Preparation method of powder sample of X-ray photoelectron spectrometer

Abstract

The invention discloses a method for preparing a powder sample of an X-ray photoelectron spectrometer, and relates to the technical field of X-ray photoelectron spectrometers, which comprises the following steps of: weighing a powder sample to be detected, putting the powder sample into a crucible, and then putting the crucible filled with the powder sample into a drying box for drying treatment; the method comprises the following steps: putting a sample and spectroscopically pure into an agate grinding body, fully grinding and uniformly mixing, sieving for later use after grinding, weighing the sieved powder, and dividing into a plurality of equal parts; preparing a tabletting mold, placing a powder sample in the tabletting mold, and grinding and uniformly mixing the sample again through an upper mold; according to the method disclosed by the invention, the spectral purity is proportionally added into the powder sample, so that the number display intensity of the powder sample during detection can be improved, and the final detection effect is further improved; according to the invention, the sample is sheeted by using the pressing machine, so that the stability of the formed sample can be improved, the loosening phenomenon in the transfer and detection process can be avoided, and meanwhile, the flatness of the surface of the sample can be ensured, so that the accuracy of detection data can be ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of X-ray photoelectron spectrometers, in particular to a method for preparing powder samples for X-ray photoelectron spectrometers. Background Art

[0002] An X-ray photoelectron spectrometer (XPS) uses X-rays to excite photoelectrons from a sample, which are then received by a specific detector to obtain an electron energy spectrum. Currently, the mainstream X-ray photoelectron spectrometer technology consists of a hemispherical energy analyzer and an oblique-incidence monochromatized X-ray source. Energy spectrum analysis is a commonly used compositional analysis method, capable of performing qualitative and semi-quantitative elemental analysis on solid samples. It has wide applications in fields such as metallurgy, materials science, biology and medicine, forensic identification, mineralogical identification, and geological systems research. Energy spectrum analysis requires a small sample volume and requires the sample to be as flat as possible to obtain accurate data. When analyzing the composition of powdered samples without sample preparation, especially when the distribution of the components being tested is uneven, it is impossible to accurately determine the overall sample composition. Therefore, powder sample preparation is a prerequisite for obtaining accurate energy spectrum analysis results.

[0003] After searching, the patent with announcement number CN 116337906 A: A method for preparing powder samples for X-ray photoelectron spectrometer, including the following steps: S1: first spray alcohol on the glass table top, take a piece of aluminum foil or copper foil and spread it flat on the glass table top; S2: spray alcohol on the surface of the aluminum foil or copper foil, and scrape it flat with a scraper; S3: take a four-sided film maker, select the coating thickness and place it, use a magnetic stirrer to stir the sample, and after stirring, add it into the film maker together with the aluminum foil or copper foil, and move in one direction; S4: complete the preparation of a film layer sample with a fixed thickness. Different from the conventional preparation method, it can prepare samples with a smoother surface and fixed thickness, can perform corresponding operations for different sample preparations, and improve preparation efficiency. It can reduce the situation of preparing multiple samples at the same time and reduce the possibility of cross-infection. In addition, after magnetic stirring, the sample is more uniform and the surface of the prepared sample is smoother.

[0004] However, the above method does not press the powder sample into tablets. Although the scraper-smearing method is efficient, the powder material is still in a relatively loose state, and there is instability during the detection or transfer process, which in turn affects the final detection results. For this reason, the present application proposes a method for preparing powder samples for X-ray photoelectron spectrometer. Summary of the Invention

[0005] In response to the above problems, the present invention provides a method for preparing powder samples for X-ray photoelectron spectrometer. By adding spectrally pure substances in a certain proportion, the numerical display intensity of the powder samples during detection can be improved. The samples are tableted using a press to improve their stability after forming, thereby solving the problems mentioned in the background technology.

[0006] The technical solution of the present invention is:

[0007] A method for preparing powder samples for an X-ray photoelectron spectrometer comprises the following steps:

[0008] S1. Weigh the powder sample to be tested and place it in a crucible, then place the crucible containing the powder sample in a drying oven for drying;

[0009] S2. Grind the sample and spectrally pure material into an agate mortar and grind them thoroughly. After grinding, sieve the powder for later use. Then weigh the sieved powder and divide it into multiple equal portions.

