阅读说明：本技术 一种石墨烯xrd表征用样品的制样方法 (Sample preparation method of sample for graphene XRD (X-ray diffraction) characterization ) 是由 鲁娜 杨新伟 王秀娟 卢科伟 张丽娟 于 2019-10-10 设计创作，主要内容包括：本发明为一种石墨烯XRD表征用样品的制样方法。一种石墨烯XRD表征用样品的制样方法,A海绵状石墨烯：将海绵状石墨烯剪切成多个不同大小的样品,按照大小的顺序依次粘贴到样品台中心位置上,再反复轻压样品表面至平整；B粉末状石墨烯：准备带有凹槽的玻璃载片,将粉末状石墨烯填入凹槽中,填满后,再反复轻压样品表面至平整后；C膏状石墨烯：准备中心带有孔洞的玻璃载片,将膏状石墨烯填入到孔洞后,将样品表面多余的膏状石墨烯刮平。本发明所述的一种石墨烯XRD表征用样品的制样方法,该方法针对海绵状、粉末状、膏状的石墨烯样品,选用一定规格的样品台对样品进行合理的处理,有效地提高了谱图质量。(The invention relates to a sample preparation method of a sample for graphene XRD (X-ray diffraction) characterization. A sample preparation method of a sample for graphene XRD (X-ray diffraction) characterization comprises the following steps: cutting the spongy graphene into a plurality of samples with different sizes, sequentially adhering the samples to the center of a sample table according to the size sequence, and repeatedly and lightly pressing the surfaces of the samples to be flat; b, powdery graphene: preparing a glass slide with a groove, filling the groove with powdered graphene, and repeatedly slightly pressing the surface of the sample until the surface is flat after the groove is filled with the powdered graphene; c, paste graphene: preparing a glass slide with a hole in the center, filling the pasty graphene into the hole, and scraping the redundant pasty graphene on the surface of the sample. According to the sample preparation method for the graphene XRD (X-ray diffraction) characterization sample, a sample table with a certain specification is selected for sponge, powder and paste graphene samples to reasonably process the sample, and the spectrogram quality is effectively improved.)

1. A sample preparation method for a sample for graphene XRD (X-ray diffraction) characterization is characterized in that the state of graphene is spongy, powdery and pasty;

a sponge graphene:

cutting the spongy graphene into a plurality of samples with different sizes, sequentially adhering the samples to the center of a sample table according to the size sequence, and repeatedly slightly pressing the surface of the sample to be flat, so that XRD detection can be carried out;

b, powdery graphene:

preparing a glass slide with a groove, filling the groove with powdered graphene, and repeatedly slightly pressing the surface of the sample to be flat after filling the groove with the powdered graphene, so that XRD detection can be carried out;

c, paste graphene:

preparing a glass slide with a hole in the center, filling the pasty graphene into the hole, scraping the redundant pasty graphene on the surface of the sample, and carrying out XRD detection.

2. A sample preparation method as claimed in claim 1,

in the spongy graphene A, the sample platform is made of one of aluminum, iron and copper.

3. A sample preparation method as claimed in claim 1,

in the spongy graphene A, the sample platform is square, and 3-5 lines of double-sided adhesive tapes are parallelly stuck to the surface of the sample platform and used for fixing a sample.

4. A sample preparation method as claimed in claim 1,

in the spongy graphene A, the light pressing comprises the following specific steps: and (3) placing a clean 100g weight on the surface of the sample for 10-20s, then taking down, placing on the sample again, repeating for 3-5 times, and lightly pressing and flattening the surface of the sample.

5. A sample preparation method as claimed in claim 1,

in the B powder graphene, the light pressing comprises the following specific steps: and (3) placing a clean 100g weight on the surface of the sample for 10-20s, then taking down, placing on the sample again, repeating for 3-5 times, and lightly pressing and flattening the surface of the sample.

6. A sample preparation method as claimed in claim 1,

in the B powder graphene, the size of the groove of the glass slide is 2cm multiplied by 2cm, and the weight of the powder graphene filled in the groove is not more than 0.06 g.

7. A sample preparation method as claimed in claim 1,

and C, filling the pasty graphene into the holes, and dipping the pasty graphene by using filter paper if liquid flows out.

8. A sample preparation method as claimed in claim 1,

in the C paste graphene, the diameter of a central hole of the glass slide is 2cm, and the weight of the paste graphene filled in the central hole is not more than 0.08 g.

