CN114112602B - Pre-detection treatment method for small amount of fragile sample for ELEMENT GD glow discharge mass spectrum detection - Google Patents
Pre-detection treatment method for small amount of fragile sample for ELEMENT GD glow discharge mass spectrum detection Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001514 detection method Methods 0.000 title claims abstract description 16
- 238000001819 mass spectrum Methods 0.000 title description 2
- 238000005520 cutting process Methods 0.000 claims abstract description 33
- 239000010453 quartz Substances 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000012360 testing method Methods 0.000 claims abstract description 23
- 238000001036 glow-discharge mass spectrometry Methods 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000012459 cleaning agent Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 229910002804 graphite Inorganic materials 0.000 claims description 22
- 239000010439 graphite Substances 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000002203 pretreatment Methods 0.000 claims description 7
- 229910003460 diamond Inorganic materials 0.000 claims description 6
- 239000010432 diamond Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000002826 coolant Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 5
- 238000004140 cleaning Methods 0.000 abstract description 6
- 238000010309 melting process Methods 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 20
- 229910052710 silicon Inorganic materials 0.000 description 20
- 239000010703 silicon Substances 0.000 description 20
- 229910052714 tellurium Inorganic materials 0.000 description 10
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 10
- 235000012431 wafers Nutrition 0.000 description 9
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 8
- 229910052711 selenium Inorganic materials 0.000 description 8
- 239000011669 selenium Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009715 pressure infiltration Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000004544 sputter deposition 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
-
- 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
- G01N27/68—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 electric discharge to ionise a gas
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- Chemical & Material Sciences (AREA)
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- Physics & Mathematics (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a pre-testing treatment method for a small amount of fragile samples for ELEMENT GD glow discharge mass spectrometry detection, which comprises the steps of firstly ultrasonically cleaning the samples to be tested, drying the samples by using gas, then selecting a crucible for melting, introducing inert gas into a quartz tube during the melting process to prevent oxidization, ensuring that the temperature is higher than the melting point temperature of the samples to be tested, fully melting and stopping heating, naturally cooling under the protection of the inert gas, cutting off the parts of the crucible higher than the samples to be tested by using a wire cutting machine, ensuring that the outer wall of the crucible is not higher than the top surface of the samples to be tested, and cleanly treating the surfaces of the samples to be tested by using a cleaning agent and drying the samples to be tested.
Description
Technical Field
The invention belongs to the field of high-purity metal component analysis, and particularly relates to a pretreatment method for detecting a small amount of fragile samples for ELEMENT GD glow discharge mass spectrometry.
Background
The glow discharge mass spectrometry is a method capable of directly injecting solid sample, and utilizing the difference of mass-to-charge ratios and response signals of different elements in the sample to perform qualitative and quantitative analysis on the sample to be detected, is generally used for detecting trace impurities in high-purity materials/metals and grading the purity, and has the advantages of high sensitivity, low detection limit, small matrix effect and the like.
ELEMENT GD is a glow discharge mass spectrometer developed by the company of the United states of America, and is widely applied to the mechanisms of various enterprises, universities, scientific research institutions and the like for carrying out glow discharge mass spectrometry detection of high-purity samples, but the instrument has strict requirements on the size of the samples, the diameter of a solid sample testing surface is required to be 20 mm-50 mm, the thickness is required to be 5-40 mm, and the upper surface and the lower surface of the sample to be tested are required to be flat and parallel because the sample needs to be fixed by a clamp holder with a specific shape. For fragile samples with small amounts (such as silicon, tellurium and selenium, which are brittle in texture), in the process of direct fixation by using holders (the shape is shown as reference numeral 13 in fig. 1), the sample becomes a thin sheet, and the acting force between the holders directly acts on the sample to be tested, so that the probability of cracking is improved, and the normal test cannot be performed. The traditional processing method is a pressure infiltration method, namely, a sample to be tested is ground into powder, the powder is pressed into another high-purity metal (generally indium and tantalum) with softer texture under pressure, the impurity signals in the high-purity metal are subtracted during testing, the test result of the sample to be tested can be obtained, and the granularity of the sample, the selection of the high-purity metal and the pressure of high-purity gas can have larger influence on the test result, so that the operation is complex and the difficulty is larger.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a pre-test treatment method for a small amount of fragile samples for ELEMENT GD glow discharge mass spectrometry detection, which can easily solve the problems that the fragile samples with small amount are difficult to prepare and the samples are easy to crack to cause unstable, cutoff and incapability of normal test of test signals in the test process of using a ELEMENTGD glow discharge mass spectrometer, reduce the sample preparation difficulty and the detection difficulty of the samples, and improve the success rate and the accuracy of the test.
