument is adopted to thin the ion thin the hole, the voltage of the ion thinning instrument is 4.5-6 kV, the angle of the ion beam emitting target is +/-10 degrees, and the time is 60-90 minutes. In the invention, the large voltage is adopted to thin to form the hole, the edge area of the hole is thinner, and the voltage can quickly form the hole and reduce the possibility of amorphization of the sample under the condition of excessive power and long-time ion thinning as an observable area.
In a specific embodiment, the voltage of the ion thinning instrument is 3-4 kV, the angle of the ion beam emitting target is +/-8 degrees, and the time is 20-30 min when the thin area of the section of the sample is enlarged; and then changing the voltage of the ion thinning instrument to be 2-3 kV, wherein the angle of the ion beam emitting target is +/-5 degrees, and the time is 20-30 min. The purpose is to expand the thin area faster and cause less amorphization damage to the sample.
In a specific embodiment, when the amorphous layer is cleaned, the voltage of the ion thinning instrument is 0.5-1 kV, the angle of the ion beam emitting target is sequentially +/-3 degrees, and the time is 10-20 min. The purpose is to achieve better amorphous layer cleaning effect.
In a specific embodiment, when the ion thinning instrument is adopted for thinning, the temperature of the section sample is-40 ℃ to-70 ℃. In the invention, ion thinning is performed in a low-temperature environment, so that the sample is prevented from being damaged due to the fact that the temperature of the sample is increased under the sputtering condition of long-time energy concentration.
In a specific embodiment, the rare earth nickelate film is RNiO 3/LaAlO3 film or RNiO 3/Si film, and R is rare earth metal. In the invention, R is Nd or Sm, and the substrate of the film is LaAlO 3 or Si substrate.
In a specific embodiment, an adhesive is used to adhere the two surfaces of the initial cut sample, wherein the adhesive is prepared from G1 adhesive resin and a hardener in a weight ratio of 10:1, and the curing temperature is 120 ℃ and the curing time is 30 min. In the invention, the purpose of adopting two initial cutting samples for opposite pasting is first that in order to protect the film surface, the glue plays a role in protecting the film surface, if only one is used, the film is directly thinned when the ions are thinned, and if the film is thinner, the ion thinning process can be completely reduced; secondly, an observable area after thinning is increased, thinning is carried out on the adhered ions, thin areas can be found on two sides of the hole, and if only one thin area is found on one side; thirdly, the ion thinning causes a hole in the center of the sample, so that the film is required to be positioned in the center of the sample, and the center position of the opposite-adhesion sample is easier to ensure than that of a single sample.
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with specific examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
Example 1
A preparation method of NdNiO 3/LaAlO3 film section transmission sample comprises the steps of (100) monocrystal LaAlO 3, nd and Ni atomic ratio being 1:1, a process flow diagram is shown in fig. 1, and comprises the following steps:
S1, sample pretreatment: the NdNiO 3/LaAlO3 film was cut into 5×5mm squares, the hot melt adhesive attached to the sample was removed with acetone, and the surface of the sample was cleaned with alcohol to obtain an initial cut sample.
S2, sample adhesion: the weight ratio of the G1 glue resin to the hardener is 10:1, uniformly mixing to form an adhesive, then smearing the adhesive on the surfaces of the initial cutting samples by using toothpicks, bonding the surfaces of the two initial cutting samples, transferring the two initial cutting samples into a spring clamp, and heating the spring clamp at 120 ℃ for 30min to solidify the spring clamp to obtain the opposite-sticking samples.
S3, cutting: and cutting the opposite-sticking sample into strips of 3X 1mm along the length direction of the initial cutting sample, taking the middle cutting sample, and obtaining a sample to be sampled with two sections, namely a first section and a second section.
S4, pre-thinning: fixing a sample to be sampled on a sample stage by adopting hot melt adhesive, fixing diamond abrasive paper on a grinding and polishing disc, holding the sample stage by holding the first section to be sampled facing downwards, enabling the first section to be sampled to be in contact with the diamond abrasive paper by means of self gravity of the sample stage, grinding and polishing, setting the rotating speed of the grinding and polishing disc to be 15 rpm/min, and sequentially adopting 30-um diamond abrasive paper, 15-um diamond abrasive paper, 6-um diamond abrasive paper, 3-um diamond abrasive paper, 1-um diamond abrasive paper and 0.1-um diamond abrasive paper, and grinding and polishing to obtain a primary grinding sample, wherein the thickness of the sample is about 700 mu m; the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches left on diamond film particles on a first section are consistent, and the scratches are indicated to be the grinding introduction of the last diamond abrasive paper, and the diamond abrasive paper of the next specification is replaced.