Technical Field

The invention belongs to the technical field of graphene materials, and particularly relates to a sample preparation method of a sample for graphene XRD (X-ray diffraction) characterization.

Background

The X-ray diffractometer is an important tool for identifying, analyzing and researching the microstructure (atomic scale magnitude) of a substance, and is a method for researching the structure of a material without damage. The relation between the unit cell parameter size of the substance, the atom arrangement in the unit cell and the material property thereof can be determined, and the phase content of the substance can be determined. The grain size, micro and macro stress, texture, orientation degree, crystallinity, intermetallic compound order degree and the like of the material can be measured. X-ray diffractometers are an indispensable method for substance characterization.

Graphene (Graphene) is a new material with a monolayer sheet structure composed of carbon atoms. The ideal graphene material has the excellent characteristics of high light transmittance, ultrahigh carrier mobility, high specific surface area, extremely high in-layer thermal conductivity, extremely high Young modulus and the like. The states, the number of layers and the structures of the graphene prepared by different processes are different, and how to effectively detect and analyze various samples is also important research work of new graphene materials.

The XRD characterization method is one of the main methods applied to graphene material characterization at present, the method can be used for analyzing the oxidation degree, the reduction degree, the interlayer spacing, the disorder degree and the defect condition of graphene, and researchers summarize characteristic spectrograms of various different graphene materials in recent years. For graphene and graphene oxide samples, because C, H, O light elements have weak absorption to X-rays, the X-rays can penetrate the samples deeply, when conventional diffraction measurement is performed, the angle position of the diffraction signal of the sample at a deeper position deviates toward a low-angle direction, the peak shape of a low-angle diffraction peak is asymmetric, the phenomenon of diffraction peak broadening is more serious, and the shape, surface, thickness, fineness and the like of the sample to be detected all affect the XRD detection result and the spectrogram quality of the graphene sample. In order to better analyze the graphene sample by using an XRD characterization method, XRD diffraction data should have higher accuracy, so that the influence of various errors is reduced as much as possible, and the interference of experimental conditions on the diffraction data is removed to obtain a high-quality diffraction spectrogram.

In order to ensure the accuracy of the XRD diffraction data of the graphene, a sample stage with a specific specification is selected to reasonably process a sample to be detected according to the state of the graphene. In view of the above, the present invention provides a novel sample preparation method for a sample for graphene XRD characterization.

Disclosure of Invention

The invention aims to provide a sample preparation method for a sample for graphene XRD (X-ray diffraction) characterization, which is used for reasonably processing a spongy, powdery and pasty graphene sample by selecting a sample table with a certain specification, and effectively improving the spectrogram quality.

In order to realize the purpose, the adopted technical scheme is as follows:

a sample preparation method for a sample for graphene XRD (X-ray diffraction) characterization is disclosed, wherein the state of graphene is spongy, powdery and pasty;

a sponge graphene:

cutting the spongy graphene into a plurality of samples with different sizes, sequentially adhering the samples to the center of a sample table according to the size sequence, and repeatedly slightly pressing the surface of the sample to be flat, so that XRD detection can be carried out;

b, powdery graphene:

preparing a glass slide with a groove, filling the groove with powdered graphene, and repeatedly slightly pressing the surface of the sample to be flat after filling the groove with the powdered graphene, so that XRD detection can be carried out;

c, paste graphene:

preparing a glass slide with a hole in the center, filling the pasty graphene into the hole, scraping the redundant pasty graphene on the surface of the sample, and carrying out XRD detection.

Further, in the sponge-like graphene A, the material of the sample stage is one of aluminum, iron and copper.

Further, in the spongy graphene A, the sample platform is square, and 3-5 lines of double-sided adhesive tape are parallelly attached to the surface of the sample platform and used for fixing the sample.

Further, in the sponge-like graphene a, the light pressing specifically comprises the following steps: and (3) placing a clean 100g weight on the surface of the sample for 10-20s, then taking down, placing on the sample again, repeating for 3-5 times, and lightly pressing and flattening the surface of the sample.

Further, in the B powder graphene, the light pressing specifically includes: and (3) placing a clean 100g weight on the surface of the sample for 10-20s, then taking down, placing on the sample again, repeating for 3-5 times, and lightly pressing and flattening the surface of the sample.

Furthermore, in the B powder graphene, the size of a groove of the glass slide is 2cm multiplied by 2cm, and the weight of the powder graphene filled in the groove is not more than 0.06 g.

Furthermore, in the C paste graphene, the paste graphene is filled into the holes, and if liquid flows out, the paste graphene is dipped by filter paper.