The technical scheme of the method is as follows: firstly, ultrasonically cleaning a sample to be tested, drying by using gas, and selecting a crucible with a proper size for melting according to the mass of the sample; the melting process is carried out under the protection of inert gas, the pressure is atmospheric pressure, the temperature is higher than the melting point temperature of a sample to be detected, the melting process is ensured to be fully melted and stopped heating, and natural cooling is carried out under the protection of inert gas; after cooling, cutting off the part of the crucible higher than the sample to be tested by using a wire cutting machine, so that the outer wall of the crucible is not higher than the top surface of the sample to be tested, and using a cleaning agent to clean the surface of the sample to be tested and blow-drying the sample to be tested, thus obtaining the sample meeting the test requirement.
The specific steps of the invention are as follows:
(1) Placing a sample to be tested in deionized water for ultrasonic cleaning to avoid introducing impurities, blowing the cleaned sample by using gas, wiping the inside and outside of a crucible by using absolute ethyl alcohol, and blowing the cleaned sample by using gas;
(2) Placing the sample to be tested treated in the step (1) in the crucible treated in the step (1), placing the crucible filled with the sample to be tested in a quartz tube, introducing inert gas into the quartz tube to discharge residual air in the tube, and then placing the quartz tube filled with the crucible in an electric furnace for heating and preserving heat;
(3) After the heat preservation is finished, the electric furnace is closed, the quartz tube is taken out, and after the quartz tube is naturally cooled, the crucible in the tube is taken out;
(4) Cutting off the crucible wall part of the crucible which is higher than the surface of the sample to be measured in the crucible after the crucible is taken out in the step (3) by using a linear cutting machine and using deionized water as a cutting coolant;
(5) And (3) wiping the surface of the sample to be tested in the crucible cut in the step (4) clean, and drying by using gas to obtain the sample to be tested meeting the test requirement.
Preferably, the gas in the step (1) and the step (5) is argon, nitrogen or compressed air.
Preferably, the crucible is made of high-purity graphite, polished inside and outside, is of a cylindrical structure, has an inner diameter of 23-30 mm and a wall thickness of 2-5 mm, and is 5-10 mm high.
Preferably, the inert gas in the step (2) is high-purity argon or high-purity nitrogen.
Preferably, in the step (2), heating is performed to a temperature 10-40 ℃ higher than the melting point of the sample to be detected, and the temperature is kept for 10-40 min.
Preferably, the cutting line of the wire cutting machine in the step (4) is a diamond wire.
Preferably, in step (5), absorbent cotton or dust-free paper/cloth is used as a wiper and is dipped in absolute ethanol or deionized water as a cleaning agent for wiping.
The invention is characterized in that: according to the invention, the fragile sample to be measured is tightly combined with the crucible in a melting material mode, when the crucible with the sample to be measured is processed by the invention and is fixed between ELEMENT GD clamping devices, most of extrusion force between the clamping devices acts on the crucible wall, so that the problem that the sample cannot be tested due to the fact that the sample is directly clamped between the clamping devices and the extrusion force between the clamping devices directly acts on the sample to be measured in the traditional sample measurement process is avoided; the invention also provides a sample pre-measurement treatment method when the number of samples to be measured is small, so that the problem that the clamp is damaged due to the fact that the samples to be measured are thin and the GDMS sputtering times break down the samples to be measured is avoided.
The beneficial effects of the invention are as follows:
(1) Compared with the traditional pretreatment method (pressure permeation method), the pretreatment method for detecting a small amount of fragile samples by using ELEMENT GD glow discharge mass spectrometry is simple and feasible, has low technical requirements on operators, and does not need to use high-purity indium, tantalum and other materials with higher cost.
(2) The sample treated by the method can meet the detection requirement of a ELEMENT GD glow discharge mass spectrometer, a small amount of fragile sample which is difficult to directly put in a ELEMENT GD clamp is prepared into the sample which can meet the normal test requirement, and the problems that the clamp is damaged and damaged possibly after the sample is broken down are prevented.