S4, thinning: after the first section is sampled, ground and polished, the turnover surface (namely the second section) of the product is fixed on a sample table by using hot melt adhesive, diamond abrasive paper is fixed on a grinding and polishing disc, the rotating speed of the grinding and polishing disc is set to be 15 rpm/min, and 30 mu m of diamond abrasive paper is used for polishing until the thickness of the sample is about 100 mu m; setting the rotation speed of a polishing disc to be 10 rpm/min, and polishing the sample to the thickness of about 25 mu m by using 15 mu m, 6 mu m and 3 mu m diamond sand paper respectively; setting the rotation speed of a grinding and polishing disc to be 5 rpm/min, and carrying out final polishing by using diamond sand paper with the diameter of 1 mu m and 0.1 mu m to obtain a section sample; the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches left on diamond film particles on a second section are consistent, and the scratches are indicated to be the grinding introduction of the last diamond abrasive paper, and the diamond abrasive paper of the next specification is replaced.
S5, sticking the ring: and (3) sticking the molybdenum ring on the section sample by using AB glue, transferring the section sample table and the sample together into acetone solution after the AB glue is solidified, soaking 40 min until the hot melt glue on the sample table is dissolved, and separating the section sample from the sample table to obtain the section sample to be thinned by ions.
S6, ion thinning: placing a sample with a section to be thinned in an ion thinning instrument provided with a liquid nitrogen cooling control system, adding liquid nitrogen, setting the thinning temperature to be-50 ℃, and starting double-sided thinning after the temperature is stable; simultaneously adopting an ion thinning instrument to thin the first section and the second section of the section sample to form an outlet, wherein the voltage of the ion thinning instrument is6 kV, the angle of the ion beam emitting target is +/-10 degrees, and the time is 70 min; the voltage of the ion thinning instrument is 3 kV, the angle of the ion beam emitting target is +/-8 degrees, the time is 25 min, and then the voltage of the ion thinning instrument is changed to 2 kV, the angle of the ion beam emitting target is +/-5 degrees, and the time is 25 min; and finally cleaning the amorphous layer, wherein the voltage of the ion thinning instrument is 1 kV, the angle of the ion beam emitting target is sequentially +/-3 degrees, and the time is 15 min, so that a NdNiO 3/LaAlO3 film section transmission sample is obtained. The thickness of the NdNiO 3/LaAlO3 film section transmission sample is about 20 mu m, pit treatment is not needed, and the final NdNiO 3/LaAlO3 film section transmission sample can be obtained after low-temperature ion thinning by about 2h.
FIG. 2 is an optical view of a NdNiO 3/LaAlO3 thin film cross-section transmission sample prepared in example 1 of the present invention. As shown in fig. 2, the middle hole is created by ion thinning, and the edge area of the hole is the viewable area.
FIG. 3 is a High Resolution Transmission Electron Microscope (HRTEM) image of NdNiO 3/LaAlO3 thin film interfaces prepared in example 1 of the present invention. As shown in fig. 3, the transmission sample was imaged clearly at high resolution, and good ductility of NdNiO 3 film was observed.
Example 2
A preparation method of SmNiO 3/LaAlO3 film section transmission sample comprises the steps of (100) monocrystal LaAlO 3, sm and Ni with atomic ratio of 1:1, a process flow diagram is shown in fig. 1, and comprises the following steps:
S1, sample pretreatment: the SmNiO 3/LaAlO3 film was cut into 5×5mm squares, the hot melt adhesive attached to the sample was removed with acetone, and the surface of the sample was cleaned with alcohol to obtain an initial cut sample.
S2, sample adhesion: the weight ratio of the G1 glue resin to the hardener is 10:1, uniformly mixing to form an adhesive, then smearing the adhesive on the surfaces of the initial cutting samples by using toothpicks, bonding the surfaces of the two initial cutting samples, transferring the two initial cutting samples into a spring clamp, and heating the spring clamp at 120 ℃ for 30min to solidify the spring clamp to obtain the opposite-sticking samples.
S3, cutting: and cutting the opposite-sticking sample into strips of 3X 1mm along the length direction of the initial cutting sample, taking the middle cutting sample, and obtaining a sample to be sampled with two sections, namely a first section and a second section.
