CN112557496B - Preparation method and application of needle-shaped sample for glow discharge mass spectrum detection - Google Patents
Preparation method and application of needle-shaped sample for glow discharge mass spectrum detection Download PDFInfo
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- CN112557496B CN112557496B CN202011317495.2A CN202011317495A CN112557496B CN 112557496 B CN112557496 B CN 112557496B CN 202011317495 A CN202011317495 A CN 202011317495A CN 112557496 B CN112557496 B CN 112557496B
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- 238000001514 detection method Methods 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000001819 mass spectrum Methods 0.000 title abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 57
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 47
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000004020 conductor Substances 0.000 claims abstract description 6
- 239000004065 semiconductor Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 21
- 238000001036 glow-discharge mass spectrometry Methods 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 230000003749 cleanliness Effects 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 9
- 229910017604 nitric acid Inorganic materials 0.000 description 9
- 238000005406 washing Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 238000005201 scrubbing Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000126 substance Substances 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
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Toxicology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a preparation method and application of a needle-shaped sample for glow discharge mass spectrum detection, and belongs to the technical field of analysis and detection. According to the invention, liquid gallium is injected into the needle-shaped sample rack, then a sample to be detected is inserted into the liquid gallium, then the sample rack is inserted into liquid nitrogen for cooling, after the liquid gallium is solidified, the sample rack is taken out, and the needle-shaped sample is obtained, so that the obtained needle-shaped sample has a good cooling effect when being used for detecting a glow discharge mass spectrum, the sample can be prevented from melting when detecting a low-melting-point sample, and meanwhile, the size range of the sample which can be detected by the glow discharge mass spectrum is widened, and conductors and semiconductors with the size of 0-3 mm multiplied by 8-22mm can be directly measured.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, and particularly relates to a preparation method and application of a needle-shaped sample for glow discharge mass spectrum detection.
Background
In recent decades, glow discharge mass spectrometry has become the most common technique for analyzing trace or ultra-trace impurities in high purity materials. The current commercial glow discharge mass spectrometers are equipped with needle-shaped and sheet-shaped sample cells, so that conductor and semiconductor samples meeting the size requirements can be directly measured, such as an Astrum type glow discharge mass spectrometer manufactured by Nu Instruments Ltd, and a sheet-shaped sample of 12-40X 1-20mm and a needle-shaped sample of 0.5-3X 18-22mm can be directly measured. In the actual detection, different detection methods can be selected according to the types of the samples and the detection requirements. However, during sheet detection, more C, N, O pollution is introduced due to larger contact area between the sample holder and the sample cell, so that larger interference is formed on detection of some elements, the contact area between the needle-shaped sample holder and the sample cell is smaller, the pollution of C, N, O is smaller, and smaller C, N, O value can be obtained, so that the interference on detection of many elements is also smaller. Meanwhile, in the application of high-purity products, the requirements on C, N, O are higher and higher, the detection limit of an infrared gas analyzer is difficult to meet the requirements, a glow discharge mass spectrometer becomes an effective detection means of C, N, O in the future, and needle detection is a preferred method for measuring C, N, O. However, because the contact area between the needle-shaped sample rack and the sample cell is small, and the outlet of the needle-shaped sample rack is circular, for some non-cylindrical or small-size samples, the temperature is reduced mainly by two screws on the bracket, so that the cooling effect is not very good, and the tip of the sample is easy to melt when measuring samples of some low-melting metals (such as Ga, cd, te and the like); in addition, the method is suitable for measuring rod-shaped samples with the length of 18mm-22mm, and samples with shorter lengths can not be directly measured.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method and application of a needle-shaped sample for glow discharge mass spectrometry detection, so that the sample has a better cooling effect when the glow discharge mass spectrometry detection is carried out, the sample is prevented from melting when the sample with a low melting point is detected, and meanwhile, the sample with a shorter length can be directly measured, and the size range of the sample is widened.
To achieve the above object, in a first aspect, the present invention provides a method for preparing a needle-like sample for glow discharge mass spectrometry detection, comprising the following preparation steps:
(1) After liquid gallium (namely gallium simple substance, ga) is injected into the needle-shaped sample rack, a sample to be tested is inserted into the liquid gallium;
(2) And inserting the sample frame into liquid nitrogen, preventing the liquid nitrogen from immersing the sample frame, and taking out the sample frame after the liquid gallium is solidified to obtain the needle-shaped sample.
According to the preparation method, the gallium is injected into the needle-shaped sample frame, and the sample to be detected is inserted into the gallium, so that the sample to be detected and the gallium are bonded together, the needle-shaped sample can be fully contacted with the needle-shaped sample frame, the heat conduction efficiency between the sample to be detected and the sample frame is improved, the sample to be detected has a good cooling effect, and the sample can be prevented from being melted when the sample with a low melting point (such as Ga, cd, te and the like) is detected; meanwhile, the preparation method widens the size range of a sample which can be detected by glow discharge mass spectrometry, and can directly measure conductors and semiconductors with the size of 0-3 mm multiplied by 8-22 mm. In addition, when the sample rack is inserted into liquid nitrogen for cooling, the liquid nitrogen is prevented from immersing the sample rack so as to avoid sample pollution and oxidation.