(3) The method improves the success rate and the accuracy of the test when a small amount of fragile samples are analyzed by ELEMENT GD.
Drawings
FIG. 1 is a schematic process flow diagram of the method of the present invention;
FIG. 2 (a) is a diagram showing the morphology of a sample to be tested (high purity silicon) obtained by the method of the present invention after being fixed between ELEMENT GD holders and detected by a glow discharge spectrometer;
FIG. 2 (b) is a morphology diagram of a small amount of high purity silicon wafer which is not treated by the present invention and meets the test size, directly placed between ELEMENT GD holders for fixing, and the high purity silicon wafer is broken;
FIG. 3 is a graph showing the time course of a sample signal processed by the method;
the reference numerals in the drawings: 1-a small amount of fragile sample to be measured, 2-deionized water, 3-absolute ethyl alcohol, 4-crucible, 5-gas, 6-quartz tube, 7-inert gas, 8-electric furnace, 9-wire cutting machine cutting wire, 10-cutting cooling water, 11-wiper dipped with cleaning agent, 12-sample to be measured meeting the requirement after treatment, and 13-ELEMENT GD glow discharge mass spectrometer clamp holder.
Detailed Description
The invention is further described below with reference to the drawings and examples.
Example 1: as shown in fig. 1, the pretreatment method for detecting a small amount of fragile samples by using ELEMENT GD glow discharge mass spectrometry specifically comprises the following steps:
(1) Placing 22g of high-purity silicon sample in deionized water 2 for ultrasonic cleaning to avoid introducing impurities, wiping the inside and outside of the crucible which is polished inside and outside of the high-purity graphite by using absolute ethyl alcohol 3, and drying by using compressed air (shown in figures 1A to C, wherein A-ultrasonic cleaning the sample to be tested, B-wiping the crucible, C-drying the sample to be tested and the crucible);
(2) Placing the high-purity silicon sample treated in the step (1) in a high-purity graphite crucible 4 (with the inner diameter of the crucible being 23mm, the wall thickness being 2mm and the inner height being 5 mm) with the specific size in the step (1), placing the high-purity graphite crucible 4 in a clean quartz tube 6, introducing high-purity argon into the quartz tube 6, discharging residual air in the tube, placing the quartz tube 6 with the high-purity graphite crucible 4 in an electric furnace 8, heating to 1430 ℃ (the melting point of silicon is 1410 ℃) (shown in the attached drawing 1D, D is that the crucible with the sample to be tested is placed in the quartz tube, introducing inert gas and heating in the electric furnace), preserving heat for 15min, and at the moment, the high-purity silicon to be tested is completely melted and is in close contact with the high-purity graphite crucible (shown in the attached drawing 1E, E is preserving heat and melting the sample to be tested);
(3) After the heat preservation is finished, the electric furnace is closed, the quartz tube 6 is taken out, the quartz tube is naturally cooled to 50 ℃, the high-purity graphite crucible 4 with the high-purity silicon to be detected in the quartz tube 6 is taken out (shown in a figure 1F, F is a crucible with a sample to be detected after cooling);
(4) Cutting the part of the crucible wall higher than the surface of the sample to be measured in the step (5) by using a diamond wire cutting machine (shown in a figure 1G), wherein G is the redundant part of the crucible cut by using the wire cutting machine under the protection of the coolant), and the cutting line 9 of the wire cutting machine is a diamond wire;
(5) And (3) cleaning the surface of the high-purity silicon sample to be tested by dipping the high-purity graphite crucible 4 with the high-purity silicon material after cutting in the step (5) in absolute ethyl alcohol and deionized water in sequence, and drying by compressed air to obtain the high-purity silicon sample (the thickness of the high-purity silicon wafer is 2mm and the diameter is 23 mm), (shown in the attached figures 1H and I, J), wherein H is used for cleaning the surface of the sample to be tested, I is used for successfully preparing the sample to be tested meeting the test requirement, and J is used for placing and fixing the processed sample to be tested in ELEMENT GD).