Furthermore, in the C paste graphene, the diameter of a central hole of the glass slide is 2cm, and the weight of the paste graphene filled in the central hole is not more than 0.08 g.

1. The method can be suitable for detecting the spongy graphene sample, the powdery graphene sample and the pasty graphene sample in different states.

2. According to the method, different types of graphene samples are processed by selecting a sample table with a certain specification, so that the quality of a spectrogram is improved, and the processing method is simple.

3. The sample processing process can realize standardized control, and the technical problem of detection result deviation caused by different operation technical levels of sample preparation personnel is solved. And the XRD characterization can be carried out on the graphene in various different states, the diffraction intensity value has better reproducibility, and the deviation of each detection result is reduced.

4. The method is simple to operate, and the graphene sample processing process can realize standardized control, so that the interference of the change of the detection condition on the diffraction data is reduced. The method can be suitable for monitoring the quality of different batches of products in the production process, and can also be suitable for analyzing the difference between parallel comparison samples in a laboratory and representing various different types of graphene samples.

Drawings

FIG. 1 is an XRD characterization of example 1;

FIG. 2 is an XRD characterization of example 2;

FIG. 3 is an XRD characterization of example 3;

figure 4 is an XRD characterization pattern of example 4.

Detailed Description

In order to further illustrate the sample preparation method for XRD characterization of graphene according to the present invention, and achieve the intended purpose of the invention, the following embodiments, structures, features and effects thereof will be described in detail. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.

The sample preparation method of the sample for graphene XRD characterization according to the present invention will be further described in detail with reference to the following specific examples:

the technical scheme of the invention is as follows:

a sponge graphene:

the spongy graphene is cut into a plurality of samples with different sizes, the samples are sequentially pasted to the center of the sample table according to the size sequence, and the surface of the sample is repeatedly lightly pressed until the sample is flat, so that XRD detection can be carried out.

Preferably, the material of the sample stage is one of aluminum, iron, copper and the like. The material of the sample stage can be selected from the materials with regular crystal structures of aluminum, iron, copper and the like, strong peak shapes and strong diffraction peaks, and the diffraction peaks are not overlapped with those of graphene, so that the penetration effect can be found in time, and the detection process can be better detected.

Preferably, the sample platform is square, and 3-5 lines of double-sided adhesive tapes are parallelly attached to the surface of the sample platform and used for fixing the sample.

Preferably, the light pressing comprises the following specific steps: and (3) placing a clean 100g weight on the surface of the sample for 10-20s, then taking down, placing on the sample again, repeating for 3-5 times, and lightly pressing and flattening the surface of the sample. According to the invention, the weight is used for flattening, so that the process is standardized, the interference can be reduced, the deviation of each detection can be reduced, the repeatability of the detection result can be improved, and the technical problem that the detection result has deviation due to different operation technical levels of a sample preparation worker can be avoided.

B, powdery graphene:

preparing a glass slide with a groove, filling the groove with the powdery graphene, and after the groove is filled with the powdery graphene, repeatedly slightly pressing the surface of the sample to be flat, and then carrying out XRD detection.

Preferably, the light pressing comprises the following specific steps: and (3) placing a clean 100g weight on the surface of the sample for 10-20s, then taking down, placing on the sample again, repeating for 3-5 times, and lightly pressing and flattening the surface of the sample. According to the invention, the weight is used for flattening, so that the process is standardized, the interference can be reduced, the deviation of each detection can be reduced, the repeatability of the detection result can be improved, and the technical problem that the detection result has deviation due to different operation technical levels of a sample preparation worker can be avoided.

Preferably, in the B powder graphene, the size of the groove of the glass slide is 2cm multiplied by 2cm, and the weight of the powder graphene filled in the groove is not more than 0.06 g. By limiting the size of the groove and the weight of the sample filled into the groove, the influence of excessive sample density on diffraction data is avoided.

C, paste graphene:

preparing a glass slide with a hole in the center, filling the pasty graphene into the hole, scraping the redundant pasty graphene on the surface of the sample, and carrying out XRD detection.

Preferably, the pasty graphene is filled into the hole, and if liquid flows out, the pasty graphene is dipped by using filter paper.

Preferably, in the C paste graphene, the diameter of a central hole of the glass slide is 2cm, and the weight of the paste graphene filled in the central hole is not more than 0.08 g. At the size, when the weight of a sample exceeds 0.08g, a steamed bun peak appears in a map, and nothing can be detected.