Preferably, the volume of the liquid gallium is 0.07-0.09 mL. More preferably, the liquid gallium has a volume of 0.08mL. When the volume of the liquid gallium is 0.07-0.09 mL, the sample and the liquid gallium can be ensured to be bonded together, and meanwhile, the gallium cannot overflow the sample frame, and particularly when the volume of the liquid gallium is 0.08mL, the sample and the liquid gallium can be better bonded together, and meanwhile, the gallium cannot overflow the sample frame.
Preferably, the size of the sample to be measured is 0-3 mm×0-3 mm×8-22 mm. In the present text, 0 to 3mm×0 to 3mm×8 to 22mm, 0 to 3mm does not include both ends, and 8 to 22mm includes both ends. If the sample to be measured is cylindrical, the size ranges are: the diameter is smaller than 3mm, and the length is 8-22 mm.
Preferably, the purity of the liquid gallium is greater than or equal to 99.9999wt%.
Preferably, the liquid gallium is prevented from flowing out of the outlet of the sample holder when the sample to be measured is inserted into the liquid gallium. If liquid gallium flows out from the outlet of the sample holder, the tightness is poor and short circuit can occur during glow discharge mass spectrum detection.
Preferably, the preparation method is completed in an environment with cleanliness of hundred or more.
Preferably, before the step (1), the needle-shaped sample holder is scrubbed with hydrofluoric acid, then washed clean with pure water, then heated in acid, then washed clean with pure water and dried.
Preferably, the needle-like sample is placed in an acid for heating, and the acid is a mixture of nitric acid and hydrochloric acid.
Preferably, the volume ratio of the nitric acid to the hydrochloric acid is nitric acid: hydrochloric acid=1:3.
Preferably, the sample to be tested is a high-purity metal conductor or semiconductor.
In a second aspect, the invention provides a method for detecting needle-shaped samples by using glow discharge mass spectrometry, wherein a sample frame with needle-shaped samples obtained by the preparation method is arranged in a sample cell of a glow discharge mass spectrometer, and the sample cell is cooled by liquid nitrogen and then subjected to direct current glow discharge mass spectrometry detection.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the gallium is injected into the needle-shaped sample frame, and the sample to be detected is inserted into the gallium, so that the sample to be detected and the gallium are bonded together, the heat conduction efficiency between the sample to be detected and the sample frame is improved, the sample to be detected has a good cooling effect, and the sample can be prevented from being melted when the sample with a low melting point (such as Ga, cd, te and the like) is detected; meanwhile, the size range of a sample which can be detected by glow discharge mass spectrum is widened, and conductors and semiconductors with the size of 0-3 mm multiplied by 8-22mm can be directly measured.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The embodiment provides a preparation method of a needle-shaped sample for glow discharge mass spectrum detection. The preparation method of the needle-shaped sample for glow discharge mass spectrum detection in the embodiment comprises the following steps:
(1) Scrubbing a needle-shaped sample frame with hydrofluoric acid once, washing with pure water, heating in mixed acid of nitric acid and hydrochloric acid (the volume ratio of nitric acid to hydrochloric acid is 1:3) for 30min, washing with pure water for 2-3 times, and drying in a hundred-grade clean bench;
(2) 0.08mL of liquid gallium (purity 99.9999 wt%) was injected into the needle-like sample holder, and then a gallium sample (i.e., ga, specification Φ2.5 x 22 mm) was inserted into the liquid gallium;
(3) And clamping the sample frame by using polytetrafluoroethylene forceps, inserting the sample frame into a liquid nitrogen cup filled with liquid nitrogen, keeping a sample port of the sample frame above the liquid nitrogen liquid level, and taking out the sample frame after the liquid gallium is solidified to obtain the needle-shaped sample.
The sample holder with the needle-shaped sample obtained by the preparation method is placed into a sample cell of a glow discharge mass spectrometer (the sample cell is cooled by liquid nitrogen), after the sample is cooled for 5min, the sample is subjected to direct current glow discharge mass spectrometry detection under the set glow discharge parameters, the needle-shaped sample is not melted in the detection process, and the detection result is shown in table 1.
TABLE 1 detection results of gallium samples
As shown in Table 1, after 40min of sputtering, the contamination on the surface of the sample to be tested was eliminated, and the relative standard deviation (RSD/%) of the characteristic elements was within 10%, which indicates that the detection had good reproducibility.