S4, pre-thinning: fixing a sample to be sampled on a sample stage by adopting hot melt adhesive, fixing diamond abrasive paper on a grinding and polishing disc, holding the sample stage by holding the first section to be sampled facing downwards, enabling the first section to be sampled to be in contact with the diamond abrasive paper by means of self gravity of the sample stage, grinding and polishing, setting the rotating speed of the grinding and polishing disc to be 15 rpm/min, and sequentially adopting 30-um diamond abrasive paper, 15-um diamond abrasive paper, 6-um diamond abrasive paper, 3-um diamond abrasive paper, 1-um diamond abrasive paper and 0.1-um diamond abrasive paper, and grinding and polishing to obtain a primary grinding sample, wherein the thickness of the sample is about 700 mu m; the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches left on diamond film particles on a first section are consistent, and the scratches are indicated to be the grinding introduction of the last diamond abrasive paper, and the diamond abrasive paper of the next specification is replaced.
S4, thinning: after the first section is sampled, ground and polished, the turnover surface (namely the second section) of the product is fixed on a sample table by using hot melt adhesive, diamond abrasive paper is fixed on a grinding and polishing disc, the rotating speed of the grinding and polishing disc is set to be 15 rpm/min, and 30 mu m of diamond abrasive paper is used for polishing until the thickness of the sample is about 100 mu m; setting the rotation speed of a polishing disc to be 10 rpm/min, and polishing the sample to the thickness of about 25 mu m by using 15 mu m, 6 mu m and 3 mu m diamond sand paper respectively; setting the rotation speed of a grinding and polishing disc to be 5 rpm/min, and carrying out final polishing by using diamond sand paper with the diameter of 1 mu m and 0.1 mu m to obtain a section sample; the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches left on diamond film particles on a second section are consistent, and the scratches are indicated to be the grinding introduction of the last diamond abrasive paper, and the diamond abrasive paper of the next specification is replaced.
S5, sticking the ring: and (3) sticking the molybdenum ring on the section sample by using AB glue, transferring the section sample table and the sample together into acetone solution after the AB glue is solidified, soaking 50 min until the hot melt glue on the sample table is dissolved, and separating the section sample from the sample table to obtain the section sample to be thinned by ions.
S6, ion thinning: placing a sample with a section to be thinned in an ion thinning instrument provided with a liquid nitrogen cooling control system, adding liquid nitrogen, setting the thinning temperature to be-70 ℃, and starting double-sided thinning after the temperature is stable; simultaneously adopting an ion thinning instrument to thin the first section and the second section of the section sample to form an outlet, wherein the voltage of the ion thinning instrument is 6 kV, the angle of the ion beam emitting target is +/-10 degrees, and the time is 60 min; the voltage of the ion thinning instrument is 3 kV, the angle of the ion beam emitting target is +/-8 degrees, the time is 30 min, then the voltage of the ion thinning instrument is 2 kV, the current is 20min, the angle of the ion beam emitting target is +/-5 degrees, and the time is 20 min; and finally cleaning the amorphous layer, wherein the voltage of the ion thinning instrument is 1 kV, the angle of the ion beam emitting target is +/-3 degrees, and the time is 20 minutes, so that a SmNiO 3/LaAlO3 film section transmission sample is obtained. The SmNiO 3/LaAlO3 film cross-section sample had a thickness of about 20 μm and was not subjected to pit treatment, and the final transmission sample was obtained after low temperature ion thinning of about 2: 2h.
Fig. 4 is a High Resolution Transmission Electron Microscope (HRTEM) image of SmNiO 3/LaAlO3 thin film interfaces prepared in example 2 of the present invention. As shown in fig. 4, the transmission sample was imaged clearly at high resolution, and good ductility of SmNiO 3 film was observed.
Example 3
A preparation method of SmNiO 3/Si film section transmission sample comprises the steps of (100) monocrystal Si, sm and Ni with atomic ratio of 1:1, a process flow diagram is shown in fig. 1, and comprises the following steps:
s1, sample pretreatment: after the SmNiO 3/Si film is cut into blocks of 5X 5mm, acetone is used for removing the hot melt adhesive attached on the sample, and then alcohol is used for cleaning the surface of the sample, so that an initial cut sample is obtained.
S2, sample adhesion: the weight ratio of the G1 glue resin to the hardener is 10:1, uniformly mixing to form an adhesive, then smearing the adhesive on the surfaces of the initial cutting samples by using toothpicks, bonding the surfaces of the two initial cutting samples, transferring the two initial cutting samples into a spring clamp, and heating the spring clamp at 120 ℃ for 30min to solidify the spring clamp to obtain the opposite-sticking samples.