[0010] S3. Prepare a tableting mold, place a portion of the powder sample in the tableting mold, and grind and mix the sample again using the upper mold;

[0011] S4. Place the mold into the tablet press and press to the set pressure value, and maintain the pressure for a period of time;

[0012] S5. Take the mold out of the press, separate the upper and lower molds, take out the solid powder sample after tableting, measure the flatness of the outer surface of the solid sample, and store it for future use after the flatness is qualified.

[0013] In a further technical solution, the drying time of the powder sample to be tested in step S1 is 10-12 minutes, and the drying temperature is 105-110°C.

[0014] In a further technical solution, the ratio of the sample to the spectrally pure sample in step S2 is 20:1.

[0015] In a further technical solution, the mesh size of the sieve used to sieve the powder sample in step S2 is 2000 mesh.

[0016] In a further technical solution, the weight of each powder sample in step S2 is 2 g, and the error range is ±0.1 g.

[0017] In a further technical solution, the pressure value for pressing the mold in step S4 is 7-8 tons, and the holding time is 1-2 minutes.

[0018] In a further technical solution, the flatness of the outer surface of the solid sample in step S5 is 1-10 μm.

[0019] The beneficial effects of the present invention are:

[0020] 1. By adding spectrally pure chlorinated paraffin into the powder sample, the numerical display intensity of the powder sample during detection can be increased, thereby improving the final detection effect;

[0021] 2. By using a press to press the sample, its stability after forming can be improved, avoiding loosening during transfer and testing. At the same time, the flatness of the surface can be ensured to ensure the accuracy of the test data. DETAILED DESCRIPTION

[0022] The embodiments of the present invention are further described below.

[0023] Example 1:

[0024] A method for preparing powder samples for an X-ray photoelectron spectrometer comprises the following steps:

[0025] S1. Weigh the powder sample to be tested and place it in a crucible, then place the crucible containing the powder sample in a drying oven for drying;

[0026] S2. Grind the sample and spectrally pure material into an agate mortar and grind them thoroughly. After grinding, sieve the powder for later use. Then weigh the sieved powder and divide it into multiple equal portions.

[0027] S3. Prepare a tableting mold, place a portion of the powder sample in the tableting mold, and grind and mix the sample again using the upper mold;

[0028] S4. Place the mold into the tablet press and press to the set pressure value, and maintain the pressure for a period of time;

[0029] S5. Remove the mold from the press, separate the upper and lower molds, take out the solid powder sample after tableting, measure the flatness of the outer surface of the solid sample, and store it for future use after the flatness is qualified;

[0030] By adding spectrally pure substances into the powder sample, the numerical display intensity of the powder sample during detection can be increased, thereby improving the final detection effect; by using a press to make the sample into tablets, the stability after molding can be improved, avoiding loosening during transfer and detection, and at the same time ensuring the flatness of the surface to ensure the accuracy of the detection data.

[0031] Wherein, in step S1, the drying time of the powder sample to be tested is 10-12 minutes, and the drying temperature is 105-110°C.

[0032] Wherein, the ratio of the sample to the spectrally pure sample in step S2 is 20:1.

[0033] Wherein, the mesh size of the sieve used to sieve the powder sample in step S2 is 2000 mesh.

[0034] The weight of each powder sample in step S2 is 2 g, and the error range is ±0.1 g.

[0035] The pressure applied to the mold in step S4 is 7-8 tons, and the holding time is 1-2 minutes.

[0036] Wherein, the flatness of the outer surface of the solid sample in step S5 is 1-10 μm.

[0037] Example 2:

[0038] Select glucosamine hydrochloride as raw material:

[0039] S1. Weigh the glucosamine hydrochloride to be tested and place it in a crucible. Then, place the crucible containing the glucosamine hydrochloride in a drying oven for drying. Set the drying temperature to 105° C. and the drying time to 10 minutes.