Example 2
The embodiment provides a preparation method of a needle-shaped sample for glow discharge mass spectrum detection. The preparation method of the needle-shaped sample for glow discharge mass spectrum detection in the embodiment comprises the following steps:
(1) Scrubbing a needle-shaped sample frame with hydrofluoric acid once, washing with pure water, heating in mixed acid of nitric acid and hydrochloric acid (the volume ratio of nitric acid to hydrochloric acid is 1:3) for 30min, washing with pure water for 2-3 times, and drying in a hundred-grade clean bench;
(2) 0.08mL of liquid gallium (purity 99.9999 wt%) was injected into the needle-like sample holder, and then tellurium sample (i.e. Te, specification 2mm x 18 mm) was inserted into the liquid gallium;
(3) And clamping the sample frame by using polytetrafluoroethylene forceps, inserting the sample frame into a liquid nitrogen cup filled with liquid nitrogen, keeping a sample port of the sample frame above the liquid nitrogen liquid level, and taking out the sample frame after the liquid gallium is solidified to obtain the needle-shaped sample.
The sample holder with the needle-shaped sample obtained by the preparation method is placed into a sample cell of a glow discharge mass spectrometer (the sample cell is cooled by liquid nitrogen), after the sample is cooled for 5min, the sample is subjected to direct current glow discharge mass spectrometry detection under the set glow discharge parameters, the needle-shaped sample is not melted in the detection process, and the detection result is shown in table 2.
TABLE 2 detection results of tellurium samples
As shown in Table 2, after 40min of sputtering, the contamination on the surface of the sample to be tested was eliminated, and the relative standard deviation (RSD/%) of the characteristic elements was within 20%, which indicates that the detection had good reproducibility.
Example 3
The embodiment provides a preparation method of a needle-shaped sample for glow discharge mass spectrum detection. The preparation method of the needle-shaped sample for glow discharge mass spectrum detection in the embodiment comprises the following steps:
(1) Scrubbing a needle-shaped sample frame with hydrofluoric acid once, washing with pure water, heating in mixed acid of nitric acid and hydrochloric acid (the volume ratio of nitric acid to hydrochloric acid is 1:3) for 30min, washing with pure water for 2-3 times, and drying in a hundred-grade clean bench;
(2) 0.08mL of liquid gallium (purity 99.9999 wt%) was injected into the needle-like sample holder, and then an antimony sample (i.e., sb, 1mm x 2mm x 8mm in specification) was inserted into the liquid gallium;
(3) And clamping the sample frame by using polytetrafluoroethylene forceps, inserting the sample frame into a liquid nitrogen cup filled with liquid nitrogen, keeping a sample port of the sample frame above the liquid nitrogen liquid level, and taking out the sample frame after the liquid gallium is solidified to obtain the needle-shaped sample.
The sample holder with the needle-shaped sample obtained by the preparation method is placed into a sample cell of a glow discharge mass spectrometer (the sample cell is cooled by liquid nitrogen), after the sample is cooled for 5min, the sample is subjected to direct current glow discharge mass spectrum detection under the set glow discharge parameters, the needle-shaped sample is not melted in the detection process, and the detection result is shown in table 3.
TABLE 3 detection results of antimony samples
As shown in Table 3, after 50min of sputtering, the contamination on the surface of the sample to be tested was eliminated, and the relative standard deviation (RSD/%) of the characteristic elements was within 20%, which indicates that the detection had good reproducibility.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. A method for preparing a needle-like sample for glow discharge mass spectrometry detection, the method comprising the steps of:
(1) After liquid gallium is injected into the needle-shaped sample rack, a sample to be tested is inserted into the liquid gallium;
(2) And inserting the sample frame into liquid nitrogen, preventing the liquid nitrogen from immersing the sample frame, and taking out the sample frame after the liquid gallium is solidified to obtain the needle-shaped sample.
2. The method according to claim 1, wherein the volume of the liquid gallium is 0.07 to 0.09mL.
3. The method of claim 2, wherein the liquid gallium has a volume of 0.08mL.
4. The method according to claim 1, wherein the sample to be measured has a size of a x b x c, wherein 0 < a < 3mm,0 < b < 3mm,8 mm.ltoreq.c.ltoreq.22 mm.
5. The method of claim 1, wherein the liquid gallium has a purity of 99.9999wt% or more.
6. The method of claim 1, wherein the liquid gallium is prevented from flowing out of the outlet of the sample holder when the sample to be measured is inserted into the liquid gallium.
7. The method of claim 1, wherein the method is performed in an environment of greater than hundred degrees of cleanliness.
8. The method according to claim 1, wherein the needle-like sample holder is scrubbed with hydrofluoric acid, rinsed with pure water, heated in acid, rinsed with pure water and dried before the step (1).
9. The method according to claim 1, wherein the sample to be measured is a high-purity metal conductor or semiconductor.
10. A method for detecting needle-like samples using glow discharge mass spectrometry, the method comprising the steps of: loading a sample holder containing a needle-like sample obtained by the preparation method according to any one of claims 1 to 9 into a sample cell of a glow discharge mass spectrometer, cooling the sample cell with liquid nitrogen, and performing direct current glow discharge mass spectrometry detection.
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