S3, cutting: and cutting the opposite-sticking sample into strips of 3X 1mm along the length direction of the initial cutting sample, taking the middle cutting sample, and obtaining a sample to be sampled with two sections, namely a first section and a second section.
S4, pre-thinning: fixing a sample to be sampled on a sample stage by adopting hot melt adhesive, fixing diamond abrasive paper on a grinding and polishing disc, holding the sample stage by holding the first section to be sampled facing downwards, enabling the first section to be sampled to be in contact with the diamond abrasive paper by means of self gravity of the sample stage, grinding and polishing, setting the rotating speed of the grinding and polishing disc to be 15 rpm/min, and sequentially adopting 30-um diamond abrasive paper, 15-um diamond abrasive paper, 6-um diamond abrasive paper, 3-um diamond abrasive paper, 1-um diamond abrasive paper and 0.1-um diamond abrasive paper, and grinding and polishing to obtain a section sample, wherein the thickness of the sample is about 700 mu m; the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches left on diamond film particles on a first section are consistent, and the scratches are indicated to be the grinding introduction of the last diamond abrasive paper, and the diamond abrasive paper of the next specification is replaced.
S4, thinning: after the first section is sampled, ground and polished, the turnover surface (namely the second section) of the product is fixed on a sample table by using hot melt adhesive, diamond abrasive paper is fixed on a grinding and polishing disc, the rotating speed of the grinding and polishing disc is set to be 15 rpm/min, and 30 mu m of diamond abrasive paper is used for polishing until the thickness of the sample is about 100 mu m; setting the rotation speed of a polishing disc to be 10 rpm/min, and polishing the sample to the thickness of about 25 mu m by using 15 mu m, 6 mu m and 3 mu m diamond sand paper respectively; setting the rotation speed of a grinding and polishing disc to be 5 rpm/min, and carrying out final polishing by using diamond sand paper with the diameter of 1 mu m and 0.1 mu m to obtain a section sample; the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches left on diamond film particles on a second section are consistent, and the scratches are indicated to be the grinding introduction of the last diamond abrasive paper, and the diamond abrasive paper of the next specification is replaced.
S5, sticking the ring: and (3) sticking the molybdenum ring on the section sample by using AB glue, transferring the section sample table and the sample together into acetone solution after the AB glue is solidified, soaking 40 min until the hot melt glue on the sample table is dissolved, and separating the section sample from the sample table to obtain the section sample to be thinned by ions.
S6, ion thinning: placing a sample with a section to be thinned in an ion thinning instrument provided with a liquid nitrogen cooling control system, adding liquid nitrogen, setting the thinning temperature to be-40 ℃, and starting double-sided thinning after the temperature is stable; simultaneously adopting an ion thinning instrument to thin the first section and the second section of the section sample to form an outlet, wherein the voltage of the ion thinning instrument is 5 kV, the angle of the ion beam emitting target is +/-10 degrees, and the time is 60 min; the voltage of the ion thinning instrument is 3 kV, the angle of the ion beam emitting target is +/-8 degrees, the time is 15 min, then the voltage of the ion thinning instrument is changed to 2 kV, the angle of the ion beam emitting target is +/-5 degrees, and the time is 15 min; and finally cleaning the amorphous layer, wherein the voltage of the ion thinning instrument is 0.8 kV, the angle of the ion beam emitting target is sequentially +/-3 degrees, and the time is 10min, so as to obtain a SmNiO 3/Si film section transmission sample. The thickness of the SmNiO 3/Si film cross-section pre-thinned sample is about 20 μm, pit treatment is not needed, and the final transmission sample can be obtained after low-temperature ion thinning is about 2h.