[0040] S2. Glucosamine hydrochloride and spectrally pure glucosamine hydrochloride were placed in an agate mortar and ground thoroughly. After grinding, the mixture was sieved through a 2000-mesh sieve for later use. The sieved glucosamine hydrochloride was then weighed and divided into multiple portions of 2 ± 0.1 g;

[0041] S3. Prepare a tableting mold, place one portion of glucosamine hydrochloride in the tableting mold, and grind and mix the glucosamine hydrochloride and spectrally pure glucosamine hydrochloride again through the upper mold;

[0042] S4. Place the mold into the tablet press and press to 8 tons, and maintain the pressure for 1 minute;

[0043] S5. Take out the mold from the pressing machine, separate the upper and lower molds, take out the solid glucosamine hydrochloride sample after tableting, and measure the flatness of the outer surface of the solid glucosamine hydrochloride sample. The flatness is qualified if it is between 1-10 μm.

[0044] Example 3:

[0045] Select glucosamine sulfate potassium salt as raw material:

[0046] S1. Weigh the glucosamine sulfate potassium salt to be tested and place it in a crucible. Then, place the crucible containing the glucosamine sulfate potassium salt in a drying oven for drying. Set the drying temperature to 110° C. and the drying time to 12 minutes.

[0047] S2. Grind glucosamine sulfate potassium salt and spectrally pure glucosamine sulfate potassium salt thoroughly in an agate mortar and grind to mix. After grinding, sieve the mixture through a 2000-mesh sieve for later use. Weigh the sieved glucosamine sulfate potassium salt and divide it into equal portions of 2 ± 0.1 g.

[0048] S3. Prepare a tableting mold, place a portion of glucosamine sulfate potassium salt in the tableting mold, and grind and mix the glucosamine sulfate potassium salt and spectrally pure glucosamine sulfate potassium salt again through the upper mold;

[0049] S4. Place the mold into the tablet press and press to 7 tons, and maintain the pressure for 2 minutes;

[0050] S5. Remove the mold from the pressing machine, separate the upper and lower molds, take out the pressed solid glucosamine sulfate potassium salt sample, and measure the flatness of the outer surface of the solid glucosamine sulfate potassium salt sample. The flatness is qualified if it is between 1-10 μm.

[0051] The above-described embodiments merely represent specific implementations of the present invention. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, and all such variations and improvements fall within the scope of protection of the present invention.

Claims

1. A method for preparing powder samples for X-ray photoelectron spectrometry, characterized in that: The following steps are involved: S1. Weigh the powder sample to be tested and place it in a crucible, then place the crucible containing the powder sample in a drying oven for drying; S2. Grind the sample and spectrally pure material into an agate mortar and grind them thoroughly. After grinding, sieve the powder for later use. Then weigh the sieved powder and divide it into multiple equal portions. S3. Prepare a tableting mold, place a portion of the powder sample in the tableting mold, and grind and mix the sample again using the upper mold; S4. Place the mold into the tablet press and press to the set pressure value, and maintain the pressure for a period of time; S5. Take the mold out of the press, separate the upper and lower molds, take out the solid powder sample after tableting, measure the flatness of the outer surface of the solid sample, and store it for future use after the flatness is qualified.

2. The method for preparing powder samples for X-ray photoelectron spectrometry according to claim 1, wherein: In step S1, the drying time of the powder sample to be tested is 10-12 minutes, and the drying temperature is 105-110°C.

3. The method for preparing powder samples for X-ray photoelectron spectrometry according to claim 1, wherein: The ratio of the sample to the spectrally pure sample in step S2 is 20:

1.

4. The method for preparing powder samples for X-ray photoelectron spectrometry according to claim 1, wherein: The mesh size of the sieve used to sieve the powder sample in step S2 is 2000 mesh.

5. The method for preparing powder samples for X-ray photoelectron spectrometer according to claim 1, characterized in that: The weight of each powder sample in step S2 is 2 g, and the error range is ±0.1 g.

6. The method for preparing powder samples for X-ray photoelectron spectrometry according to claim 1, wherein: The pressure value of pressing the mold in step S4 is 7-8 tons, and the holding time is 1-2 minutes.

7. The method for preparing powder samples for X-ray photoelectron spectrometry according to claim 1, characterized in that: In step S5, the flatness of the outer surface of the solid sample is 1-10 μm.