Example 2: as shown in fig. 1, the pretreatment method for detecting a small amount of fragile samples by using ELEMENT GD glow discharge mass spectrometry specifically comprises the following steps:
(1) Putting 45g of high-purity tellurium sample into deionized water 2 for ultrasonic cleaning to avoid introducing impurities, wiping the inside and outside of the crucible which is polished inside and outside of the crucible by using absolute ethyl alcohol 3, and drying by using argon;
(2) Placing the high-purity tellurium sample treated in the step (1) in a high-purity graphite crucible (with the inner diameter of the crucible being 25mm, the wall thickness being 2.5mm and the inner height being 6 mm) with the specific size in the step (1), placing the high-purity graphite crucible 4 in a clean quartz tube 6, introducing high-purity nitrogen into the quartz tube 6, discharging residual air in the quartz tube, placing the quartz tube 6 with the high-purity graphite crucible 4 in an electric furnace 8, heating to 465 ℃ (tellurium melting point 452 ℃), and preserving heat for 20 minutes, wherein the high-purity tellurium to be detected is completely melted and is in close contact with the high-purity graphite crucible 4;
(4) After the heat preservation is finished, closing the electric furnace 8, taking out the quartz tube 6, and taking out the high-purity graphite crucible 4 with the tellurium to be detected in the quartz tube after the quartz tube 6 is naturally cooled to 30 ℃;
(5) Cutting off the part of the crucible wall higher than the surface of the high-purity tellurium sample to be detected in the step (5) by using a diamond wire cutting machine and using deionized water 2 as a cutting coolant (namely cutting off 4.3 mm);
(6) And (3) cleaning the surface of the high-purity tellurium sample to be detected by dipping the high-purity graphite crucible 4 with the high-purity tellurium material after cutting in the step (5) with anhydrous ethanol and deionized water in sequence, and drying by using argon gas to obtain the high-purity tellurium sample (the thickness of the high-purity silicon wafer is 1.7mm, and the diameter is 25 mm) meeting the test requirement.
Example 3: as shown in fig. 1, the pretreatment method for detecting a small amount of fragile samples by using ELEMENT GD glow discharge mass spectrometry specifically comprises the following steps:
(1) Putting 90g of high-purity selenium sample into deionized water 2 for ultrasonic cleaning, wiping the inside and outside of a high-purity graphite crucible 4 with absolute ethyl alcohol 3, and drying with nitrogen;
(2) Placing the high-purity selenium sample treated in the step (1) in a high-purity graphite crucible 4 (the inner diameter of the crucible is 28mm, the wall thickness is 3mm, the inner height is 8 mm) with the specific size in the step (1), placing the high-purity graphite crucible 4 in a clean quartz tube 6, introducing high-purity argon into the quartz tube 6, discharging residual air in the tube, placing the quartz tube 6 with the high-purity graphite crucible 4 in an electric furnace 8, heating to 240 ℃ (the melting point of silicon is 221 ℃), and preserving heat for 20 minutes, wherein the high-purity selenium is completely melted and is in close contact with the high-purity graphite crucible;
(3) After the heat preservation is finished, closing the electric furnace 8, taking out the quartz tube 6, and taking out the high-purity graphite crucible 4 with the high-purity selenium to be detected in the quartz tube after the quartz tube 6 is naturally cooled to 20 ℃;
(4) Cutting off the part of the crucible wall higher than the surface of the sample to be detected with high purity selenium in the step (5) by using a diamond wire cutting machine and using deionized water 2 as a cutting coolant (namely cutting off by 5 mm);
(5) And (3) cleaning the surface of the high-purity silicon sample to be detected by dipping the high-purity graphite crucible with the high-purity selenium material after cutting in the step (5) in anhydrous ethanol and deionized water in sequence, and drying by using nitrogen gas to obtain the high-purity selenium sample (the thickness of the high-purity silicon wafer is 3mm, and the diameter of the high-purity silicon wafer is 28 mm) meeting the test requirement.