FIG. 5 is a Transmission Electron Microscope (TEM) image of a sample of a cross-section of a film of example 3 SmNiO 3/Si of the present invention. The cross-sectional structure is shown in fig. 5, smNiO 3 thin films of uniform thickness, about 77 a nm a thin layer of amorphous SiO 2 is present between the crystalline Si substrate and the thin film.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. The preparation method of the rare earth nickelate film section transmission sample is characterized by comprising the following steps of:
Cutting the rare earth nickelate film to obtain an initial cutting sample; adhering and oppositely pasting the surfaces of the two initial cutting samples, curing, and cutting along the length direction of the initial cutting samples after curing is finished to obtain a sample to be sampled, wherein the sample to be sampled is provided with a first section and a second section;
Fixing the first cutting surface on a sample stage, sequentially adopting 30 mu m diamond sand paper, 15 mu m diamond sand paper, 6 mu m diamond sand paper, 3 mu m diamond sand paper, 1 mu m diamond sand paper and 0.1 mu m diamond sand paper, and grinding and polishing after the first cutting surface contacts with the diamond sand paper by means of self gravity of the sample stage to obtain a primary grinding sample;
In the first section grinding and polishing process, when the first section to be sampled is contacted with the diamond abrasive paper and then ground and polished, the grinding and polishing rotating speed of the diamond abrasive paper is 15-30 rpm/min, and the thickness of a primary grinding sample after the grinding and polishing of the first section is 700 mu m; in the first section grinding and polishing process, the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the directions of scratches on diamond film particles on the first section are observed to be consistent, and the diamond abrasive paper of the next specification is replaced;
Fixing the second section on a sample stage, sequentially adopting 30 mu m diamond sand paper, 15 mu m diamond sand paper, 6 mu m diamond sand paper, 3 mu m diamond sand paper, 1 mu m diamond sand paper and 0.1 mu m diamond sand paper, and grinding and polishing after the second section contacts with the diamond sand paper by means of self gravity of the sample stage to obtain a section sample;
In the grinding and polishing process of the second section, when the second section to be sampled is contacted with the diamond abrasive paper and then is ground and polished, the grinding and polishing rotating speed is 15-20 rpm/min when the diamond abrasive paper with the diameter of 30 mu m is adopted for grinding and polishing; when 15 mu m diamond sand paper, 6 mu m diamond sand paper and 3 mu m diamond sand paper are adopted for grinding and polishing, the grinding and polishing rotating speeds are 10-15 rpm/min; when the 1 mu m diamond sand paper and the 0.1 mu m diamond sand paper are adopted for grinding and polishing, the grinding and polishing rotating speeds are 5-10 rpm/min; in the grinding and polishing process of the second section, the condition for replacing the diamond abrasive paper is that under a 100 times optical microscope, the direction of scratches left on diamond film particles on the first section is consistent, and the diamond abrasive paper of the next specification is replaced;
and simultaneously adopting an ion thinning instrument to thin the first section and the second section of the section sample to form a hole, enlarging a thin area of the section of the sample, and finally cleaning an amorphous layer to obtain the rare earth nickelate thin film section transmission sample.
2. The method for preparing a rare earth nickelate thin film section transmission sample according to claim 1, wherein in the second section grinding and polishing process, after grinding and polishing by using 30 μm diamond sand paper, the thickness of the section sample is 100 μm; sequentially adopting 15 mu m diamond sand paper, 6 mu m diamond sand paper and 3 mu m diamond sand paper for grinding and polishing, wherein the thickness of a section sample is 25 mu m; after polishing with 1 μm diamond coated abrasive and 0.1 μm diamond coated abrasive in this order, the thickness of the cross-sectional sample was 25. Mu.m.
3. The method for preparing a rare earth nickelate film section transmission sample according to claim 1, wherein when an ion thinning instrument is adopted for thinning to an outlet, the voltage of the ion thinning instrument is 4.5-6 kV, the angle of an ion beam emission target is +/-10 degrees, and the time is 60-90 min.
4. The method for preparing a rare earth nickelate thin film section transmission sample according to claim 1, wherein the voltage of an ion thinning instrument is 3-4 kV, the angle of an ion beam emission target is + -8 degrees, and the time is 20-30 min when the thin section of the sample is enlarged; and then changing the voltage of the ion thinning instrument to be 2-3 kV, wherein the angle of the ion beam emitting target is +/-5 degrees, and the time is 20-30 min.
5. The method for preparing a rare earth nickelate thin film cross-section transmission sample according to claim 1, wherein the voltage of the ion thinning instrument is 0.5-1 kV, the angle of the ion beam emission target is ±3°, and the time is 10-20 min when the amorphous layer is cleaned.
6. The method for preparing a rare earth nickelate thin film section transmission sample according to claim 1, wherein the temperature of the section sample is-40 ℃ to-70 ℃ when the ion thinning instrument is adopted for thinning.
7. The method for preparing a rare earth nickelate film section transmission sample according to claim 1, wherein the rare earth nickelate film is RNiO 3/LaAlO3 film or RNiO 3/Si film, and R is rare earth metal.
8. The preparation method of the rare earth nickelate film section transmission sample according to claim 1, which is characterized in that two surfaces of the initial cutting sample are adhered by adopting an adhesive, wherein the adhesive is prepared from G1 adhesive resin and a hardening agent according to the weight ratio of 10:1, and the curing temperature is 120 ℃ and the curing time is 30 min.
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