The sample (high purity silicon) to be measured obtained by the method is fixed between ELEMENT GD holders, and after being detected by a glow discharge chromatograph, the sample has a shape shown in figure 2 (a) and a complete shape, the change of signals with time is shown in figure 3, and the signal curve is stable. A small amount of high-purity silicon wafers meeting the test size are directly placed between ELEMENT GD clamps for fixing without treatment of the invention, and the high-purity silicon wafers are broken to form the wafer shown in the figure 2 (b), so that the test requirements cannot be met and the test cannot be completed normally. The method provided by the invention can be used for carrying out pretreatment on a small amount of fragile samples, so that ELEMENT GD can be satisfied for carrying out glow discharge mass spectrometry detection smoothly.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. A pretreatment method for detecting a small amount of fragile samples by using ELEMENT GD glow discharge mass spectrometry, which is characterized by comprising the following specific steps:
(1) Placing a sample to be tested in deionized water for ultrasonic cleaning to avoid introducing impurities, blowing the cleaned sample by using gas, wiping the inside and outside of a crucible by using absolute ethyl alcohol, and blowing the cleaned sample by using gas; the crucible is made of high-purity graphite, is polished inside and outside, is of a cylindrical structure, has an inner diameter of 23-30 mm and a wall thickness of 2-5 mm, and has a height of 5-10 mm;
(2) Placing the sample to be tested treated in the step (1) in a crucible treated in the step (1), placing the crucible filled with the sample to be tested in a quartz tube, introducing inert gas into the quartz tube to discharge residual air in the tube, placing the quartz tube filled with the crucible in an electric furnace, heating to a temperature 10-40 ℃ higher than the melting point of the sample to be tested, and preserving heat for 10-40 min;
(3) After the heat preservation is finished, the electric furnace is closed, the quartz tube is taken out, and after the quartz tube is naturally cooled, the crucible in the tube is taken out;
(4) Cutting off the crucible wall part of the crucible which is higher than the surface of the sample to be measured in the crucible after the crucible is taken out in the step (3) by using a linear cutting machine and using deionized water as a cutting coolant;
(5) And (3) wiping the surface of the sample to be tested in the crucible cut in the step (4) clean, and drying by using gas to obtain the sample to be tested meeting the test requirement.
2. The method of pre-assay treatment of a small amount of fragile sample for ELEMENT GD glow discharge mass spectrometry detection of claim 1, wherein: the gas in the step (1) and the step (5) is argon, nitrogen or compressed air.
3. The method of pre-assay treatment of a small amount of fragile sample for ELEMENT GD glow discharge mass spectrometry detection of claim 1, wherein: the inert gas in the step (2) is high-purity argon or high-purity nitrogen.
4. The method of pre-assay treatment of a small amount of fragile sample for ELEMENT GD glow discharge mass spectrometry detection of claim 1, wherein: and (3) naturally cooling the quartz tube to below 100 ℃.
5. The method of pre-assay treatment of a small amount of fragile sample for ELEMENT GD glow discharge mass spectrometry detection of claim 1, wherein: and (3) the cutting line of the wire cutting machine in the step (4) is a diamond wire.
6. The method of pre-assay treatment of a small amount of fragile sample for ELEMENT GD glow discharge mass spectrometry detection of claim 1, wherein: in the step (5), absorbent cotton or dust-free paper/cloth is used as a wiper and is dipped in absolute ethyl alcohol or deionized water serving as a cleaning agent for wiping.
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| CN104458370A (en) * | 2014-11-23 | 2015-03-25 | 昆明贵金属研究所 | Method for preparing glow discharge mass spectrometer analysis test sample |
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| CN109298065A (en) * | 2018-11-07 | 2019-02-01 | 新疆众和股份有限公司 | The detection method of impurity content in a kind of Al alloy powder |
| CN110865168A (en) * | 2019-11-15 | 2020-03-06 | 江苏隆达超合金航材有限公司 | Method for rapidly analyzing main amount, trace amount and trace elements in alloy slag |
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| WO2012048460A1 (en) * | 2010-10-13 | 2012-04-19 | 大连理工大学 | Low resistivity high thermal-stability copper-nickel-molybdenum alloy film and producing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104458370A (en) * | 2014-11-23 | 2015-03-25 | 昆明贵金属研究所 | Method for preparing glow discharge mass spectrometer analysis test sample |
| CN108680412A (en) * | 2018-06-04 | 2018-10-19 | 中钢集团新型材料（浙江）有限公司 | A kind of sample preparation methods and test method for calcined coke coefficient of thermal expansion |
| CN109298065A (en) * | 2018-11-07 | 2019-02-01 | 新疆众和股份有限公司 | The detection method of impurity content in a kind of Al alloy powder |
| CN110865168A (en) * | 2019-11-15 | 2020-03-06 | 江苏隆达超合金航材有限公司 | Method for rapidly analyzing main amount, trace amount and trace elements in alloy slag |
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